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Indonesian National Standard
Portland cement
ICS 91.100.10 National Standardization Body
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List of contents
List of contents.................................................................................................................................... i
List of Tables............................................................................................................................. iii
List of Figures........................................................................................................................ iv
Foreword................................................................................................................................... v
1 Scope.................................................................................................................. 1
2 Normative references................................................................................................................... 1
3 Terms and definitions............................................................................................................ 1
4 Types and uses................................................................................................................... 2
5 Quality requirements........................................................................................................................... 2
6 Sampling method................................................................................................... 5
7 Test method........................................................................................................................... 10
7.1 Chemical test method......................................................................................................... 10 7.1.1

Cement test method and permitted variations..............................................................10
7.1.2 General................................................................................................................... 12
7.1.3 Referee method.......................................................................................................14
7.1.3.1 Insoluble part.................................................................................................14 7.1.3.2

Silicon dioxide (SiO2) ............................................... ............................................ 15 7.1.3.3 Group
of ammonium hydroxide (R2O3) ............................................................... .......... 18 7.1.3.4 Iron (III)
oxide (Fe2O3)............................ .................................................. .... 20 7.1.3.5 Phosphorus
pentaoxide (P2O5)................................. ......................................... 22 7.1.3.6 Titanium dioxide
(TiO2) .................................................. ............................... 24 7.1.3.7 Zinc
oxide.......................................................................................................... 26
7.1.3.8 Aluminum oxide..........................................................................................26
7.1.3.9 Calcium oxide (CaO)..........................................................................................26 7.1.3.10

Magnesium oxide ( MgO).............................................................................29
7.1.3.11 Sulfur................................................................................................................ 30
7.1.3.12 Loss of glow......................................................................................................... 34

7.1.3.13 Sodium and potassium oxide................................................................................ 35
7.1.3.14 Manganese oxide................................................................................................. 39

7.1.3.15 Chloride............................................................................................................ 41
7.1.3.16 Organic compounds that dissolve in chloroform......................................................45
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7.1.4 Alternative test method (Optional)...............................................................................48

7.1.4.1 Calcium oxide..................................................................................................... 48
7.1.4.2 Magnesium oxide volumetric method...................................................................49
7.1.4.3 Titanium dioxide.............................................................................................. 52 7.1 .4.4

Phosphorus pentaoxide.......................................................................................... 57 7.1.4.5
Manganese oxide.................................................................................................. 60
7.1.4.6 Free calcium oxide........................................................................................... 61
7.2 Physics test method.............................................................................................................. 64 7.2.1

Auxiliary materials and equipment............................................................................64 7.2.2
Testing smoothness with blaine and turbidimeter tools ............................... 65 7.2.2.1 With
blaine tools... .................................................. ........................................... 65 7.2.2.2 With a
turbidimeter ...... .................................................. ............................... 75 7.2.3 Normal consistency
test ............. .................................................. .................. 89 7.2.4 Testing time of
binding ............................... .................................................. .... 92 7.2.5 Expansion test with
autoclave................................................. ........................... 98 7.2.6 Determination of the
compressive strength of hydraulic cement mortar.......................................................103
7.2.7 Rapid stiffening test of portland cement (paste method)...............................114
7.2.8 Determination of hydration heat............................................................................................ 118
7.2.9 Test for expansion due to sulfate...........................................................................126 7.2.10

Testing the air content of mortar.................................................................................129
8 Requirements for passing the test................................................. .................................................. ...............

132 9 Packaging................................................................................................................. 132
10 Terms of marking.......................................................................................................................... 132
11 Storage and transportation........................................................................................................... 132
Appendix A........................................................................................................................... 133
Appendix B........................................................................................................................... 134
Appendix C............................................................................................................................. 136
Bibliography............................................................................................................................. 139
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List of Tables
Table 1 ÿ Main chemical terms..................................................................................................... 2 Table 2 ÿ
Additional chemical terms...................................................................................................... 3
Table 3 ÿ Main physics requirements..................................................................................................... 4
Table 4 ÿ Additional physics requirements................................................................................................ 4
Table 5 ÿ Test time interval after sampling...................................................6
Table 6 ÿ Permissible difference in test results.............................................................................11
Table 7 ÿ Comparison of MgO levels with the required amount of reagent................51
Table 8 ÿ Comparison of MgO levels with the amount of standard solution...............................................52
Table 9 ÿ Specific gravity of mercury, air viscosity (ÿ) and ÿ at a certain temperature..............73
Table 10 ÿ Cement coating porosity values............................................................................73
Table 11 ÿ Airflow time range.......................................................................................... 74
Table 12 ÿ Dimensions of the turbidimeter apparatus............................................................................. 78
Table 13 ÿ h, d and h/d

2
values used in the calibration of turbidimeter equipment..........82
Table 14 ÿ Burette dimensions......................................................................................................... 82
Table 15 ÿ Example of recording turbidimeter test data and calculations

specific surface......................................................................................................... 88
Table 16 ÿ Allowable variation of die casting (mm).............................................104
Table 17 ÿ Standard sand requirements......................................................................................... 106
Table 18 ÿ Mortar composition.................................................................................................. 108
Table 19 ÿ Test time tolerances.......................................................................................... 110
Table 20 ÿ Accuracy........................................................................................................................ 113
Table 21 ÿ
Deviation............................................................................................................... 129
Table 22 ÿ Ottawa sand grain gradations......................................................................................... 130
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list of Figures
Figure 1 ÿ Cement sampling pipe.................................................................................... 8 Figure 2 ÿ Packaged cement
take-up pipes.................................................................8
Figure 3 ÿ Blaine tool................................................................................................................ 67
Figure 4a ÿ Front view of the turbidimeter with the door open..................................................75
Figure 4b ÿ Front view of the turbidimeter with the door open..................................................76
Figure 5 – Turbidimeter rear view................................................................................. 76
Figure 6 – Time burette.............................................................................................................. 77
Figure 7 – Turbidimeter electrical system.............................................................................................. 77 Figure 8 –

Vicat tool................................................................................................................. 89
Figure 9 – Gilmore tool............................................................................................................... 97
Figure 10 – Cement paste slab shape............................................................................ 98
Figure 11 – Prism print..................................................................................................... 99
Figure 12 – Comparator........................................................................................................... 100
Figure 13 – Stirrer machine................................................................................................... 104
Figure 14 – Mixer............................................................................................................ 104
Figure 15 – Bowl.............................................................................................................................. 105
Figure 16 – Flow table................................................................................................................ 105
Figure 17 – The sequence of collisions................................................................................................. 110
Figure 18 – Calorimeter tool................................................................................................... 119
Figure 19 – Stirrer calorimeter............................................................................................... 119
iv
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Foreword
ST hN i sI 2 s 0t a 4 n9 d : 2a 0 r d1 5 w , a P so r r e
asdintna addy nu sds 4 fta or ry rdk agt yi ns pd t eah icneI k. c aiIr n ge ear e sd
t l va in s d C w e mi t he nt ht e is a i m r e o v f i s i ni o c
.ia dn sig t eio einnx ,p t toh re et srce o imf s cpae rl ms e os s na i v t c ec h o sa
n r eo af s S in N g I t1 h 5 e - 2n 0a 4t i o9 n-
m tn r emg ne o g ditn h it iper a es c q. kuT aihr gee i mn mg
2 0 l 0 c4 a ,p Pa co ir t t y l a o n f d t C ee cm e em n et .
e ,an ni tns a m tfeo ecr hl3y n td i h c a ae y l sa c, dh 7da i ndti goa eny s too af
n t
nt2h d5is2k8g
This standard was prepared and formulated by the Technical Committee 91-02, Chemistry and Construction Materials.
This standard is the result of a consensus held in Jakarta on 29 April 2013, which was
attended by representatives of stakeholders such as producers, consumers, test centers
and other relevant technical agencies. This standard has also gone through the stages of
national consensus, namely the opinion poll on 27 November 2013 – 25 January 2014, and
voting from 12 May – 10 July 2014.
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Portland cement
1 Scope This standard

defines quality requirements, sampling systems and test methods for portland cement. This standard is
applicable to 5 types of portland cement, with a packing limit of up to 50 kg and excluding cement used for
ready mix.
2 Normative references
ASTM C 430-08, Standard Test Method for Fineness of Hydraulic Cement by the 45-µm (No.
325) Sieves
AMSeTthModCs 6fo7r0C-1o3n,sStrtuacntdioanrdMPartaecritaiclse for Preparing Precision and Bias Statements for

Test
3 Terms and definitions
3.1
portland cement
hydraulic cement produced by grinding Portland cement slag, consisting mainly of hydraulic calcium silicate
and grinding together with additives in the form of one or more crystalline forms of calcium sulfate
compounds and may be supplemented with other additives
3.2
air content of hydraulic cement hydraulic
cement containing a specified amount of added air to cause air to be contained in the mortar within
specified limits when measured by a method
3.3
Cement paste
is a mixture of cement and water, either hardened or non-hardened
3.4
false sets
lose rapidly the plasticity of cement paste, mortar or concrete
3.5
humid chamber
an enclosed space for the storage and curing of samples of paste, mortar and concrete which has a
regulated temperature and high relative humidity
3.6
mortar
a mixture consisting of cement, fine aggregate and water in good condition
hardened or not hardened
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4 Types and uses
4.1 Type I, namely portland cement for general use which does not require special requirements as
required for other types.
4.2 Type II, namely portland cement which in use requires moderate resistance to sulfate or heat of hydration.
4.3 Type III portland cement which in use requires high strength in the initial stage after setting occurs.
4.4 Type IV, namely portland cement which in use requires low hydration heat.
4.5 Type V, namely portland cement which in its use requires high resistance to sulphate.
5 Quality requirements
5.1 Chemical requirements of portland cement must meet the following requirements:
Table 1 ÿ Main chemical terms

unit in %
No Description Types of portland cement

I III IV V
1 SiO2 , minimum -
II b,c)
20,0 6,0 - - -
- - - -
2 Al2O3 , maximum 6,0
, maximum - - -
3 Fe2O3 b,c) 6,0 6.5
6.0 6.0 6.0 6.0
4 MgO, maximum
5 SO3, maximum
If C3A ÿ 8.0 3.0 3.0 3.5 2,3d ) 2,3d )
d)
If C3A ÿ 8.0 3.5 4.5
6 Loss of glow, maximum 5.0 3.0 3.0 2.5 3.0
7 parts insoluble, maximum 3.0 1.5 1.5 1.5 1.5
8 C3S, maximum a) - - - 35 b) -
9 C2S, minimum a) - - - 40 b) -
10 C3A , maximum a) - 8.0 15 7 b) 5 b)
11 C4AF + 2C3A or a)
C4AF + C2F, maximum - - - - 25 c)
NOTE a)
Chemical limitation requirements based on calculations for certain potential compounds do
not necessarily imply that the oxides of said potential compounds are in a pure state.
C = CaO, S = SiO2, A = Al2O3, F = Fe2O3, Example C3A = 3CaO.Al2O3

Titanium dioxide (TiO2) and phosphorus pentaoxide (P2O5) are included in Al2O3.
The value commonly used for Al2O3 in calculating potential compounds (eg C3A) for
specification purposes is the amount of precipitate obtained by adding NH4OH minus
the amount of Fe2O3 (R2O3 – Fe2O3) obtained in wet chemical analysis.
If: % Al2O3 ÿ 0.64 , then the percentages of C3S, C2S, C3A and C4AF are calculated as follows:
% Fe2O3
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Table 1 - Main chemical terms (continued)

I II III IV V
C3S = (4.071 x % CaO) – (7.600 x %SiO2) – (6.718 x % Al2O3) –(1.430 x % Fe2O3) – (2.852 x
% SO3)
C2S = (2.867 x %SiO2) – (0.7544 x % C3S)
C3A = (2.650 x % Al2O3) – (1.692 x % Fe2O3)
C4AF = (3.043 x % Fe2O3)
If: % Al2O3
ÿ 0.64 , formed a solid solution ( C4AF + C2F) = 4CaO. Al2O3.Fe2O3
% Fe2O3
Cement with this composition does not contain C3A. then (C4AF +
C2F) and C3S are calculated as follows:
(C4AF + C2F) = (2.100 x %Al2O3) + (1.702 x %Fe2O3)
C3S = (4.071 x % CaO) – (7.600 x %SiO2) – (4.479 x % Al2O3) –(2.859 x % Fe2O3) – (2.852 x
% SO3)
C2S is still calculated using the formula above: Calculations for all potential compounds are based on
the results of the determination of the oxide which is calculated to be as close as possible to 0.1%. All
calculation results are reported as close as possible to 1.0%.
b)
If what is required is the heat of hydration as stated in the additional physical requirements table (Table
4), then this chemical requirement does not apply.
c)
If what is required is expansion due to sulfate listed in the additional physical requirements table (Table
4), then these chemical requirements do not apply.
d)
Cannot be used. Table 2 ÿ Additional chemical requirements a)

unit in %

I II III IV V
1 C3A , maximum - - 8 - -
2 C3A , minimum - - 5 - -
3 (C3S + 2 C3A) , - - - -
maximum 58b )
4 Alkali, as
c)
(Na2O + 0.658 K2O), maximum 0.60 c) 0.60 c) 0.60 c) 0.60 c) 0.60
NOTE a)
These additional chemical requirements apply only as specifically required.
b) The same as the description for the mabin) chemical terms.
c)
Applicable only when cement is used in concrete in which the aggregate is reactive
to alkali.
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5.2 Portland cement physics requirements must meet the following requirements:
Table 3 ÿ Main physical terms
Types of portland cement

No Description I II III IV V
1 Subtleties:
2
Air permeability test, m /kg
with tools :
- Turbidimeter, min 160 160 160 160 160
- Blaine, min 280 280 280 280 280
2 Eternity :
Autoclave expansion, max % 0.80 0.80 0.80 0.80 0.80
3 compressive strength:
- Age 1 day, kg/cm 2 - - 120 -

, minimum
2
- Age 3 days, kg/cm 135
, minimum 710a0) 240 -80
2 215 175 - 150
- Age 7 days, kg/cm , minimum -70
120 a)
- Age 28 days, kg/cm 2 minimum
, 300 - - 170 210
4 Fixing time (alternative method) with tools:
a) Gillmore
- Initial, minute, minimum 60 60 60 60 60

- End, minute, maximum b) Vicat 600 600 600 600 600
- Initial, minute, minimum 45 45 45 45 45

- End, minute, maximum NOTE 375 375 375 375 375
a)
This compressive strength requirement applies if the hydration heat requirements are as listed in the
additional physical requirements table (Table 4) or if the C3S + C3A requirements as listed in the additional
chemical requirements table are required (Table 2).
Table 4 ÿ Additional physics requirements a)

number Description
II III IV V
1
Final penetration pseudo-binding, I
50 50 50 50 50
% minimum
2 Hydration calories
- Age 7 days, cal/gram, max - - -
70 b) 60
- Age 28 days, cal/gram, max - - - -

70
3 Compressive Strength:
2
Age 28 days, kg/cm minimum , - - - -
280
4 Expansion due to sulfate 14

- 220 b) - -
days, %, max 0.040
5 Air content of mortar,

12 12 12 12 12
% volume, maximum
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Table 4 - Additional physics requirements (continued)

No Description I II III IV V
NOTE a)
These
b)
additional physics requirements apply only when specifically requested.
If the hydration heat requirements are required, then the C3S + C3A requirements as listed in
the additional chemical table (Table 2) are not required.
This compressive strength requirement applies if the hydration heat requirements are as stated in
the additional physical requirements table (Table 4) or if the C3S + C3A requirements are required
as stated in the additional chemical requirements table (Table 2).
6 Sampling method
6.1 Description of specific terms for standard methods
6.1.1 Cement lots
A cement lot is a specific quantity of cement submitted for inspection at any given time. One
lot can represent one or more bins that have been filled with cement sequentially. One lot
can also represent the contents of one or more units of transport equipment issued from the
same bin.
6.1.2 Adjusted sampling frequency
This is the test program prepared for testing of only two cement samples obtained from
each available lot, and prepared for testing at the usual stages as described below.
The program uses likelihood factors and is designed in such a way that if the test results
from the two samples meet the requirements of the program, it can be interpreted as a 95%
confidence level and less than 5% of the samples will be outside the specification limits.
6.2 Purpose and use
6.2.1 The sampling procedure described above is intended for use in hydraulic
cement sampling requirements, once it has been manufactured and ready for use.
marketed.
This procedure is not intended as a sampling procedure for quality control during the
production process.
The test procedures that have been described include the number of samples for the tests
to be carried out and provide guidance in terms of preparing reports.
6.2.2 Most of the requirements and specifications required by building construction are
that the hydraulic cement to be used in the work must meet the requirements as stated in
the purchasing specifications, such as the specifications according to Article 5.
If the aforementioned regulations or specifications require sampling of the cement produced

then the provisions given in 6.4.1 must be implemented.
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6.3 Implementation procedures
6.3.1 This implementation procedure includes a sampling and testing process with a view to
determining whether the cement sample meets the requirements of the acceptance specification.
Testing of cement samples is carried out using certain methods to determine whether the test
results obtained from the cement samples meet the specifications and the test results are stated
as the basis for acceptance or rejection of the lot of cement represented by the sample.
6.3.2 It is neither intended nor required that cement be tested using all the chemical and
physical test methods listed in this standard.
6.4 Type and size of cement samples; sampling
6.4.1 Grab samples are cement obtained from conveyor belts, from bulk cement warehouses
or from bulk cement ships.
Samples can also be taken from a continuous stream of cement at 10-minute intervals using
an automatic sampling device, also known as a sample sample.
The quoted samples taken at each of these time intervals, over a specified period of time shall
be combined into composite samples, representing the cement produced over a specified
period of time.
6.4.2 All cement samples, whether quoted samples or composite samples weigh at least 5 kg.
6.4.3 Cement samples must be packaged in vapor and airtight containers which have
been numbered regularly and sequentially.
6.5 Time required to complete the test
6.5.1 The cement producer should prepare so that the cement can be sampled, the test is
carried out as early as possible before the time the test results are required. So that at least the
time interval that applies to 6.5.2 can be followed.
6.5.2 When these things have been done, the testing laboratory shall prepare the test results
not later than the stated number of days after the time of sampling.
Table 5 ÿ Time interval after
sampling No Testing Time lapse (days)

1 Compressive strength (1 day old test results) 8
Chemical analysis, autoclave, normal consistency with
vicat tool, smoothness with blaine tool, fast stiff paste
method.
2 Compressive strength (3 days old test results) 10
3 Compressive strength and hydration heat (7 days old test result) 14
4 Expansion due to sulfate (14 days old test result) 21
5 Compressive strength and heat of hydration (test results 28 days old) 35
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6.6 Sampling
6.6.1 From the conveyor belt being conveyed to the bulk cement warehouse
Take a sample of cement quotation weighing at least 5 kg at an interval of about 6 hours.
6.6.2 Semen sampling at the time of transfer
Sampling of cement from the warehouse when the cement is being transferred from one bin
to another. Take one cement sample from the cement stream being transported, for every
400 tonnes of cement or multiples thereof, but the samples shall not be less than the cement
quotations and combine to obtain a composite sample.
6.6.3 Other methods of sampling
If the two sampling methods above cannot be used, cement samples can be obtained
using one of the methods below:
6.6.3.1 From the bulk cement warehouse in the discharge pit
Take a cement sample from the dispensing hole while the cement flow is constant, until
all sampling is complete. Estimated amount of cement that must be taken in tons using
the formula:
0.001 73
x d³ x 0.2
35.314
Note: d
is
the depth of cement in meters, which is above the discharge hole.
If the cement sample is taken from a cylindrical bulk cement warehouse, the sample will only
be taken from one of the discharge holes. If the volume of bulk cement in the warehouse
exceeds 1 200 tonnes, and also if the warehouse is rectangular in shape, the cement
samples taken but not from the discharge pits are such that they must represent more than
half of the cement stored in the warehouse.
When the cement is flowing through the discharge hole, take cement samples at certain
intervals, so that it must represent more than half of the amount of cement stored in
the warehouse.
While the cement is flowing through the discharge hole, take cement samples at certain
intervals, so that for every 400 tons of cement flow, at least 2 samples are taken from bins
or silos.
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6.6.3.2 ari gudan cement curah and n bulk d use ith me tool
what the heck
sampling
If the depth h to be sama pslaemd pdloinegs tnoootl efoxrcteheed2s.a1meethaesr,

sthowsanminpFleigduerpeth1.cTahnebleenogbtthaibnetdwuesein g
1, 5 m to 1.8pimpeasnwditahninaonsueetrerpireidpsieaom.f peeterfrooraf taiopnpsrotxh.a3t
5camnmb,ewohpiecnhecdonasnidstcsloosf e2dcboyrrtuugrantinegd tshte l
The tip of the outer pip is

tapered so that it makes it easier for penetration.
Take samples of cement from points that are spread d differently

just average with depth which
so that all of theelesmteanktesn will be represented by the
different
6.6.3.3 ari bag g cement it's a example in nature

with tool i. take
pockets user
Stick it
crosswise method
and pull a hole puncchloesretasktehse aisr ahmolpelewithayboaugr tahsumshbo,
wthneinn cFeigmuernet 2it,. tthhee.bag then Take one sample
from Kanto for every 5 tons or g of cement
the multiplier.
Figure 1 ÿ Intake example se en

pipe
G mbar 2 ÿ
Ipa Peng take all n in golden k
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6.6.3.4 From delivery of bulk cement by rail or truck
6.6.3.4.1 Single delivery
If the shipment is carried out using only one train car or one cement truck, which is
continuously loaded and comes from one source, take one sample of cement weighing 5 kg.
If it is not continuously loaded and the source is unknown, combine 5 or more parts of
cement samples from several different points to be used as test samples.
6.6.3.4.2 Multiple dispatch
If the shipment consists of several railroad cars or several cement trucks loaded from
the same source and on the same day, take cement samples for every 100 tons or
multiples thereof, but not less than 2 samples. Treatment of cement samples
ains tahne esexactmiopnle"soafmapcle weenigt hlot tf.oAr ntedsstianmg"p. le test in accordance with the
procedure described
6.7 Storage of cement samples
After the cement sample is taken, immediately place it in an airtight and moisture-tight
place to prevent water absorption or aeration from the cement sample.
If the cement sample is placed in a container made of cans, close it tightly and seal it
immediately. Use bags consisting of several layers of moisture-resistant paper, or plastic
bags, which are strong enough so they don't break. Try to seal them immediately after filling
in such a way that the air in the bag escapes and the absorption of moisture and aeration is
prevented.
The cement sample shall be treated as described in the section "Preparation of the
test sample".
6.8 Preparation of test sample
Prior to testing, sift the cement through an 850 µm sieve (a No. 200 sieve or another
sieve that has approximately the same opening size).
In order for the sample to mix well, break up any lumps, and collect the dirt. Remove any
hardened impurities and lumps that could not be broken during sieving. Store cement in
an airtight place to prevent absorption of moisture before testing.
6.9 Failure to comply with requirements and retesting
6.9.1 If any of the test results fails to meet the requirements, the lot of cement is not
reported as cement that does not meet the specifications until the failure is confirmed by the
number of retests.
6.9.2 A retest may consist of one type of test or all of the tests in its entirety.
6.9.3 Retests shall be carried out in accordance with the specifications

used. If these conditions are not provided, the procedure below should be
used.
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6.9.4 Retest a portion of the cement sample used in the initial test. Use of another method for the
determination of the properties of the cement is required in the retest and in this case only the test
results obtained by the other method are used.
The retest shall consist of the number of determinations required as for the initial test. The number of
repetitions used is based on the accuracy requirement. If two or more determinations are required,
the reported price must be the average value of all test results within the accuracy limits of the 95%
confidence level method, as stated in the specifications that are used or generally known.
7 Test method
7.1 Chemical test method
Any test method that exhibits acceptable accuracy and deviation can be used for hydraulic cement
analysis, including the referee test method, as described in 7.1.1.
Specific chemical test methods are given for convenience for those who want to use them.
Test methods are grouped as referee test methods and alternative test methods. The referee test
method is an accepted wet chemical test method, which provides a basic integrated scheme of
hydraulic cement analysis.
Alternative test methods generally provide an individual determination of a particular component and
can be used alone or alternatively and an integrated determination if desired by the analyst as shown
in the individual methods. Each analyst must be able to demonstrate high skills as described in 7.1.1,
if this method is used.
7.1.1 Cement test method and permissible variations
7.1.1.1 Referee test method
The referee test method as stated in 7.1.3.1 to 7.1.3.16 or other test methods determined according
to 7.1.4, is used if the results of the analysis using the referee test method are doubtful to meet the
chemical requirements.
In such a case, the cement cannot be rejected for not meeting the chemical requirements unless all
the determination of the elements and all the necessary preliminary separations have been carried
out by the referee test method.
In case of doubt, the analysis should be carried out twice on different days.
If the results do not agree with the allowable variations in Table 1, the determination is repeated until
2 or 3 results meet the allowable variations for purposes of analytical comparison and calculation of
the average of acceptable results, the percentages should be calculated to be as close as possible to
0.01 (or 0.000 1 for organic compounds soluble in chloroform), although some average results are
reported to the nearest 0.1.
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Table 6 ÿ Permissible difference in test results

Maximum difference from the
Maximum
No difference average of two SRM
Component Certificate designations
two tests of 0.16 (units in %) ÿ 0.2
1 SiO2 (Silicon dioxide)
2 Al2O3 (Aluminum oxide) 0.20 ÿ 0.2
3 Fe2O3 (Iron(III) oxide) 0.10 ÿ 0.10
4 CaO (Calcium oxide) 0.20 ÿ 0.30
5 MgO (Magnesium oxide) 0.16 ÿ 0.2
6 SO3 (Sulfur trioxide) 0.10 ÿ 0.1
7 HP (Disappearance) 0.10 ÿ 0.10
8 Na2O (Sodium oxide) 0.03 ÿ 0.05
9 K2O (Potassium oxide) 0.03 ÿ 0.05
10 TiO2 (Titanium dioxide) 0.02 ÿ 0.03
11 P2O5 (Phosphorus pentaoxide) 0.03 ÿ 0.03
12 ZnO (Zinc oxide) 0.03 ÿ 0.03

13 Mn2O3 (Manganese oxide) 0.03 ÿ 0.03
14 S (Sulfide) -
0.01
15 Cl (Clride) -
0.003
16 IR (Insoluble portion) -
0.10
17 FL (Calcium oxide free) -
0.20
18 Alk sol (Alkali which
dissolves in water -
0.75/w
19 Chl sol (an organic
compound that dissolves in -
chloroform) 0.004
7.1.1.2 Alternative test methods
In some cases alternative methods provide shorter procedures or are more suitable for routine
determination of certain components than the referee test method (see NOTE).
In some cases, a more complex and lengthy procedure is still used as an alternative test method for
comparing results with different procedures or for use when special materials are being tested with
foreseeable defects, or when special preparation for analysis is required. . The test results from
alternative test methods may be used as a basis for acceptance or rejection if the results clearly
show that the cement does or does not meet the specifications.
NOTE This is not intended to limit the use of the referee's test method for reference analysis. A referee
test method is better to use than an alternative test method when it is absolutely necessary.
A reference test method shall be used if an alternative test method is not provided.
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Multiple analysis and blank determination are not required when using alternative test methods. But if a
blank determination is desired for an alternative test, this one may be used and it need not be made if it
has been obtained concurrently with the analysis.
The final results, when corrected for blank values, should in each case be shown.
7.1.2 General
a) It is sufficient to weigh the reagent whose weight is expressed by "approximately 5 grams".

rough value.
b) The contents of the solution stated as "approximately 300 mL are sufficient to be observed by eye, the
contents of which are "10 mL" are sufficient with a measuring cup and the contents stated "exactly 25 mL"
must be measured with a burette or pipette.
c) "Cold" must mean room temperature, "warm" between (30-40) oC, and "hot" must
interpreted temperature close to the temperature of boiling water (90-95) oC.

d) Burette readings must be up to 0.01 mL and if used is a solution with a titer
low, a micro-buret should be used.
e) If water is used in the test, what is meant by water is distilled water.
7.1.2.1 Equipment and materials
7.1.2.1.1 Equipment
(1) Equipment for weighing: Analytical balance with a capacity of not more than 200 grams.
The balance must be capable of producing repeat readings with no difference
more than 0.000 2 grams with an accuracy of 0.000 2 grams.

(2) Laboratory equipment made of glass and polyethylene materials:
a) Measuring flasks, burettes and pipettes must be of high precision.
b) Special types of glassware such as tinted glass, high silica glass and alkali resistant glass.
c) Containers made of polyethylene for all lye and standard solutions. d) The desiccator is
equipped with a desiccant such as magnesium perchlorate, activated alumina, or sulfuric acid.
Anhydrous calcium sulfate can also be used, but calcium chloride is not suitable for this
analysis.
e) Filter paper: coarse porous, fine porous, and medium porous. f) Crucible:
Crucible made of platinum with a capacity of (15-30) mL. g) Heating furnace: A furnace
equipped with a pyrometer with an accuracy of ÿ 25 oC.
7.1.2.1.2 Materials
For all tests, “chemical grade” reagents shall be used, unless otherwise advised.
Other reagents used must have sufficiently high purity without compromising the accuracy of the
determination.
(1) Reagent concentration
a) Ready-to-use reagent
Ready-to-use standard reagent solutions or in diluted concentrations can be used if provided with
specifications for the level of purity.
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b) Concentrated acid and ammonium hydroxide
If acids and ammonium hydroxide are only equipped with requirements based on names and
chemical formulas, this must mean that the reactants must be in a concentrated state according to
the specific gravity (bj) or weight concentration as follows: Acetic acid (CH3COOH )
99.95%
Hydrochloric acid (HCl) bj 1.19
Hydrofluoric acid (HF) 48%
Nitric acid (HNO3) bj 1.42
Phosphoric acid (H3PO4) 85%

Sulfuric acid (H2SO4) bj 1.84 Ammonium
hydroxide (NH4OH) bj 0.90
c) Acid and dilute ammonium hydroxide

Specified as a ratio of the volume of concentrated reagent to the volume of water added, for example
HCl (1+99), means that 1 volume of concentrated HCl (bj 1.19) is added to 99 volumes of water.
d) Standard solution
The concentration of the standard solution is expressed in terms of normality (N) or as the equivalent
in grams per milliliter of the component specified. At least three determinations must be made to obtain
an average result from standardization.
e). Concentration of non-standard solutions prepared by dissolving solid reagents in
certain unit weight dissolved in water, unless the solvent is specified otherwise.
(2) Indicator solution
a) Methyl red: 2 gram methyl red/L in 95% ethanol. b)
Phenolphthalein: 1 gram of phenolphthalein/L in 95% ethanol.
7.1.2.2 Suggested sequence of reports of components of chemical analysis of portland cement
(1) Major components a)

SiO2 (Silicon
dioxide)
b) Al2O3 (Aluminum oxide) c)

Fe2O3 (Iron (III) oxide) d)
CaO
(Calcium oxide) e) MgO
(Magnesium oxide) f) SO3 (Sulfur
trioxide) g) Fading
(2) Minor components a)

Na2O (Sodium oxide) b)
K2O (Potassium oxide) c)
TiO2 (Titanium dioxide) d)
P2O5
(Phosphorus pentaoxide) e) ZnO (Zinc
oxide) f) Sulfur sulphide g)
Mn2O3 (Manganese oxide )
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(3) Separate determination

a) Insoluble portion
b) Organic compounds soluble in chloroform c)
Free calcium oxide d) Alkalis soluble in water
7.1.3 Referee method
7.1.3.1 Insoluble portion
7.1.3.1.1 Summary of test method
In this method the insoluble portion of semen is determined by digesting the sample in HCl.
After filtering, it is then digested with sodium hydroxide. The residue obtained was ignited
and weighed.
Wcohmepnlethteisiftethset mpoertthlaonddisceumseednot
nslabgleinsdceodmcpelmetelyt,ddeeccoommppoosseitdio. n in acid is considered
Ammonium nitrate solution is used in the final wash to prevent fine insoluble matter
from escaping the filter paper.
7.1.3.1.2 Reagents
a) Ammonium nitrate solution ( 20 gram/L NH4NO3).

b) Sodium hydroxide solution (NaOH 10 gram/L).
7.1.3.1.3 Procedure
a) Weigh 1 gram of sample, put it in a 250 mL beaker, add 25 mL of

water and 5 mL HCl.
b) If necessary, heat the solution and press down on the sample with the end of the stirring rod
glass until completely decomposed.
c) Dilute the solution to 50 mL with hot water and heat on a hot plate to near boiling point.
d) Filter through medium porous filter paper into a 400 mL beaker, wash the beaker, filter
paper and precipitate 10 times with hot water and the filtrate is used for SO3 determination .
e) Transfer the filter paper and precipitate to the original beaker, add 100 mL of hot
NaOH solution (10 gram/L) and digest for 15 minutes at almost boiling temperature.
f) During digestion, stir the mixture occasionally and crush the filter paper with a stirring
rod. Acidify the solution with HCl and using methyl red as indicator, add excess HCl
(4-5) drops.
g) Filter with medium porous filter paper and wash the precipitate at least 14 times with hot
NH4NO3 solution (20 gram/L) to ensure that the filter paper and its contents are
thoroughly washed. The filter paper and its contents are placed in a crucible of known
weight. Burn and ignite at a temperature of (900 - 1 000) oC at least
least 30 minutes. Cool in a desiccator then weigh.
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h) Blank
Perform a blank determination using the same reagent and
method. Take the result as a correction in the calculations.
7.1.3.1.4 Calculations
Calculate the content of the insoluble part to the nearest 0.01%.
Sediment weight X 100

% insoluble part Sample weight
=
7.1.3.2 Silicon dioxide (SiO2)
For portland cement of which the insoluble portion is not known, first determine it
according to 7.1.3.1.
cFeomr peonrttltahnedpceercmeenntat gtheeinpseorlcuebnletaigsegoref aintesroltuhbalne 1p%or,tigoon

tios l7e.s1s.3t.h2a.2n. 1%, go to 7.1.3.2.1, for
7.1.3.2.1 Silicon dioxide with an insoluble fraction of less than 1%
7.1.3.2.1.1 Summary of test method
In this test method silicon dioxide (SiO2) is determined gravimetrically.
Add ammonium chloride and the solution must not be evaporated until dry. This method
was developed especially for hydraulic cements which are almost completely decomposed
by hydrochloric acid and should not be used for hydraulic cements which contain mostly
acid-
insoluble materials and require pre-smelting of sodium carbonate. For such cements, or if
standard specifications are required for the cement being analyzed, the procedure in
7.1.3.2.2
shall be used.
7.1.3.2.1.2 Reagents
a) Ammonium chloride (NH4Cl).

b) Hydrochloric acid (HCl). c)
Hydrochloric acid (HCl)(1+99). d)
Nitric acid (HNO3). e) Sulfuric
acid (H2SO4)(1+1). f)
Hydrofluoric acid (HF).
7.1.3.2.1.3 Procedure
a) Mix the cement evenly 0.5 gram sample with approximately 0.5 gram NH4Cl in a 50
mL beaker, cover the beaker with a watch glass and carefully add 5 mL HCl by
pouring through the inner edge of the beaker . After the chemical reaction is
complete, remove the watch glass, add 1 or 2 drops of HNO3, stir the mixture with a
glass stirrer, cover again and place the beaker on the steam bath for 30 minutes.
During this digest time, stir the contents of the glass occasionally and break up any
lumps that are still there to facilitate complete decomposition of the
cement.
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Place the filter paper with a porous medium in the funnel, transfer the silicic acid
clumps to the top of the filter as much as possible without diluting, and let the solution
drip.
Rub the inner wall of the beaker with a stirring rod equipped with a rubber scourer,
and rinse the beaker and the stirring rod with hot (1+99) HCl.
Wash the filter paper with hot HCl (1+99) and then wash it with hot water little by little
10 or 12 times, save the filtrate and washing water for the determination of the
ammonium hydroxide group.
b) Transfer the filter paper and precipitate into a crucible of known weight, dry and ignite
slowly at a low temperature until the carbon from the filter paper disappears without
any flame from the filter paper, then continue heating at a temperature of (1 100 - 1
200) oC for 1 hour.
Then heat it again until the weight remains (w1). Treat the SiO2 obtained
containing a small amount of impurity in a crucible with 1 mL or 2 mL of water, 2 drops of H2SO4 (1+1) and approximately 10 mL of HF, and
carefully evaporate until dry.
Finally, ignite the small residue at (1 050 – 1 100) oC for 5 minutes, cool in a desiccator
and weigh (w2). The difference in weight between this (w2) and before being given
HF (w1) is the weight of SiO2. Keep in mind that the residual weight remaining after
evaporation of SiO2 is a combination of aluminum oxide and iron (III) oxide, and put it
into the solution obtained for the determination of the ammonium hydroxide group.
c) If the evaporation yield with HF exceeds 0.002 0 gram, the determination of silica must
be repeated, steps must be taken to ensure decomposition of
the sample before
determination the separation
of (Al2O3 + Fe2O3,ofCaO
silica is carried
and MgO) isout and the subsequent
determined with a new filtrate and
the residue
obtained after adding HF has a weight of 0.002 0 gram or less, except as specified
in 7.1.3.2.1.3 point d ) and 7.1.3.2.1.3 item e).
d) If after two or three repeated determinations and it turns out that the residue obtained
after adding HF is still greater than 0.002 0 gram, it can be stated that contamination
occurred during sampling or during the time the cement manufacturing process was not
complete. In such cases the resulting precipitate should not be melted down and added
to the filtrate for the determination of the ammonium hydroxide group, but should be
reported as the precipitate obtained.
e) In this case, add 0.5 gram of sodium or potassium pyrosulfate (Na2S2O7 or K2S2O7)
into the crucible and heat it almost incandescent until the impurity precipitate melts,
cool and
dissolve with water and combine with the filtrate, and unite with the laundry stored
for determination of the ammonium group hydroxide.
f) Perform blank determination using the same reagent and test
method and take the result as a correction in the calculation.
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7.1.3.2.1.4 Calculation
Calculate the SiO2 content to the nearest 0.1%.
(w1-w2)
% SiO =
2 w X 100
Note: w1
is
the weight of the precipitate before adding HF,
grams; w2 is the weight of the precipitate after adding
HF, grams; w is the sample weight, grams.
7.1.3.2.2 Silicon dioxide with an insoluble moiety greater than 1%
This test method is based on melting sodium carbonate followed by evaporation

repeated hydrochloric acid solution until dry to change the form of silica into an insoluble form.
The solution was filtered and the insoluble silica precipitate was ignited and weighed. SiO2
was evaporated with HF, then ignited and weighed.
a) Sodium carbonate (Na2CO3).

b) Hydrochloric acid (HCl). c)
Hydrochloric acid (HCl)(1+3). d)
Hydrochloric acid (HCl)(1+99). e)
Hydrochloric acid (HCl)(1+1).
a) Weigh a number of samples that have been ignited which is equivalent to 0.5 grams of
sample as calculated according to the following formula:
W= {0.5 (100.00-HP)}
100
Information:
W is the weight of the sample ignited,
grams; HP is dissipated, %.
Material which has been ignited in the loss determination may be used as an
example. Mix the samples evenly with (4–6) grams of Na2CO3 by grinding in an
agate mortar.
Cover the base of the crucible with a thin layer of Na2CO3, add the cement- Na2CO3 mixture
on top then cover the mixture with a thin layer of Na2CO3.
Place the covered crucible over medium heat and increase the flame slowly to maximum (ÿ1
100 oC) and maintain this temperature until the mixture is quiescent ( ÿ45 min).
Remove
and the
rotate burner,
the remove
crucible slowlythe
so cover and
that the placecontents
molten it elsewhere, clamp
spread and the crucible
solidify as awith
thin tongs
layer on
the
inside of the crucible wall.
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Cool the crucible with the lid on. Rinse the outer walls of the crucible and place the crucible
in a 300 mL casserole which is one-third filled with water.
Warm the casserole and stir so that the crust in the crucible crumbles and can be removed
easily.
Using a glass stirring rod, remove crucible from casserole, rinse thoroughly with water. Rinse
the crucible and lid with HCl (1+3), the rinse water is added to the casserole.
Carefully and slowly add 20 mL HCl (bj 1.19) to the covered casserole. Remove and rinse
the cover. If there are granular particles it means that the melting is not complete and the
test must be repeated using a new sample.
Attention:
The sequence of testing steps must be followed exactly to produce precise and accurate
results.
b) Evaporate the solution until dry over a steam bath (until no lumps are seen) without further
heating the residue, add (5-10) mL HCl, let stand for at least 2 minutes, add the same
amount of water (5 mL -10 mL) .
Close the crucible and digest for 10 minutes on a steam bath or hot plate.
Dilute the solution with an equal amount of hot water, filter with medium porous filter paper
and wash the separated SiO2 with hot HCl (1+99), then with hot water, save the precipitate.
c) Evaporate the filtrate again until dry and bake the precipitate in the oven at (105-
110) oC for 1 hour, cool, add (10-15) mL HCl (1+1) and digest at
steam bath or hot plate for 10 minutes. Dilute with the same amount of water, immediately
filter with new filter paper, and wash the SiO2 precipitate as in 7.1.3.2.2.3 point b), stir the
filtrate mixture with washing water and save it for the determination of the ammonium
hydroxide group according to 7.1.3.3 the determination of the ammonium group hydroxide.
Continue the determination of SiO2 according to 7.1.3.2.1.3 point b).
7.1.3.3 Group ammonium hydroxide (R2O3)

In this method aluminum oxide, iron (III) oxide, titanium dioxide, and phosphorus
pamenmtaoonkiusmidahiddireonkdsaidpak.aAnpadbair lia fidlt ir laakt,uksaenteldaehngSainO2 lebdi ihpishaahtik-

ahnatideenndgaapnancamraanpgeannadmiobkashiadna will precipitate. The precipitate is ignited and weighed as oxide.
7.1.3.3.2 Reagents
a) Hydrochloric acid (HCl bj

1.19). b) Hydrochloric acid (HCl)
(1+2). c) Ammonium hydroxide (NH4OH)
(1+1). d) Ammonium nitrate (NH4NO3).
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7.1.3.3.3 Procedure
a) The filtrate stored in 7.1.3.2.1.3 point a) (see procedure item) with a volume of 200 mL, if
necessary, added HCl to ensure the total amount of acid in the filtrate (10-15) mL.
Add a few drops of methyl red indicator and heat to boiling.

Then drop NH4OH (1+1) until the solution is yellow, and add one drop in excess.
Heat the solution containing the precipitate to boiling and boil for (50-60) seconds.
To avoid bumping during the boiling of the solution, it can be done in another way, namely:
Digest on a hot plate which has the same temperature as a steam bath for 10 minutes.
Let the precipitate descend (no more than five minutes) and filter using medium porous filter
paper. Wash with hot ammonium nitrate solution (20 gram/L NH4NO3 ), for slightly precipitates,
wash twice, while for large precipitates, wash four times.
b) Collect the filtrate and transfer the precipitate and its filter paper into a glass
chemical originally used for precipitation.
Dissolve the precipitate with hot HCl (1+2). Stir until the filter paper disintegrates and then
dilute the solution with 100 mL of boiling water. Precipitate the hydroxide according to 7.1.3.3.3
point a). Filter the solution and wash the precipitate with (4-10) mL of hot ammonium nitrate
solution (20 gram/L NH4NO3 ).
Combine the filtrate and its washing solution with the original fitrate and save it for the
determination of CaO according to 7.1.3.9.3 point a).
c) Place the precipitate in a crucible of known weight, heat slowly until the carbon from the filter
paper is removed, and finally to prevent reduction, carefully heat it at (1 050 - 1 100) oC until
the weight remains and weigh as ammonium hydroxide group .
d) Perform a blank determination using the same reagent and method

and take the result as a correction in the calculation.
7.1.3.3.4 Calculation
Calculate the R2O3 content to the nearest 0.1%.
% R2O3 =
Sediment weight x100
Sample weight
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7.1.3.4 Iron (III) oxide (Fe2O3)
The Fe2O3 content of cement is determined from individual samples by reducing iron(III) to iron(II) with tin(II) chloride
(SnCl2) and titrating with standard potassium bichromate (K2Cr2O7) solution .
This designation is unaffected by the titanium and vanadium that may be present
in cement.
7.1.3.4.2 Reagents
a) Barium diphenilamine sulfonate indicator solution.
Dissolve 0.3 gram of barium diphenilamine sulfonate in 100 mL of water.
b) Potassium dichromate standard solution (1 mL = 0.004 gram Fe2O3)
- Graintda atenmd pderyratthuerepr(i1m8a0r-y20s0ta) nodCarudnrtiel

) NBS 136
athgeenwtepigohtat srseimumaindsic. hromate (K2Cr2O7
- Weigh carefully as much as 2.457 00 grams for 1 liter of the prepared

solution.
- Dissolve in water and dilute appropriately to the desired volume in an appropriately sized flask. This
standard solution is a primary standard solution and does not need to be determined again.
c) Tin(II) chloride solution
- Dissolve 5 grams of tin(II) chloride (SnCl2.2H2O) in 10 mL of HCl and dilute

to 100mL.
- Add iron-free lead granules and boil until the solution is in a drip
bottle covered with tin granules.
7.1.3.4.3 Procedure
For Portland cement where the insoluble portion is unknown, first determine the insoluble portion according to
the test method described in this procedure. If the insoluble portion is known, proceed according to 7.1.3.4.3
item a) or
7.1.3.4.3 item b). a) For portland cement with an insoluble fraction of less than 1%
- Weigh 1 gram of sample into a 500 mL beaker or other suitable container.
- Add 40 mL of cold water, while shaking the container add 10 mL of HCl. If necessary, heat the solution and
crush the cement with a flat-tipped glass stir bar until all the cement has dissolved completely. Continue
the analysis according to 7.1.3.4.3 point b) i).
b) For cement with an insoluble fraction content greater than 1%
- Weigh 0.500 grams of sample, mix with 1 g of LiBO2 using a mortar and pestle. Transfer it to a crucible
which, before being heated, contains 0.1 gram of LiBO2 which is spread in the bottom.
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- Cover with 0.1 gram of LiBO2 which was first used to clean the mortar and pestle. Place
the uncovered crucible in a furnace that has been set at 1 100 oC for 15 minutes.
Remove the crucible from the furnace and check the melting is complete. If it is not
completely melted, return the crucible to the furnace for 30 minutes. Double check the
perfection of melting. If melting is still incomplete, discard the sample and repeat the
melting procedure using 0.250 gram sample or a smaller amount of sample with the
same amount of LiBO2.
- When the melt is complete, shake immediately, carefully melt and pour into a 150 mL
beaker containing 10 mL HCl and 50 mL water. Stir continuously until the molten product
dissolves, usually 10 minutes or less.
- If a magnetic stirrer is used, remove and rinse the stir bar
and continue the analysis according to 7.1.3.4.3 point b) i).
i) Heat the solution to a boil and add the SnCl2 solution drop by drop while stirring
and boil until the solution is colorless.
Add one drop in excess and cool the solution to room temperature by placing the
beaker in a pan filled with cold water.
After cooling and without delay rinse the inside of the beaker walls with water,
and add 10 mL of cold saturated mercuric chloride (HgCl2) all at once.
Stir the solution rapidly for one minute by shaking the beaker and add 10 mL of
H3PO4 (1+1) and two drops of barium diphenilamine sulfonate indicator solution.
Add sufficient water until the volume after titration is between (75 -100) mL.
Titrate with a standard solution of potassium dichromate. The end point will be
shown where one drop causes a violet red color that remains on the addition of
excess K2Cr2O7 solution .
7.1.3.4.4 Blank
Perform a blank determination using the same reagent procedure.
Record the volume of K2Cr2O7 solution required to determine the end point as described in
7.1.3.4.3 point b) i).
A certain amount of iron is needed to reach the end point, if you don't see a clear violet color
after adding four drops of K2Cr2O7 standard solution , then there is no iron in the blank.
Calculate the Fe2O3 content with an accuracy of 0.01% (reported with an accuracy of 0.1%) as
follows:
% Fe2O3 = E x (VB) x 100

W
Note: E is
the
equivalent of Fe2O3 to K2Cr2O7 solution , gram/mL; V is milliliters
of K2Cr2O7 required for sampling; B is milliliters of K2Cr2O7
required for blank determination; W is the sample weight to the
nearest 0.1 milligram.
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7.1.3.5 Phosphorus pentaoxide (P2O5)
This colorimetric test method is used to determine P2O5 in portland cement. Under these test conditions, there
are usually no other elements that can interfere with the portland cement.
7.1.3.5.2 Equipment
Spectrophotometer, the instrument shall be equipped to measure the absorbance of the solution at a wavelength of
725 nm. The wavelength measurement must be repeatable within ÿ1 nm or less. In the absorbance range from 0.1
– 1.0, the absorbance measurement shall be repeatable within a tolerance of ÿ1% or less. To ensure that the
spectrophotometer can be used with a satisfactory level of accuracy, qualify the instrument according to specifications
using procedure 7.1.3.5.4.
7.1.3.5.3 Reagents
a) Ammonium molybdate solution
- Enter 500.0 mL of 10.6 N H2SO4 in a 1 liter measuring flask
- Dissolve 25.0 grams of ammonium molybdate (NH4)6Mo7O24.4H2O) in 250 mL of warm water and transfer
to a measuring flask containing H2SO4, while shaking the flask.
- Cool, dilute up to 1 liter with water, and store in a plastic bottle.
b) Ascorbic acid powder
To facilitate dissolution, use the smoothest.
c) Standard hydrochloric acid (6.5 ÿ 0.1N)
- Dilute 540 mL HCl (bj 1.19) up to 1 Liter with water.
- Standardize against standard NaOH solution 7.1.3.5.3 point f) using phenolphthalein indicator.
- Define normality precisely and set at 6.5 N ÿ 0.1 N with dilution

water.
- Re-standardize to ensure that proper normality has been achieved.
d) Standard solution of phosphate A
Dissolve 0.191 7 grams of dry potassium dihydrogen phosphate (KH2PO4) in water and dilute to 1 liter
in a measuring flask.
e) Standard solution of phosphate B
Dilute 50 mL of phosphate solution A to 500 mL with water.
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f) Standard sodium hydroxide solution (1 N)

- Dissolve 40.0 grams of sodium hydroxide (NaOH) in water, add 10 mL of freshly filtered
saturated solution of barium hydroxide (Ba(OH)2) , and dilute to 1 liter with freshly
boiled and cooled water.
- Shake the solution from time to time for several hours, and strain into a plastic bottle.
Keep the bottle tightly closed to protect the solution from CO2 in the air.
- Standardize acidimetrically against potassium phthalic acid or benzoic acid issued by

the NBS (standard sample 84 f and 350), using the test method contained in the
certificate accompanying the sample.
- Determine the normality of the solution precisely.
g) Standard sulfuric acid (10.6 N ÿ 0.1 N)

Into a 1 Liter volumetric flask cooled in water, add approximately 600 mL
wteamtepre, rtahteunrea, dddilu3t0e0tom1L lHite2rSwOit4h (wbja1te.8r.40) slowly and carefully. After

cooling to room
Standardize against standard NaOH solution 7.1.3.5.3 point f) use phenolphthalein
as indicator.
Define normality and adjust to 10.6 N ± 0.1 N with water dilution.
Restandardize to ensure that proper normality has been
achieved.
7.1.3.5.4 Procedure
a) Prepare a series of phosphate solutions of (0 -0.5)% PO.
P re p ar e e a c h b y a d di n g ap pr op r ia te v o lu m e s o f
of 6 .5 N h y d r o ch lo r ic a c id to a 2 5 0 m L m e a s ur in
st a n d a rd p h o s p ha te B s ol ut io n a n d 25.0 mL
g f la s k . Di lu t e u p to m a rk w it h w a te r.
NOTE One milliliter of standard solution of B phosphate in 250 mL of solution is equivalent to 0.004%
P2O5 gram of cement sample. A series of concentrated solutions (mother liquor) of standard
phosphate B whose volumes are: 0; 12.5; 25; 50; 74; 100 and 125 mL is equivalent to the P2O5
content in the
cement sample of 0 ; 0.05; 0.10; 0.20; 0.30; 0.40; and 0.50%.
b) Prepare a blank by adding 25.0 mL of standard HCl to a 250 mL measuring flask and
diluting to 250 mL with water. Do the coloring on the row of phosphate solutions and
blanks in accordance with 7.1.3.5.4 point e) to 7.1.3.5.4 point g) so that the color appears.
c) Plot of absorbance values (standard absorbance minus blank absorbance) obtained as

ordinate and concentration of P2O5 as abscissa. Create a curve showing the relationship
between
absorbance and P2O5 concentration.
d) Transfer 0.25 gram sample into a 250 mL beaker and moisten with 10 mL cold water to
prevent clumping. Add 25.0 mL of standard HCL and digest with moderate heating and stir
until complete solution. Filter into a 250 mL measuring flask and wash the filter paper and
the separated silica precipitate with hot water. Let the solution cool and dilute with water to
250 mL.
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e) Transfer the 50.0 mL aliquot of the sample into a 250 mL beaker, add 5.0 mL of ammonium molybdate
solution and 0.1 gram of ascorbic acid powder. Stir the contents of the beaker by shaking until the
ascorbic acid is completely dissolved. Heat the solution to a boil, remove the lid and continue boiling for
(1.5 ± 0.5) minutes.
Cool to room temperature and transfer to a 50 mL measuring flask. Rinse the beaker with a little water and
add the rinse water to the measuring flask. Dilute up to 50 mL with water.
f) Take a blank measurement at a wavelength of 725.0 nm. g) Prepare 50.0 mL aliquots
of the blank solution prepared as in the sample solution.

Measure the absorbance according to 7.1.3.5.4 item f) and subtract the absorbance value obtained for the
sample solution in 7.1.3.5.4 item e). In order to obtain the final absorbance of the sample solution.
h) Using the pure absorbance values obtained, record the percentage of P2O5 in the cement sample as
shown in the calibration curve. Report % P2O5 to the nearest 0.01.
7.1.3.6 Titanium dioxide (TiO2)
In this test method, the titanium dioxide (TiO2) in portland cement is determined colorimetrically using tyron reagent.
Under these test conditions, only iron is the element in portland cement which causes very little disturbance,
equivalent to 0.01% for every 1% Fe2O3.
7.1.3.6.2 Equipment
Spectrophotometer, the instrument shall be equipped to measure the absorbance of the solution at a wavelength of
410 nm. The wavelength measurement must be repeatable if ± 1 nm is obtained. In the absorbance range from
0.1
– 1.0, the absorbance measurement shall be repeatable within a tolerance of ÿ1% or less.
7.1.3.6.3 Reagents
a) Buffer pH 4.7 68 g
NaC2H3O2.3H2O plus 380 mL water and 100 mL CH3COOH 5 N
b) Disodium salt ethylenedinitrilo tetra acetate dihydrate (0.2 M EDTA)
- Dissolve 37.5 grams of EDTA in 350 mL of warm water and filter - Add
0.25 grams of FeCl3.6H2O and dilute to 500 mL.
c) Hydrochloric acid (1+6) d)
Standard hydrochloric acid (6.5 N)
Dilute 540 mL HCl (bj 1.19) to 1 Liter with water.
e) Ammonium hydroxide (NH4OH)( 1+1) f) Potassium
pyrosulfate
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g) Titanium dioxide, mother liquor A

- Melt slowly 0.031 4 grams of 99.74% TiO2 (NBS SRM 154b) in a crucible over a low
flame or other titan compounds as a substitute and add approximately 2 grams or 3
grams of K2S2O7.
- Let stand until cold, and crucible in a beaker containing 125 mL
H2SO4 (1+1).
- Heat and stir until the melt is completely dissolved.
- Cool, transfer to a 250 mL measuring flask, and dilute the solution to
boundary sign.
h) Titanium dioxide, aqueous standard solution B (1 mL = 0.012 5 mg TiO2)

Pipette 50 mL of mother liquor A TiO2 into a 500 mL volumetric flask, and dilute to the
mark. One mL of this solution is equal to 0.0125 mg TiO2 which is equivalent to 0.05%
TiO2 if the procedure in 7.1.3.6.4 points e) to
7.1.3.6.4 item f).
i) Sulfuric acid (1+1)
j) Tyrone (disodium-1,2-dihydrobenzen-3,5 disulphonate)
7.1.3.6.4 Procedure
a) Prepare a series of aqueous standard solutions of B TiO2 covering concentrations from 0%–1.0% TiO2.
Prepare each solution in a 50 mL measuring flask.
NOTE One mL of aqueous standard solution B TiO2 in 50 mL is equivalent to 0.05% TiO2 for
0.250 0 gram sample of cement. Solutions of 0, 5, 10, 15 and 20 mL of standard TiO solut2ion
are equivalent to the TiO2 content in sample 0; 0.25; 0.50; 0.75; and 1%. Dilute each to 25 mL
with
w a te r .
b) Ad d c h e mical reagent according to the procedure in 7.1.3.6.4 point e) until it appears
color.
c) Measure the absorbance according to 7.1.3.6.4

point f). d) Plot the absorbance value as ordinate and TiO2 concentration as abscissa. Create a
curve shows the relationship between absorbance and concentration.
e) Transfer the 25.0 mL aliquot of the sample prepared in 7.1.3.5.4 item d) (see P2O5
determination) into a 50 mL measuring flask. Add 5 mL of tyron and 5 mL of EDTA, stir
and then add dropwise NH4OH (1+1).
Stirring is carried out carefully after each drop until the color changes from yellow to green,
blue, or ruby. Then return it to a yellow color by adding drop by drop HCl (1+6) and
stirring after each drop.
Add 5 mL of buffer, dilute to volume and shake.

f) Measure the absorbance of the blank solution at a wavelength of 410
nm. g) Using the absorbance values specified in 7.1.3.6.4 point f), record the TiO2 content of
the cement sample as indicated in the calibration curve to the nearest 0.01.
Correct the presence of iron in the example to determine actual TiO2 with the
following formula: Actual TiO2 = % TiO2 measurement – (0.01 x % Fe2O3).
Report % TiO2 to the nearest 0.01.
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7.1.3.7 Zinc oxide
Each test method can be used in testing zinc oxide, provided that it is able to meet the
requirements listed in the table of differences in allowable test results (Table 6).
7.1.3.8 Aluminum oxide
Calculation:
Calculate the percentage of Al2O3 by subtracting the amount of Fe2O3, TiO2 and P2O5 from the
percentage of the ammonium hydroxide group. All determinations must be made using the referee
method as described in the points concerned. All percentages must be calculated to the nearest
0.01%. Report Al2O3 with accuracy of 0.1% for non-referee analysis, the percentages of Fe2O3, TiO2
and P2O5 can be determined by any procedure whose qualifications have been demonstrated.
7.1.3.9 Calcium oxide (CaO)

In this test method, manganese is removed from the filtrate after the determination of SiO2 and the
ammonium hydroxide group. Then calcium oxide is precipitated as oxalate. After filtering, redissolve
the oxalate and titrate with potassium permanganate (KMnO4).
NOTE For the referee test method or for determination with high accuracy, the separation of
manganese according to 7.1.3.9.3 point b). For determinations with low accuracy, and if only the
amount of manganese oxide is insignificant then point b) may be ignored in 7.1.3.9.3.
Strontium is usually present in Portland cement as a minor element, and is precipitated together
with calcium as oxalate and then titrated and calculated as CaO.
If the SrO level is known and a correction of CaO to SrO is desired, for example, for research
purposes or to compare results with SRM certified values, the CaO determined by this method may
be corrected for SrO.
In the determination to comply with cement specifications, the correction of CaO to SrO does not
have to be done.
7.1.3.9.2 Reagents
a) Ammonium acetate solution (50 gram/L) b)

Potassium permanganate standard solution (0.18 N).
- prepare a solution of potassium permanganate (KMnO4) containing 5.69 gram/L.
- Leave this solution at room temperature for at least one week,
or bring to a boil and cool to room temperature.
- Transfer the clear solution without disturbing the sediment at the bottom of the bottle; then filter
the solution that has been separated earlier through a funnel that is given a glass wool
bottom or through a glass filter.
- Do not filter through materials containing organic matter.
- Sbaimgipaannludaarnlayma. dark colored bottles, preferably bottles that have been painted black on
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- Standardize against (0.700 0 - 0.800 0) grams of primary standard sodium oxalate, according to the
standard sodium oxalate instructions, and record the temperature at the time the standardization
was carried out (see NOTES).
- Calculate the CaO equivalence of the solution as follows:
1 mL of 1N KMnO4 solution is equivalent to 0.067.01 gram of pure sodium oxalate.
Weight of Na oxalate x fraction of purity

KMnO4 normality =
mL of KMnO4 solution x 0.067 01
1 mL of 1N KMnO4 solution is equivalent to 0.028 04 grams of CaO.
F=
Normality of KMnO4 x 0.028 04 x 100 solution
0.5
Information:
F is the equivalence of CaO to KMnO4 solution in % CaO/mL
based in 0.5 gram of cement sample.
NOTE Since the KMnO4 solution is unstable, this solution is restandardized at least once
every two months.
7.1.3.9.3 Procedure
a) Acidify the combined filtrate determined by the precipitation of the ammonium group
hydroxide 7.1.3.3.3 point b).
Neutralize with HCl until the color of the methyl red end point is reached, add 6 drops of excess HCl
to make it really acidic.
b) Separation of manganese
- Evaporate until the volume is ÿ100 mL.

- Add 40 mL of saturated bromine water to the hot solution and add NH4OH immediately until the
solution is alkaline.
- The addition of 10 mL of NH4OH is generally sufficient.
- A piece of filter paper approximately 1 cm wide is pla2c,ed in a beaker and pressed down with the
help of the tip of the stirring rod to prevent bumping and precipitating of manganese oxide
hydrate (MnO).
- Boil the solution for 5 minutes or more, make sure the solution is completely lye
at all times.
- Let the sediment down, filter using medium porous filter paper, and wash with hot water.
- If the precipitate does not appear immediately, allow the settling time to one hour
before filter.
- Separate any manganese dioxide that has precipitated. Acidify the filtrate with HCl using litmus
paper as indicator and boil until the bromine has evaporated (NOTE 1).
NOTE 1 Potassium iodide starch paper can be used to demonstrate the complete
evaporation of excess bromine. Apply damp paper to the boiling solution vapors. The
paper should not change color, and if the paper turns blue the bromine is still present.
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c) Add 5 mL HCl, dilute to 200 mL and add a few drops of methyl red indicator and 30 mL
of warm ammonium oxalate solution (50 gram/L)
(NOTE 2). Heat the solution to (70-80) oC and add NH4OH (1+1) drop by drop,
while stirring until the color changes from red to yellow.
h
(noOt TmEo3re).),Lweiathveocthceassionuatilosntirwriinthgofuotrhtheeatfinirgstm30orme inutesc.ontinue

for (60 ÿ 5) minutes
NOTE 2 If the ammonium oxalate solution is not clear, it should be filtered before use.
NOTE 3 This neutralization must be carried out slowly, otherwise precipitated calcium
oxalate tends to pass through the filter paper. If a number of these determinations are made
simultaneously the following technique can help to ensure gradual neutralization. Add 2 or 3
drops of NH4OH to the first beaker while stirring, then 2 or 3 drops to the second beaker, and
so on, return to the first beaker with the addition of 2 or 3 drops again until the color of the
indicator in each beaker changes.
d) Filter using fine filter paper, and wash the precipitate 8 to 10 times with hot water, the
total amount of water used in rinsing the beaker and washing should not be more than
75 mL. During this washing, the water from the washing bottle must go straight to the
inside of the filter paper, until the precipitate drops, then spray the water slowly directly
towards the center of the filter paper so that the precipitate is thoroughly mixed and
washed. Acidify the filtrate with HCl and save for determination of MgO.
e) Place the beaker under the funnel containing the precipitate, pierce the top of the filter
paper cone with the stirring rod, place the stirring rod in the beaker, and wash the
precipitate into the beaker and wash the precipitate into the beaker
bW y a us sh i nthgehfoilttewraptaepr.eDr r5optimÿ1e0s wdriothpshootf wHa2tSerO. 4 (1+1) around
p a p e r.
the top edge of the filter
Dilute to 200 mL, and add 10 mL H2SO4 (1+1). Heat the solution to a temperature
close to the boiling point, and immediately titrate with 0.18 N KMnO4 solution
(NOTE 4).
NOTE 4 Since the KMnO4 solution is unstable, this solution is restandardized at least
once every two months.
Continue the titration slowly until a precise pink color persists for at least 10 seconds.
A d d t h e fi l t e r p a pe r c o n t ain in g th p r e c ip it at e
co n ti n u e t i t ra t io n u n ti l t h e co lo r per s is t s fo r a t
a n d s o ak it. If n o pink color appears,
le a st 1 0 se co n d s.
NOTE 5 The temperature of the 0.18 N KMnO4 solution as penetration shall not vary from
the standard temperature by more than 5.5 oC. Larger deviations can lead to serious errors
in the determination of CaO.
7.1.3.9.4 Blank
Make a blank determination using the same procedure and using the same amount
of reagent and record milliliters of KMnO4 required for determination of the end point.
NOTE When the amount of calcium oxalate is very small, oxidation by KMnO4 is
slow. Before titration add a little MnSO4 into the solution as a catalyst.
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Calculate the percentage of CaO with an accuracy of 0.1 as follows:
% CaO = E (VB)
Information
:
E is the CaO equivalent to the KMnO4 solution in % CaO/mL based on 0.5 gram
example;
V is the KMnO4 solution required by the sample, mL; B is the
KMnO4 solution required by the blank, mL.
If necessary, correct the percentage of CaO to SrO as follows:
% CaOc = % CaOi – 0.54 %SrO
Note: CaOc =
corrected CaO; CaOi =
CaO obtained from 7.1.3.9.5
0.54 = ratio of molecular weight of CaO to SrO ÿ ÿÿ,ÿ ÿÿÿ,ÿÿÿ
7.1.3.10 Magnesium oxide (MgO)
In this test method, magnesium is precipitated as magnesium ammonium phosphate from the
filtrate after removing the calcium. The precipitate was ignited and weighed as ammonium
pyrophosphate (Mg2P2O7). The MgO equivalent was then calculated.
7.1.3.10.2 Reagents
Dibasic ammonium phosphate (100 g/L) (NH4)2HPO4.
7.1.3.10.3 Procedure
- Acidify the filtrate from the determination of CaO 7.1.3.9.3 point d) with HCl and evaporate by
boiling to approximately 250 mL.
- Cool the solution to room temperature, add 10 mL dibasic ammonium phosphate ((NH4)2HPO4)
(100 g/L) and 30 mL NH4OH.
- Stir the solution vigorously while adding NH4OH and then extend the stirring time 10 minutes
-15 minutes.
- Leave the solution for at least 8 hours at air temperature.
- Wash the residue 5 or 6 times with NH4OH (1+20) and ignite in a crucible or porcelain cup of
known weight, first heat slowly until the filter paper turns into charcoal and then burn, and
finally ignite at 1 100 oC for 30 minutes – 45 minutes.
NOTE Work must be done with care during this boiling. Phosphate deposits can be reduced in contact
with carbon at high temperatures. There is a dangerous possibility of carbon trapping by deposits in the
too fast annealing process.
- Weigh the residue as magnesium pyrophosphate (Mg2P2O7).
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7.1.3.10.4 Blank Make

a blank determination using the same procedure and using the same number of reagents, and correct
the results obtained in the analysis.
Calculate the percentage of MgO with an accuracy of 0.1 as follows:
% MgO = W x 72.4
Note: W is
grams of Mg2P2O7; is the
used Mg2P2O7 (0.362) divided by the sample weight of 72.4
(0.5mgorlaemcusl)armrualttiioploief
d2bMyg1O00to.
NOTE Work must be done with care during this boiling. Phosphate deposits can be reduced in
contact with carbon at high temperatures. There is a dangerous possibility of being trapped
carbon by deposits in the too-rapid heating process.

7.1.3.11 Sulfur
7.1.3.11.1 Sulfur trioxide
In this test method sulfate is precipitated from an acidic solution of cement with barium chloride (BaCl2).
The precipitate was ignited and weighed as barium sulfate (BaSO4) and the SO3 equivalence was
calculated.
a) In 1 gram of sample, add 25 mL of cold water, while stirring vigorously

and add 5 mL HCl.
NOTE 1 The filtrate of acid resulting in the determination of an insoluble residue of 7.1.3.1.3
may be used for the determination of SO3 unless another example is used.
b) If necessary, heat the solution and crush the sample with the end of the stirring rod
flat-tipped glass until the cement completely decomposes.
NOTE 2 The brown residue of the manganese component is negligible.
c) Dilute the solution to 50 mL and digest for 15 minutes at almost boiling temperature. Filter through
medium porous filter paper and wash off the residue with hot water.
d) Dilute the filtrate to 250 mL and heat to a boil. e) Add slowly drop by drop
10 mL of hot BaCl2 (100 gram/L) and continue boiling until a precipitate forms completely. Digest the
solution for (12-24) hours at almost boiling temperature.
NOTE 3 If the determination of the fast method is desired, the digest time can be accelerated to
a minimum of 3 hours. Nevertheless cement can be rejected because it meets the
specification requirements, only based on the results obtained when using digest time (12-24)
hours.
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f) Keep the solution volume between (225-260) mL and add water if necessary. Filter through
fine porous filter paper, wash the precipitate with hot water, place the filter paper and
contents in a crucible that has been weighed. Heat at (800-900) oC, cool in a desiccator
and weigh.
NOTE 4 When the instrumented test method is used for sulfur or when comparing the results
of wet analysis and the instrument test method is less than 0.05%.
7.1.3.11.1.3 Blank
Make a blank determination using the same procedure and using the same amount of reagent,
and correct the results obtained in the analysis.
Calculate the percentage of SO3 with an accuracy of 0.01 as follows:
% SO3 = W x 34.3
Note: W is
the gram of BaSO4 to the sample; 34.3 is
the ratio of SO3 molecules to BaSO4 (0.343) multiplied by 100.
7.1.3.11.2 Sulfides

In this test method, sulfur sulfide is determined by converting slowly as hydrogen sulfide (H2S)
from an acidic solution of cement in a solution of ammoniacal zinc sulfate (ZnSO4) or ammoniacal
cadmium chloride (CdCl2).
Sulfur sulfide is titrated with standard potassium iodate (KIO3) solution. Sulfites, thiosulfates and
other compounds including sulfides and sulfates are considered absent.
If the compound is present, it can cause errors in the determination.
7.1.3.11.2.2 Equipment
Gas generator flask.

Connect the 500 mL dry boiling flask to the long-stemmed separatory funnel through the rubber
bulb cap. The bent separatory funnel stalk is adjusted so that it does not interfere
cfloanskn,eccotinngebcut ltbh,ethseepeanrdatoofrythfeunsneeplatroattohrey afuirncnoeml
sptraelkssisord. ipped to the bottom of the boiling Connect the bulb with an L-shaped glass
pipe and a 200 mm long straight glass pipe.

Put the straight glass into a tall 400 mL beaker. The three-necked distillation flask with a long
gas cylinder is positioned between the compressor and the separatory funnel and is an excellent
aid in regulating airflow.
The rubber used in this equipment must be of high purity, with a low sulfur content and must be
washed with warm HCl.
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7.1.3.11.2.3 Reagents
a) Ammoniacal cadmium chloride solution

Dissolve 15 g of cadmium chloride (CdCl2.2H2O) in 150 mL of water and 350 mL of NH4OH.
b) Ammoniacal zinc sulfate solution
Dissolve 50 grams of zinc sulfate (ZnSO4.7H2O) in 150 mL of water and 350 mL of
NH4OH. Filter the solution after letting it stand for at least 24 hours.
c) Standard solution of potassium iodate (0.03 N)
- Prepare a solution of potassium iodate (KIO3) and potassium iodide (KI) as follows: -
Heat KIO3 at 180 oC to constant weight. Weigh 1.070 1 gram KIO3
and 12 grams of KI.
- Dissolve and dilute up to 1 Liter in a measuring flask.
- This primary standard solution does not need to be standardized.

- One milliliter of this solution is equivalent to 0.000 480 9 grams of sulfur.
NOTE This solution is very stable, but must be re-standardized before each use. Solutions that
are one year old must be discarded or the concentration standardized again.
d) Tin(II) chloride solution
To a small flask containing 10 grams of tin(II) chloride (SnCl2.2H2O), add 7 mL of HCl (1+1),
warm the mixture carefully until this salt dissolves, cool the solution, and add 95 mL of water.
This solution must be prepared when needed, as these salts tend

hydrolyzed.
e) Starch solution
To 100 mL of boiling water, add a cold suspension of 1 gram of starch solution in 5 mL of
water and cool. Add a cold solution of 1 gram of sodium hydroxide (NaOH) in 10 mL of water,
then 3 grams of potassium iodide (KI), and stir vigorously.
a) Place 15 mL of ammoniacal ZnSO4 solution or ammoniacal CdCl2 solution (NOTE 2) and 10 mL

of water into the flask and shake wet and disperse the cement until perfect.
b) This step and the addition of SnCl2 must be done quickly to

prevent cement setting.
c) Connect the flask with the funnel and bulb. Add 25 mL of SnCl2 solution through the funnel and
shake the flask. During shaking, keep the funnel closed and the dispense tube in the
ammoniacal ZnSO4 or ammoniacal CdCl2 solution.
d) Connect the mouthpiece to the compressed air source, open the mouthpiece, start circulating
air slowly bring to a boil.
e) Continue boiling carefully for 5 or 6 minutes.
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f) Stop heating and continue airflow for 3 or 4 minutes. g) Remove the

dispensing tube and leave it in solution for use as
stirrer.
h) Cool the solution to a temperature of (20-30) oC (NOTE 3), add 2 mL of starch
solution and 40 mL of HCl (1+1) and immediately titrate with 0.03 N KIO3 solution
until a blue color is not lost ( NOTE 4).
NOTE 1 In general, ZnSO4 is better than CdCl2 because ZnSO4 is more soluble in NH4OH
than CdCl2. CdCl2 solution can be used if there is doubt about the presence of trace amounts of
sulfur sulfide, because the yellow color of cadmium sulfide (CdS) can detect these trace
amounts.
NOTE 2 If the sulfur content exceeds 0.2 or 0.25%, a small sample must be used so that
the titration with KIO3 solution does not exceed 25 mL.
NOTE 3 Cooling is very important because the end points are different in warm solutions.
NOTE 4 This solution is very stable, but must be standardized again each time it is used.
Solutions that are one year old must be discarded or the concentration standardized again.
NOTE 5 If the sulfur content is sufficient but cannot be estimated in advance, the results
obtained may be lower than they should be due to loss of H2S during the slow titration. In this
case the determination must be repeated with the titration done even faster. Perform a blank
determination using the same procedure and using the same reagent, record the volume of
KIO3 solution required to determine the end point as described in 7.1.3.11.2.4.
Calculate the percentage of sulfur sulfide (see 7.1.3.11.2) as follows:
% sulfide = E(VB) x 20
Note: E is
the equivalent of sulfide to KIO3 solution V is the ;
KIO3 solution required by the sample, mL ; B is the KIO3
solution required by the blank, mL 20 = 100 divided by
the weight of the sample used (5 grams).
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7.1.3.12 Loss of glow
7.1.3.12.1 Portland cement
In this test method, the cement is fired in a heating furnace at a predetermined temperature.
The missing portion is assumed to represent the amount of water and CO2 in the cement.
This procedure is not suitable for determining the loss of fire from portland blast-furnace
slag cement and slag cement.
Weigh 1 gram of sample in a crucible of known weight. Close and heat the crucible and its
contents to a constant weight in a heating furnace at (950 ÿ 50) oC. Allow at least 15
minutes for preheat time and at least 5
minutes for each subsequent time period.
Calculate the percentage loss of glow to the nearest 0.1 by multiplying the weight lost in
grams by 100.
%HP= W1-W2 x100

W1
Information:
W1 is the initial sample weight;
W2 is the residual sample
weight.
7.1.3.12.2 Blast-furnace portland slag cement and slag cement
This test method provides correction for the weight gain due to oxidation of sulfides
which normally occurs in portland slag blast-furnace cement and slag cement by
determining the increase in SO3 content during firing.
a) Weigh 1 gram of sample in a fixed platinum crucible and ignite in a furnace and ignite in
an electric furnace at (950 ± 50) oC for 15 minutes.
Cool in a desiccator at room temperature and weigh. Without having to be constant,
carefully transfer the material into a 400 mL beaker. Break up the lumps in the cement
with a flat-tipped stirring rod.
b) Determine SO3 content using method 7.1.3.11.1.1 to 7.1.3.11.1.4. Also determine the
SO3 content of the same unsanded cement, using the same procedure
same.
C a l c ul a t e t h e p rc n t a g e o f w e i g h t l o s s t h
iR ne tp h oe r tp te h rec e cn otra rgeec teodf S p Oe r3 cef rn ot ma gt eh e a ss a thm e pg le l
a t o cc u r s d u r ing h e a t in g a n d ad d 0 . 8 x t h e d iff e rence
o twh a lot sh sa sr ab te .e n he a t e d a n d t he o rig i n a l c e m e n t .
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7.1.3.13 Sodium and potassium oxides
7.1.3.13.1 Alkali total
This test method covers the determination of sodium oxide (Na2O) and potassium oxide (K2O) by flame photometry
or atomic absorption spectrophotometry.
NOTE This test method is suitable for hydraulic cements that are completely decomposed by HCl and
should not be used for the determination of total alkalinity in hydraulic cements containing highly acid-
insoluble materials, such as pozzolanic cements. However, it can be used for the determination of
acid- soluble alkalis only for the cement.
All types of flame photometers or atomic absorption spectrophotometers can be used as long as the level of accuracy
and precision is within specifications.
NOTE For routine testing in the laboratory, it is recommended that instrument accuracy checks be
carried out routinely, either using NBS (National Bureau of Standards) standard cement or
cement with known alkali content.
7.1.3.13.1.3 Reagents and materials
a) Laboratory containers
All containers must be made of boron silicate glass and polyethylene containers must comply with the
requirements in accordance with 7.1.2.1.1 item (2).
b) Calcium carbonate
The calcium carbonate used in the preparation of the calcium chloride standard solution shall not have greater
than 0.020% total alkali as sulfate.
NOTE Materials sold as primary raw materials or “low alkaline” ACS usually meet this
requirement. However, the buyer must be sure that the materials used are actually as required.
c) Calcium chloride (KCl) d)
Sodium chloride (NaCl) e)
Solutions on the market can be used as a substitute for these solutions under
this.
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7.1.3.13.1.4 Solution preparation
a) Calcium chloride mother liquor

Add 300 mL of water to 112.5 grams of CaCO3 in 1 500 mL beaker.
While stirring, slowly add 500 mL HCl. Cool the solution to room temperature, filter into a 1 Liter
measuring flask, dilute to 1 Liter and shake thoroughly.
This mother liquor is equivalent to 63 000 ppm (6.3%) CaO.
b) Sodium-potassium chloride mother liquor
Dissolve 1.885 8 grams of sodium chloride (NaCl) and 1.583 grams of potassium chloride (KCl) in
water (both dried at (105-110) OC for several hours before weighing). Dilute to 1 Liter in a measuring
flask and shake well. This mother liquor is equivalent to 1 000 ppm (0.10%) each for Na2O and K2O.
Separate solutions of Na2O and K2O can be used as long as the solution has the same concentration
for both calibration and semen analysis. c) Standard solution Prepare the standard solution required
for the instrument method used. Measure the required volume of the NaCl – KCl mother liquor using a
calibrated pipette or pipette. Calcium chloride mother liquor, if required, can be measured with an
adequate measuring cup. If the instrument used requires an internal standard, measure the standard
solution with a pipette or burette. Place each solution in a measuring flask, dilute to the mark, and
shake thoroughly.
If a more dilute solution is required in this method, pipet the required diluted solution into an
appropriately sized measuring flask, if necessary add the internal standard solution, dilute to the mark,
and shake thoroughly.
7.1.3.13.1.5 Equipment calibration
According to the manufacturer's operating instructions.
(1) Cement solution

Prepare the cement solution according to the manufacturer's specific procedures. If there is no special
procedure, or if needed, do it according to the steps in 7.1.3.13.1.6 point (1) a) or 7.1.3.13.1.6 point (1) b).
NOTE The presence of SiO2 in solution affects the accuracy of some flame photometers.
In this
use case theseparated
a solution instrument
byfails to .provide
SiO2 results
Separation with the
method desiredto
according level
the of accuracy,
method thea)test
below. must
Place
(1.000 ±
0.001) gram of cement into a 150 mL beaker and disperse it with 20 mL of water by shaking the
beaker, while shaking, add 5.0 mL HCl at once. Dilute immediately to 50 mL with water. Crush
lumps of undispersed cement with a flat-end stir bar. Digest on a steam bath or hot plate for
15 minutes, then filter with medium porous filter paper into a 100 mL measuring flask. Wash
the beaker and paper with hot water, cool the measuring flask to room temperature, dilute
to 100 mL, shake the solution thoroughly.
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b) Place (1.000 ± 0.001) gram of cement into a platinum evaporating cup and disperse it with 10
mL of water by shaking. While shaking, add 5.0 mL HCl at a time. Crush lumps with a flat-end
stir bar and heat on a steam bath, until dry. Make sure that the gelatin does not form
anymore. Treat the residue with 2.5 mL HCl and approx. 20 mL water. Digest on a steam
bath for 5 – 10 minutes and immediately filter through a 9 cm diameter filter paper into a 100
mL measuring
flask.
Wash thoroughly by washing again with a certain amount of hot water until the total volume of
the solution becomes 80 mL – 95 mL. Cool to room temperature, dilute to mark, and whisk
thoroughly. If it has been found that separation of SiO2 is required to obtain the desired
accuracy for a particular flame photometer, SiO2 should always be separated if analysis is to
be used as a basis for rejection as not meeting the requirements, or if it is doubtful that it
meets specifications. Where specified, analysis is carried out with this instrument without
separation of SiO2, provided that the deviation from the certificated value obtained from the
tests carried out, shall not be two times greater than the indicated limit.
c) If the test method used requires a more dilute solution, internal standard or both, make the
same dilution as in 7.1.3.13.1.4 item c).
The standard solution and the sample solution to be analyzed shall be prepared in the same
manner and at the same dilutions as the cement standard solution being analyzed
for instrument qualification.
(2) Procedure for Na2O (NOTE 1)
Heat and set the instrument for Na2O determination as described in 7.1.3.13.1.5.
Immediately make instrument settings, atomize the cement solution and record the scale
reading (NOTE 2). Select a number of standard solutions whose distribution of Na2O levels
is close to the Na2O levels in the cement solution and take transmittance readings for each
solution.
Its value must be the same as that previously set at the time of calibration of the equipment.
If not, the equipment is recalibrated for the element. Finally, search the unknown solution
until the reading is within one transmission or meter scale corresponding to the standard
solution, or within 0.01 weight percent for instruments equipped with a digital readout
device, and the reading for the standard is the same as the calibration value. Record the
average of the two final readings obtained for the unknown solution.
NOTE 1 The determination of water-soluble alkalis shall not be considered as a substitute for the
determination of total alkali according to 7.1.3.13.1.2 to 7.1.3.13.1.7. Moreover, in this method it is
not assumed that all the alkali present in the cement is soluble. This procedure is very important to
follow carefully because there is a limit to the amount of water-soluble alkali or when to compare the
amount
of cement with the amount of cement based on the level of water-soluble alkali.
NOTE 2 The order in determining Na2O or K2O is optimal. However, the determination must be made
immediately after the tool is set and ready to be used for that purpose. If the reading exceeds the
maximum scale, do one thing, namely transfer 50 mL of the diluted solution as prepared in 7.1.3.13.1.6
point (1) into a 100 mL beaker or if desired, prepare a new solution using 0.500 grams of cement and
2, 5 mL HCl on initial addition of acid. In case silica has been separated from 0.5 gram of cement
sample, treat this dehydrated cement with 1.25 mL HCl and approximately 20 mL water, then digest,
filter and wash. For both of the above, add 5.0 mL of calcium chloride mother liquor before diluting to
the mark with water. If further dilution is required as specified in 7.1.3.13.1.4 point c) in this test
method. Set the alkaline level of this solution according to 7.1.3.13.1.6 point (2). and multiply by a
factor of 2 to calculate the percentage of alkaline oxide.
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(3) Procedure for K2O
For the determination of K2O , repeat the procedure as described in 7.1.3.13.1.6 point
(2). For instruments that can read both NaO and KO simultaneously, the K2O
determination is
2
carried out at the same time as the Na2O determination. 2
7.1.3.13.1.7 Calculations and reports
From recording averages of Na2O and K2O in unknown samples, report each oxide to
the nearest 0.01%.
7.1.3.13.2 Water-soluble alkalis
NOTE The determination of water-soluble alkalis shall not be considered as a substitute for the
determination of total alkali according to 7.1.3.13.1.2 to 7.1.3.13.1.7. Moreover, in this method it is not
assumed that all the alkali present in the cement is soluble. This procedure is very important to follow
carefully because there is a limit to the amount of water-soluble alkali or when to compare the
amount of cement with the amount of cement based on the level of water-soluble alkali.
a) Weigh 25.0 grams of the sample into a 500 mL Erlenmeyer flask and add 250 mL of
water. Cover the flask with a rubber stopper and shake thoroughly for 10 minutes at
room temperature. Filter through a Buchner funnel fitted with a holder for dry filter
paper, into a 500 mL filter flask, using a weak vacuum. Do not wash.
b) Transfer 50 mL of the diluted solution from the filtrate into a 100 mL measuring flask
and acidify with 0.5 mL HCl (specific gravity 1.19). Add 9.0 mL of CaCl2 mother
liquor (63
000 ppm CaO), as described in 7.1.3.13.1.4 point a), to a 100 mL flask, dilute the
solution to 100 mL. If this test method requires a more dilute solution, internal
standard or both, apply the same dilution as in 7.1.3.13.1.4 c).
NOTE The diluted solution of the filtrate taken for analysis must be based on an
estimate of the water-soluble alkali content. If the estimated content of K2O or Na2O is
more than 0.08% by weight of cement, or if the level of water-soluble alkali is not
known, 50 mL of the diluted solution given in 7.1.3.13.2.1 item .b) add 1 mL HCl and
vaporize on a hot plate in a 250 mL beaker to approximately 70 mL.
A d d 8 m L o f C a C l2 m ot h e r li q u o r a n d tr a n s fe r th e s a m
tboe 1a 0k e0r mw Lit. h a s m a ll am o u n t o f d i s til le d w a t e r. C o ol t h e
p l e to a 1 0 0 m L m e as u r i n g fl as k , ri n s e the
s o lu tio n t o ro o m te m p e r a t ur e a n d d i lu te
c) Determine the levels of Na2O and K2O from this solution as described in 7.1.3.13.1.6 point
(2) and 7.1.3.13.1.6 point (3). Record the ppm of each alkali in the solution
contained in the 100 mL flask.
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Calculate the percentage of total alkali that dissolves in water, expressed as Na2O, to the nearest
0.01. The total alkali which dissolves in water, is expressed as follows:
Na2O = A + E
A = B (V x 10)
C = D/(V x 10)
E = C x 0.658
Note: A is
the level of sodium oxide solution in water (Na2O), %; V is
the volume of the original filtrate in the 100.mL flask; B is
the
concentration of Na2O in the solution contained in the 100 mL flask, ppm; C is
the content of water-soluble potassium oxide (K2O), %; D is the concentration of
K2O
in the solution contained in the 100 mL flask, ppm; E is the equivalent Na2O
content in the flask.
7.1.3.14 Manganese oxide
In this test procedure manganese oxide is determined volumetrically by titration of sodium arsenite
solution after the manganese in cement is oxidized with sodium metabismutat (NaBiO3).
7.1.3.14.2 Reagents
a) Standard solution of sodium arsenite (1 mL = 0.000 3 gram Mn2O3)

Dissolve into 100 mL of water 3.0 grams of sodium carbonate (Na2CO3) and then add 0.90
grams of arsenic trioxide (AS2O3) heat the mixture until it dissolves as completely as possible. If
the solution is not clear or contains residue, filter the solution.
Cool to room temperature, transfer to a measuring flask and dilute to 1 liter volume.
Dissolve 0.58 grams of potassium permanganate (KMnO4) in 1 liter of water and standardize
against 0.03 grams of sodium oxalate (Na2C2O4) oxidimetric standard issued by the National
Bureau of Standards (Sample Standard No. 40 or its substitute) according to the instructions on
the label sodium oxalate.
Place 30.0 mL of KMnO4 solution into a 250 mL Erlenmeyer flask, then add 60 mL of HNO3 (1 +
4) and 10 mL of sodium nitrite (NaNO2, 50 gram/L).
Boil the solution until all the HNO2 has evaporated. Cool the solution, add NaBiO3 and finally
titrate with the standard solution of sodium arsenite (NaAsO2) as described in 7.1.3.14.3 item b).
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Calculate the manganese oxide (Mn2O3) equivalent to the NaAsO2 solution, in grams/mL,
as follows:
E = ( A x 7.08 ) / BC
Note: E is
the equivalence of Mn2O3 and NaAsO2 solution, gram/mL; A is
the grams of Na2C2O4 used; B is milliliters of KMnO4 solution
required by Na2C2O4; C is milliliters of NaAsO2 solution required
by 30.0 mL of KMnO4 solution; 7.08 is the molecular ratio of Mn2O3 to
5Na2C2O4 (0.236) multiplied by 30.0 mL of KMnO4 solution.
b) Sodium metabismutat (NaBiO3)

c) Sodium nitrite solution (NaNO2 50 gram/L)
a) Weigh (1.0-3.0) gram sample (NOTE 1) put into a 250 mL beaker and add (5-10) mL of
water, then with (60-75) mL of HNO3 (1+4). Boil the mixture until a complete solution is
formed.
Add 10 mL of NaNO2 solution (50 gram/L) to the above solution and boil until all the
nitrous acid has evaporated (NOTE 2), being careful not to let the volume of the solution
decrease so that it causes SiO2 to precipitate in the form of gelatin . If some of the SiO2
separates, it may be negligible, but if there is a red or brown residue, use more NaNO2
solution (50 g/L) to complete the decomposition, and then boil again to
remove nitrous
Erlenmeyer flaskacid.
and Filter
washthe
the solution through
filter paper medium porous filter paper into a 250 mL
with water.
NOTE 1 The amount of cement used for analysis depends on the Manganese content,
varying from 1 gram for ± 1% Mn2O3 to 3 grams for 0.25% Mn2O3 or less.
NOTE 2 When NaNO2 is added the evaporation of HNO2 with boiling must be
complete. If there is manganese in the cement, a small amount of NaBiO3 will give a
purple color.
b) The solution must have a volume of (100-125) mL. Cool down to room temperature.
Into the solution add NaBiO3 little by little until the total amount is 0.5 gram, while shaking
occasionally.
After the addition is complete, shake the solution intermittently for 5 minutes and then add
50 mL of cold HNO3 (1 ± 33) which has been previously boiled to remove the nitrous acid.
Filter the solution through a Gooch dish that has been coated with asbestos or carbon or
a glass filter with the help of suction. Wash the residue 4 times with cold HNO3(1+33).
Immediately titrate the filtrate with standard NaAsO2 solution.
The end point is reached when a yellow color is formed which is free from brown or violet
color and does not change with the addition of excess NaAsO2 solution.
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7.1.3.14.4 Blank
Make a blank determination, following the procedure and the same amount of reagent, correct
Calculate the percentage of Mn2O3 to the nearest 0.01 as follows:
% Mn2O3 = (EV/S) x 100
Note: E is
the equivalent of Mn2O3 to gram/mL NaAsO2 solution ; V is
the milliliters of NaAsO2 solution required for the sample; S is
the gram of sample used.
7.1.3.15 Chloride
In this test method the total chloride content in portland cement is determined by potentiometric
titration with silver nitrate. This procedure can also be used for hardened concrete, slag, and
Portland cement raw mix. In this test condition, there are no disturbing elements.
NOTE Insoluble silver salts or silver complexes stable in acidic solutions will interfere with
potentiometric measurements, the presence of iodides and bromides may interfere but fluorides do not,
sulfide salts
at concentration levels normally present in the substance will not interfere because decomposed
by acid treatment.
7.1.3.15.2 Equipment
a) Ion selective/chloride electrodes, silver/sulfide selective ion electrodes, or electrode rods

coated with silver chloride, using a suitable reference electrode.
NOTE Suitable electrodes can be obtained from Orion Beckman Instruments, Leeds and
Northup. After carefully studying the manufacturer's instructions fill in the electrode filler solution.
The silver electrode rod must be electrolytically coated with a thin layer of AgCl. To coat the
electrodes, dip a clean silver electrode rod into a saturated solution of potassium chloride (± 40
g/L) in water and apply an electric current from the dry cell through the electrode with a voltage of
1.5 V–6 V. The carbon rod from the dry cell or other electrode which is suitable is connected to
the end of the
negative pole and immersed in the solution so that the electric circuit is perfect. If the silver
chloride electrode coating is worn, renew the electrode by repeating the above procedure. All
old
silver chloride should be separated from the silver electrode rod by gentle rubbing with
fine sandpaper followed by rinsing the electrode rod with water.
b) Potentiometers with a millivolt scale that can be read to 1 mV or more accurately potentiometers
equipped with digital reading devices, but not required.
c) Class A burette, capacity of 10 mL with a scale division of 0.05 mL. A potentiometric type
burette, equipped with a drip control, is preferable, but not required.
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7.1.3.15.3 Reagents
a) Sodium chloride (NaCl), primary standard grade. (check the numbering (numbers) first, what are the letters)
before)
b) Silver nitrate (AgNO3), reagent grade. c)

Potassium chloride (KCl), reagent grade (which is required specifically for the electrode
rod silver).
d) Preparation of solution
(1) Standard sodium chloride solution (0.05 N NaCl)
- Dry sodium chloride (NaCl) at 105 oC -110 oC until heavy

permanent.
- Weigh 2.922 2 grams of dry NaCl.
- Dissolve in water and dilute to exactly 1 Liter in a measuring flask and shake well. This
solution is standard and does not need to be standardized further.
(2) Silver nitrate standard solution ( 0.05 N AgNO3)
- Dissolve 8.493 8 grams of silver nitrate (AgNO3) in water.
- Dilute up to 1 Liter in a measuring flask and shake well.
- Standardize against 5.00 mL of 0.05 N sodium chloride standard solution which has been
diluted to 150 mL with water followed by the titration test method given in 7.1.3.15.4 point
d) starting with the sentence "Place the beaker on a magnetic stirrer etc.
- The exact normality should be calculated from the average of three assignments as
following:
0.25
N=
V
Note: N is
the normality of the AgNO3 solution;
0.25 is the milli equivalent of NaCl (5.0 mL x
0.05 N); V is the volume of AgNO3 solution, mL.
Standard solutions on the market may be used as long as the normality is checked
according to standard procedures.
(3) Methyl orange indicator

Prepare a solution containing 2 grams of methyl orange in 1 liter of 95% ethyl alcohol.
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a) Weigh 5.0 grams of cement or 10.0 grams of concrete sample into a 250 mL
beaker (NOTE 1).
Disperse the sample with 75 mL of water. Without delay add slowly 25 mL of HNO3 (1 +
1), breaking up any lumps with a stirring rod. If the smell of hydrogen sulfide stones is
too strong, add 3 mL of 30% hydrogen peroxide (NOTE 2). Add 3 drops of methyl
orange indicator and stir. Cover the beaker with a watch glass and leave for (1-2)
minutes. If a yellow to yellow-orange color appears at the top of the precipitate, the
solution is not acidic enough.
Add dilute HNO3 (1+1) drop by drop while stirring so that the pink or red color does
not disappear, then add 10 drops in excess. Heat the closed beaker quickly until it
boils.
Don't let it boil for more than a few seconds.
Remove from the hot plate (NOTE 3).
NOTE 1 Use 5 grams for cement samples, and 10 grams for concrete samples and other
materials having a chloride content of less than 0.15% Cl. For materials with higher chloride
content, the number of samples is proportionally reduced. Powder ingredients do not need to be
ground. The coarse sample must be ground to pass a 20 mesh sieve. If the sample is too fine it
will cause excessive silica gel to form during digestion with nitric acid, so that filtering takes
longer.
NOTE 2 Slag and cement slag containing high sulfur sulfides can interfere with determination.
NOTE 3 It is very important to keep the beaker closed during heating and digestion to prevent
loss of chloride on evaporation. Excessive use of acid must be avoided because it will
accelerate the release of the silver chloride layer from the Silver electrode rod. Slightly acidic
slurry is sufficient.
b) Wash 9 cm diameter coarse porous filter paper four times with 35 mL of water using a
suction device equipped with a 250 mL or 500 mL Buchner funnel attached to the
suction flask. Remove the laundry and rinse the pumpkin again with a little water.
Replace the suction apparatus and filter the sample solution. Rinse the beaker and filter
paper twice using a little water. Transfer the filtrate from the flask into the original usable
beaker (NOTE 4).
NOTE 4 It is not necessary to remove slurry residue from the sides of the beaker. As well
in his embarrassment, he's happy to be umaenmg aa tn edriu an lg hase lud sinkiytap, ain't no or kn. you need to filter everything.
Titration can be carried out in Cool the filtrate to room temperature. Volume should not exceed 175 mL.
c) For instruments equipped with a digital readout it is necessary to determine the

approximate "equivalence point" by dipping the electrode into a beaker filled with water
and setting
the instrument so that the reading is approximately 20 mv lower than the middle
scale. Record the reading on the millivolt meter. Remove the beaker and wipe the
electrodes with blotting paper.
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d) In the cooled sample (NOTE 5) beaker of 7.1.3.15.4 item b) Carefully pipette 2.00 mL of
0.05 N NaCl standard solution. Place the beaker on a magnetic stirrer and insert the
rod into it TFE – fluorocarbon coated magnetic stirrer. Dip the electrode into the
solution, being careful not to touch the electrode with the stirrer, start the initial stirring
at low speed. Place the dropper portion of a 10 mL burette, which has been filled to the
mark with standard 0.05 N silver nitrate solution, in the beaker (NOTE 6).
NOTE 5 It is advisable to maintain a constant temperature during the measurement because

the solubility of silver chloride varies considerably with temperature at low concentrations.
NOTE 6 If the burette where the solution is dispensed has droplets adhering, it must be rinsed
into a beaker using several milliliters of water each time after adding the titrant.
e) Titrate in small increments, recording the amount of 0.05 N standard nitrate

solution required to obtain a millivoltmeter reading to 60.0 mV from the
equivalence point
set in water. f) Continue
the titration, each time adding 0.20 mL painter volume. Record the burette and millivoltmeter
readings in columns 1 and 2 on the 4-column recording form as shown in Appendix A.
Each time the painter is added, allow the electrodes to reach equilibrium with the sample
solution. Experience has shown that an adequate reading is obtained if the minimum
scale reading does not change within 5 seconds (usually within 2 minutes). Closer to the
equivalence point, adding the same amount of AgNO3 solution will cause a greater
change in the millivoltmeter reading. Past the equivalence point the change will decrease
again. Continue the titration for up to three more additions after the estimated
equivalence point that has been recorded.
g) Calculate
and enterthe difference
the in readings
value in column 3 of in millivolts
the from one painter addition to the other
record form.
h) Calculate the price difference in column 3 from one to the next addition and enter the
result in column 4. The equivalence point of the titration will be within the maximum
interval of
4 MV recorded in column 3. The equivalence point can be interpolated from the
data listed in column 4 as shown in Appendix A
7.1.3.15.5 Blank
Make a blank determination using 75 mL of water as a substitute for the sample, follow
the same procedure as in 7.1.3.15.4 point a) starting with the sentence "Without delay
add slowly etc. Correction of the analysis results obtained by reducing the blanks
NOTE For non-referee analysis, the determination of blanks may not be carried out.
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Calculate the percent chloride to the nearest 0.001% as follows:
3.545 x (V1-V2)
%Cl=
NW
Note: V1 is
millilite0rs.0o5f N AgNO3 solution used for sample titration (equivalence point); V2 is milliliters of
0.05 N AgNO3 solution used for blank titrations; N is the exact normality of a 0.05 N
AgNO3 solution; W is the sample weight, grams.
7.1.3.16 Organic compounds that dissolve in chloroform
This test method is specifically designed for the determination of vinsol and tallow resins in
portland cement, although mineral oil, resin, calcium stearate and other fatty acid compounds and
some organic compounds are included in this designation.
Be careful during this entire procedure. This test method can be used for cements other
than Portland cement.
Even though the cement contains a relatively high insoluble part, the emulsion will slowly
separate, and the shaking should not be too strong so that more chloroform is used and washing
is more frequent.
7.1.3.16.2 Reagents
a) Chloroform
If the blank determination as described in 7.1.3.16.4 exceeds 0.001, 5 grams of
chloroform must be distilled before use. The chloroform recovered may be slightly acidic
but may be reused on shaking with the acidic solution of the sample in the 1 Liter
separatory funnel.
The chloroform used to wash the filters and separators must be fresh or distilled.
b) Tin(II) chloride (SnCl2).

a) Place 40 grams of cement in a 1 Liter Squibb separatory funnel (NOTE 1) and stir until 250
mL of water is added in 2 equal parts.
Shake vigorously immediately for complete

breakdown. Then add the second half and beat again.
Simultaneously add quickly 185 mL which has been dissolved 10 grams of SnCl2 (NOTE
2) immediately close the funnel, invert the funnel and shake it in a circular motion for a few
seconds to loosen and disperse the cement, being careful to avoid large internal pressure
due to excessive shaking strength is not needed.
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Release the internal pressure immediately by opening and closing the shut-off valve.
Repeat shaking and releasing pressure until the cement is completely decomposed.
If necessary, break up any lumps of cement with a glass stir bar.
Immediately cool to room temperature by placing the funnel under running tap water.
NOTE 1 The use of grease to lubricate the shut-off valve and cover glass on the separator
funnel should be avoided. Wet the cover glass with water before use so it will make the job
easier.
NOTE 2 The purpose of adding SnCl2 is to avoid oxidation of sulfur sulfide to elemental
sulfur, which is soluble in chloroform.
b) Add 75 mL of chloroform to the solution, close the separatory funnel, shake vigorously
for 5 minutes, and leave for 15 minutes to separate the water and chloroform.
The chloroform layer that lies at the bottom is removed and collected into the 125
mL Squibb separatory funnel, including the foam (NOTE 3) and a few milliliters of
water layer, making sure all the foam layer has been removed.
Try to keep the amount of water layer carried as little as possible, because too much
excess water in the 125 mL separatory funnel can lead to incomplete extraction of
the foam and may result in an emulsion that is difficult to separate. Shake another
250 mL separatory funnel containing 50 mL of water and a few drops of HCl.
Shake the separatory funnel in the same way as the first 250 mL separatory funnel.
Wcahrefnulthneotcthololerot fworamtesr egpeat riantost,hpeobuoriliitnigntfolatshke. flat bottom boiling

flask (NOTE 4), being
NOTE 3 Usually shaped like facial foam. May contain organic compounds which dissolve in
chloroform after shaking in a separatory funnel, where the ratio of water to chloroform is large.
It may be possible to concentrate the foam to a small volume by rotating the separatory funnel
slowly after the foam has been dispensed into the narrow part of the separatory funnel.
NOTE 4 The liquid is then distilled, cork or rubber covers should not be heated, 250 mL or 300
mL soil analysis flasks, equipped with a condenser tube may be used. The condenser tube has
an indentation near the neck and a cooling water jacket. The recovered chloroform can be
used again as in 7.1.3.16.2 point a).
c) Add 25 mL of chloroform to the solution in the original 1 liter separatory funnel, and do it
according to 7.1.3.16.3 point b) store the original washing water in the 250 mL
separatory funnel.
Repeat using 25 mL of chloroform. Distill the combined chloroform extract in a boiling
flask until the volume is reduced to (10-15) mL. Filter the separated solution into a
100 mL beaker or platinum strengthening cup (NOTE 5) of known weight through
medium porous filter paper and then rinse with fresh chloroform.
NOTE A platinum evaporating cup is better to use because temperature equilibrium

5
is achieved more quickly. If a beaker is used, it must be allowed to reach equilibrium
temperature for at least 20 minutes before weighing.
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Rinse the flask and wash the filter paper with a small amount of fresh chloroform several times.
Evaporate the extract at a low temperature of not more than 63 oC to dry (NOTE 6)
and heat in the oven at (57–63) oC for 3 minutes.
NOTE 6 Be careful when filtering the extract because many organic compounds that dissolve
in chloroform evaporate if heated too long even if heated at moderate temperatures. If
protected
from dust accumulation, the solution may evaporate at room temperature if left overnight. If rapid
evaporation is desired, the solution may be evaporated on a hot plate at low temperature while
subjected to a stream of dry air through a glass tube 10 mm in diameter and approx. 3 mm in
thickness. Then remove the beaker from the hot plate and continue to air dry slowly until the
residue looks dry then continue with a faster airflow for 5 minutes at room temperature before
placing the beaker in the oven at (57 – 63) oC . Each 3-minute heating period in the oven, blow
hot air into the container for ÿ 15 seconds before weighing. Dry air can be passed after drying
through a drying agent, such as calcium chloride or sulfuric acid, followed by a high-efficiency
drying agent, such as magnesium perchlorate or anhydrous calcium sulfate, being careful to
avoid carrying dust from the dryer by the air.
Besides using compressed air, which is often contaminated with oil, dirt and moisture, this can
also be done by placing the chloroform solution under a glass lid and airflow through the
drying
material using an aspirator or vacuum pump.
If it is known that there is only vinsol resin, the residue is more stable and can be heated at
(100-150) oC, but not at (57 – 63) oC, that is, if there are also other unstable organic elements
to remove all remaining chloroform which may be left behind.
Blow dry air into the container for 15 seconds, cool and weigh.
Repeat heating and weighing for 2 successive weighings the difference is not more than
0.001 0 gram. The last two higher weighing results are taken as the actual weight.
7.1.3.16.4 Blank
Do a blank determination. Heat 40 grams of cement sample at (950 – 1 000) oC for 1

hour and grind again. Treat the sample that has been ignited using the same procedure
and number of reagents in the analysis, correcting the results obtained.
NOTE Be careful working so that the organic compounds are completely burned. Spread the
sample in a 100 mL platinum evaporator cup and it is recommended to use a muffle furnace not
available, a Maker type burner with high temperature can be used. Complete sample mixing must
be carried out periodically every 5 minutes if using a burner.
Calculate the percentage of organic compounds dissolved in chloroform to the nearest

0.001 by multiplying the sample weight in grams of the residue by 2.5 (100 divided by the
sample weight used 40 grams).
NOTE If the organic compound present in the cement is tallow the residues are fatty acids derived
from the hydroxide of the tallow in hot acid solution and the weight must be multiplied by 1.05 to
obtain the actual weight of the glyceride in the tallow. If the original organic compound is calcium
stearate, the residue is stearic acid, and the weight is multiplied by 1.07 to get the actual weight of the
calcium stearate.
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7.1.4 Alternative test method (Optional)
7.1.4.1 Calcium oxide

The test method includes the gravimetric determination of CaO is SiO2 and the ammonium hydroxide
group is separated, followed by precipitation of calcium as oxalate.
The precipitate was converted to CaO by igniting and weighed.
Strontium, usually present in Portland cement as a minor element, precipitates with calcium as
oxalate and is subsequently counted as CaO. If the SrO content is known and a correction from
CaO to SrO is desired for samples, for research purposes or to compare results with SRM certified
values, the CaO obtained by this test method can be corrected by reducing the percentage of SrO.
In the determination to meet the specifications of SrO correction cement for CaO is not necessary
conducted.
7.1.4.1.2 Procedure
NOTE 1 If the analysis is carried out to meet specifications, it is likely that manganese is present in
sufficient quantities to cause the percentage determination of magnesium by the alternative test
method to exceed the specification requirements. Manganese must be separated as described in
7.1.3.9.3 point
b) before determining CaO by the alternative method.
Acidify the combined filtrate from the ammonium hydroxide group determination in 7.1.3.3.1 to
7.1.3.3.4 if necessary, dilute to a volume of about 200 mL.
Add 5 mL of HCl, a few drops of methyl red indicator solution and 30 mL of warm ammonium oxalate
solution (50 g/L) (NOTE 2). Heat the solution at (70-80)
0C and add NH4OH (1+1) drop by drop while stirring until the color changes from red to yellow
(NOTE 3).
NOTE 2 If the ammonium oxalate solution is not clear, it should be filtered before use.
NOTE 3 This neutralization must be carried out slowly, otherwise precipitated calcium oxalate tends to
pass through the filter paper. If a number of these determinations are made simultaneously the
following technique can help to ensure gradual neutralization. Add 2 or 3 drops of NH4OH to the first
beaker while stirring, then 2 or 3 drops to the second beaker, and so on, return to the first beaker with
the addition of 2 or 3 drops again until the color of the indicator in each beaker changes.
Leave the solution without further heating for 1 hour (not more), stirring occasionally for the first 30
minutes. Filter using fine filter paper and wash sufficiently with cold ammonium oxalate solution (1
gram/L). Save the filtrate and washing water.
Transfer the precipitate and filter paper to the original beaker. Dissolve the oxalate precipitate in 50
mL of hot HCl (1+4) and destroy the filter paper. Dilute to 200 mL with water, add a few drops of
methyl red indicator and 20 mL of ammonium oxalate solution, heat the solution to almost boiling,
and precipitate the calcium oxalate by means of an acid solution apparatus with NH4OH solution as
described in 7.1.3.9.3 point a).

Leave the solution for 1-2 hours, strain and wash as before.
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Combine the filtrates obtained and save for determination of MgO according to 7.1.3.10.3, dry the
precipitate in a closed crucible of known weight.
Charcoal the paper without flame, burn the carbon at the lowest possible temperature, finally ignite it
with a tightly closed crucible in an electric furnace at a temperature of (1 100 – 1 200) oC.
Cool in a desiccator and weigh as CaO.
Repeat the massage until the weight remains.
7.1.4.1.3 Blank
Make a blank determination, using the same procedure and number of reagents in the analysis and
correction of the results obtained.
Calculate the percentage of CaO to the nearest 0.1 by multiplying the weight in grams of CaO by 200
(100 divided by the weight of the sample used is 0.5).
Correct by % CaO to SrO, if desired, with reduced percent SrO.
7.1.4.2 Magnesium oxide volumetric method
This test method is a suitable volumetric procedure to use when determinations of silicon dioxide
(SiO2), aluminum oxide (Al2O3), iron (III) oxide (Fe2O3), and calcium oxide (CaO) are neglected.
7.1.4.2.2 Reagents a)
Ammonium nitrate solution (20 grams NH4NO3/L)
b) Ammonium oxalate solution (50 gram/L)
c) Hydroxyquinoline solution
- Dissolve 25 grams of 8-hydroxyquinoline in 60 mL of acetic acid.
- When the solution has dissolved completely, dilute up to 2 liters with cold water.
- The milliliter temperature of this solution is equivalent to 0.001 6 grams of MgO.
d) Potassium bromate-potassium bromide standard solution (0.2 N)
- Dissolve 20 grams of potassium bromide (KBr) and 5.57 grams of potassium bromate (KBrO3)
in 200 mL of water and dilute to 1 liter.
- Determine the concentration ratio of this solution to 0.1 N Na2S2O3 solution in 7.1.4.2.2 point
e) as follows:
In 200 mL of water in a 500 mL Erlenmeyer flask add 25.0 mL of 0.2 N KBrO3-KBr solution .
ÿ Add 20 mL HCl, shake, and add immediately 10 mL Potassium iodide (KI) (250 gram/L).
ÿ Shake and titrate immediately with Na2S2O3 solution until the solution is almost colorless.
Add 2 mL of starch solution and titrate until the blue color disappears.
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- Calculate the concentration ratio of KBrO3-KBr solution to Na2S2O3 solution by

dividing the volume of Na2S2O3 solution by the volume of KBrO3-KBr used in the
titration.
e) Potassium iodide standard solution (0.1 N)

- Dissolve 25 grams of sodium thiosulphate (Na2S2O3.5H2O) in 200 mL of water, add
0.1 gram of sodium carbonate (Na2CO3), and dilute to 1 Liter.
- Leave it for at least 1 week. Immediately standardize this solution against potassium
bichromate (K2Cr2O7) primary standard . One milliliter of 0.10 N Na2S2O3 solution
is equivalent to 0.000 504 grams of MgO. f) Starch solution In 500 mL of boiling
water
add a cold suspension of 5 grams of starch which can be dissolved in 25 mL of water, cool
the solution to room temperature, add all of the cold solution made of 5 grams of
sodium hydroxide (NaOH) in 50 mL of water, add 15 grams of KI, and mix thoroughly.
7.1.4.2.3 Procedure
a) Disperse 0.5 gram (NOTE 1) sample of cement in a 400 mL beaker with 10 mL of

water, while shaking, while adding 10 mL of HCl.
Immediately dilute to 100 mL.
Gently heat and break up any coarse particles with a flat-tipped stirring rod until
completely decomposed, add 2 or 3 drops of HNO3 and heat to a boil (NOTE
2).
N O T E 1 I f S i O 2 is a m m o n
t o a n ap p r o p r ia te m e th o d ,
i u m h yd r o xi d e g ro up , a n d C a O is s e p a r a t e d a n d
b o th a r e fe r e nc e m e th o d a n d an a l te r n a t iv e t e s t
de t e r m i n e d a c c o r ding
m e t h o d , t h e fi lt ra t e that remains can be used for the determination of MgO
as described in 7.1.4.2.3 point a) starting from the last sentence in 7.1.4.2.3 point c), namely
"Add 5 mL HCl etc". .
NOTE 2 In the case of cement containing blast-furnace slag or significant amounts of sulfur
sulfide, add 12 drops of HNO3 and boil for 20 minutes to oxidize the iron and remove the
sulfide.
b) Add 3 drops of methyl red indicator to the solution and then add NH4OH until the
solution is yellow.
Heat the solution to boiling and continue boiling for (50-60) seconds.
If difficulties arise due to bumping on boiling Ammonia solution, during a 10 minute
digesting period on a steam bath, or on a heating plate having the same temperature
can
be used instead of further boiling for 50 seconds -60 seconds above combustion.
Remove from burner, steam bath, or heating plate and allow to cool down.
Use medium porous filter paper, filter the solution immediately, wash the precipitate
twice with hot NH4NO3 (20 gram/L), and save the filtrate.
Transfer the precipitate with filter paper into a beaker and dissolve it with 10 mL
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HCl (1+1). Destroy the filter paper. Dilute to ÿ 100 mL and heat
to boil.
The precipitate was filtered again and the hydroxide washed as above.
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Combine the filtrate and the first settling wash water, taking care that the volume does not
exceed 300 mL (NOTE 3). Add 5 mL of HCl, a few drops of methyl red indicator solution and 30
mL of warm ammonium oxalate solution (50 g/L).
Heat the solution at (70-80) oC and add drop by drop NH4OH (1+1), while stirring, until the color
changes from red to yellow (NOTE 4).
Leave the solution without further heating for 15 minutes on the steam bath.
Add 10 mL - 25 mL of 8-hydroxyquinoline reagent (NOTE 4) and 4 mL of NH4OH solution/100

mL of solution. Stir the solution on a mechanical mixer for 15 minutes, remove and allow it to
settle down (NOTE 5).
Filter the solution using medium porous filter paper and wash the precipitate with NH4OH (1+40).
Dissolve the precipitate with (50-75) mL hot HCl (1+9) in a 500 mL Erlenmeyer flask.
Dilute the resulting solution to 200 mL and add 15 mL HCl.
Cool the solution to 25 oC and add with a pipette or burette (10-35) mL of 0.2 N KBrO3 – KBr
solution (NOTE 6).
Stir the solution and leave it for about 30 seconds to ensure complete bromination.
Add 10 mL KI (250 g/L). Stir the solution obtained well and titrate with 0.1 N Na2S2O3 solution
until the color of the iodine becomes pale yellow. At this stage add 2 mL of starch solution and
titrate the solution until the blue color disappears.
NOTE 3 In case the cement contains blast furnace, or is considered to contain significant
Manganese, acidify with HCl, mix to 100 mL, and separate the manganese, as described
in
7.1.3.9.3 point a).
NOTE 4 An excess of 8-hydroxyquinoline reagent is necessary to avoid low MgO yields,

but overdosage will result in higher yields.
The instructions below should be used to determine the amount of reagent to be added.
Table 7 ÿ Comparison of MgO levels with the amount of reagent required

Estimated MgO content,
% 0 – 1.5 Estimated amount of reagent
needed, mL 10
1.5 – 3.0 3.0

– 4.5 4.5 – 6.0
1520 25
NOTE 5 Within 1 hour intervals the precipitate must be filtered off. When longer leads to
high yields.
NOTE 6
The amount of KBrO3-KBr standard solution should use the following table
(requirements, not notes):
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Table 8 ÿ Comparison of MgO levels with the amount of standard solution

Amount of standard solution
Estimated MgO content, %
KBrO3 – KBr, mL 10
0–1
1–2 15
2–3 20
3–4 25
4–5 30
5–6 35
7.1.4.2.4 Blank
Make a blank determination, using the same procedure and amount of reagent, and correct the results
obtained in the analysis.
Calculate the percentage of MgO to the nearest 0.1 as follows:
% MgO = E (V1R – V2) x 200
Note: is the
is millilieteqrusivoafleKnBtroOf3M–gKOBwr
istholNutaio2nS2uOse3ds; oRluistiothne, grraatimo /omf Lth; eE
V1 strengthis oaf sthoeluKtioBnrOo3f N–aK2BSr2sOo3lu.
tuiosnedto, mthLe; N20a02Sis2O1030sdoilvuitdioend; bVy2
the weight of the sample used (0.5 grams).
NOTE V1R indicates the volume of Na2S2O3 solution. which is equivalent to the volume of KBrO3-
KBr solution used, V2 represents the amount of Na2S2O3 required by the excess KBrO3-KBr which
is
not reduced by magnesium oxyquinolate.
7.1.4.3 Titanium dioxide
The test method for the dioxide (TiO2) was determined colorimetrically by comparing the color intensity
of the titanium peroxide solution in the sample with the color intensity of the titanic sulfate book peroxide
solution.
7.1.4.3.2 Interference
Interfering elements in the peroxide method for TiO2 are vanadium, molybdenum, and chromium. In
small amounts it can cause interference with other elements in cement, therefore smelting with Na2CO3
7.1.4.3.5 point d) and extraction with water is necessary.
7.1.4.3.3 Equipment
Colorimeters
The equipment shall consist of a colorimeter of the Kennicou or Duboscq type, or other colorimeter or
spectrometer designed to measure the transmittance of light, and capable of being used for measurements
at wavelengths of 400 nm-450 nm.
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7.1.4.3.4 Reagents
a) Ammonium chloride (NH4Cl). b)
Ammonium nitrate (NH4NO3 20 gram/L).
c) Iron (II) sulfate solution (1 mL = 0.005 gram Fe2O3).
Dissolve 17.4 grams of iron (II) sulfate (FeSO4.7H2O) in water containing 50 mL H2SO4 and dilute to 1L.
One milliliter is equivalent to 1% Fe2O3 in 0.5 grams of sample.
d) Hydrogen peroxide (30%).
Concentrated hydrogen peroxide (H2O2).
e) Sodium carbonate (20 g/L Na2CO3). f) Sodium
or potassium pyrosulfate (Na2S2O7 or K2S2O7).
g) Standard solution of titanic sulfate (1 mL = 0.000 2 g TiO2).

- Use standard TiO2 provided by the National Bureau of Standards (sample standard 154 or its substitutes).
Dry for 2 hours at (105 –110) oC. Transfer a (0.20-0.21) gram weight of TiO2 to a 125 mL philips beaker.
- Add 5 grams of ammonium sulfate ((NH4)2SO4) and 10 mL of H2SO4 into a beaker and insert a
short- stemmed glass separatory funnel into the mouth of the beaker.
- Heat the mixture continuously until it boils while the pumpkin is rotated over the flame. Continue heating
until the solution is completely dissolved effectively and no part of the material sticks to the walls of the
flask.
NOTE Although there is a small amount of TiO2 residue, it will not be a problem if
this procedure is carried out properly.
- Cool and immediately pour the solution into 200 mL of cold water while
stirring strong.
- Rinse the flask and funnel with H2SO4 (1 + 19), stir, then let the solution and washing water stand for at
least 24 hours. Filter into a 1 Liter measuring flask, wash the filter thoroughly using H2SO4 (1+19),
dilute to the mark with H2SO4 (1+19), and shake.
Calculate the TiO2 equivalent, from titanic sulfate solution, gram/mL, as follows:
AB
E=
1 000
Information:
E is the equivalent of TiO2, from Ti(SO4)2 solution, gram/
A mL; is grams of TiO2, the standard used (correction for loss on drying; is the
percentage B of TiO2, the standard as stated in the certificate issued by the National
Bureau of
Standards (NBS), divided by 100; 1 000 is milliliters of solution in a measuring flask.
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7.1.4.3.5 Procedure
a) Mix completely 0.5 gram of cement sample and 0.5 gram of NH4Cl in a 50 mL beaker,
cover the beaker with a watch glass, and carefully add 5 mL of HCl.
Allow the acid to flow down past the lip of the lidded beaker.
After the chemical reaction subsides, remove the cover, stir the mixture with a glass stirring
rod, cover again (NOTE 1) during the digestion time, stir the contents once again and
destroy any lumps that are still there to make it easier for the cement to decompose
completely.
Quickly place the medium porous filter paper into the funnel and transfer the precipitate
onto the filter paper. Scrub the walls in the chemistry room with the rubber policeman and
rinse the beaker and policeman.
Wash the filter paper two or three times with hot HCl (1+99), and then with a little hot
water ten or twelve times, letting each time wash the water
flowing out.
NOTE 1 Hot plates can be used instead of a steam bath. If the tool is equipped with a temperature
controller so that the heat generated is close to the heat of a steam bath.
b) Transfer the filter paper and residue to the crucible (NOTE 2), dry it and ignite slowly until
the carbon from the filter paper is completely burned without flame.
Treat the SiO2 obtained with 0.5 mL-1 mL water, 10 mL HF, and 1 drop H2SO4, and
carefully evaporate until dry. (NOTE 3).
NOTE
2 When a shorter procedure is desired for purposes other than the test method
referee,
can usually with a little neglect of the thoroughness of the procedure as 7.1.4.3.5 point b)
be omitted.
NOTE 3 If the determination of SiO2 is desired in addition to the determination of TiO2, SiO2
may be treated with HF as in 7.1.3.2.1.3 to 7.1.3.2.1.4.
c) Heat the filtrate to boiling and add NH4OH until the solution becomes completely
completely alkaline, exhibited an ammoniacal odor.
Add some filter paper pulp to the solution and boil for (50–60) seconds.
Let the precipitate form, filter through medium porous filter paper, and wash twice
times with hot NH4NO3 solution (20 gram/L).
Place the precipitate in a crucible whose SiO2 has been treated with HF and
incandescent slowly until the carbon from the filter paper is exhausted.
NOTE 4 If the determination of the ammonium hydroxide group is desired in addition at

temperature TiO2, precipitation and flashing may be made as in 7.1.3.3.3 item a) to 7.1.3.3.3 item
d). However, the crucible must contain residue from treating SiO2 with HF unless circumstances
permit to exclude this as indicated in NOTE 58.
d) Add 5 grams of Na2CO3, into the crucible and melt for (10-15) minutes (see
"Disturbance").
Cool, separate the melt from the crucible and transfer to a small beaker.
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Wash the crucible in hot water using a rubber policemen. Digest the melt and wash until
the melt is crushed then filter through medium porous filter paper with a diameter of 9 cm
and wash several times with Na2CO3 (20 gram/L).
Discard the filtrate, place the precipitate in a crucible and incandescent slowly until the carbon
from the filter paper is completely burned. Add 3 grams of Na2S2O7 or K2S2O7 to the
crucible and heat it to a glow until the residue dissolves in the melt (NOTE 5).
Cool and dissolve the molten pool in water containing 2.5 mL H2SO4.
If it is necessary to reduce the volume of the solution (NOTE 6), filter into a 100 mL
volumetric flask through 7 cm diameter medium porous filter paper and wash with hot
water.
Add 5 mL of H3PO4 and cool the solution with water, and shake thoroughly.
NOTE 5 Begin heating with caution due to pyrosulfate (also known as molten bisulfate) which is
splashed at the start of heating due to H2SO4. Avoid unnecessarily high temperatures or
prolonged
heating, as melted pyrosulfate can damage platinum. Use non-sparking pyrosulfate by partially
heating the pyrosulfate in a crucible to remove excess H2SO4. and destroy the cold melting
period.
NOTE 6 If the solution is evaporated until the volume is reduced and the contents are allowed
to cool, it can make it difficult for the precipitated sulfate to dissolve again. In the event of
excessive evaporation, do not allow the contents to cool, but add hot water and digest on a
steam bath or heat until all precipitates are dissolved again, with the possibility that some non-
dissolving SiO2 may remain .
NOTE 7 Over time hydrogen peroxide will decompose. The strength can be determined by
adding a certain amount to 200 mL of cold water and 10 mL of H2SO4. (1+1) and then titrated
with a
standard solution of potassium permanganate (KMnO4) prepared according to 7.1.3.9.2 point
b). If the standard solution contains 0.005 635 7 grams KMnO4 /mL, then 49.5 mL of this
solution is
required by 0.50 mL of 30% H2O2 .
e) Prepare a reference standard solution from Ti (SO4)2 standard solution or a series of

reference standard solutions in a 100 mL measuring flask, depending on the type of
colorimeter used.
Into each solution, add 3 grams of Na2S2O7 or K2S2O7 which has been dissolved in
water, then add an amount of Fe2SO4 solution which is equivalent to Fe2O3 containing 0.5
grams of cement, 2.5 mL of H2SO4 and 5 mL of H3PO4 solution (NOTE 8 ). When the
solurotiomis at temperature, add 1.0 mL of 30% H2O2 , dilute to the mark with water and
shake thoroughly (NOTE 9).
NOTE 8 The color produced by Fe2(SO4)3 solution is partly due to the bleaching effect of
H2SO4, H3PO4 and alkali salts on ferrous ions and peritanic ions. The sequence must be
followed to obtain high precision. However, if a shorter procedure is desired for purposes other
than referee analysis, the addition of pyrosulfate, FeSO4 and H3PO4 solutions to the reference
solution can be removed if the Fe2O3 in the cement sample is less than 5%. This can cause the
precision to be slightly reduced.
NOTE 9 Color develops quickly and is stable for some time, but if the peroxide solution is left for
a long time, oxygen bubbles will appear and disturb the color ratio. If the contents of the first
tube
are agitated, fine bubbles may form which must be allowed to clear before comparisons are
made. The comparison between the standard solution and the sample must be done in
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f) Compare the color, light transmittance or absorbance of the sample solution with
reference standard solution.
The method of comparing colored solutions or measuring transmittance or absorbance

depends on the type of equipment (see 7.1.4.3.5 g through 7.1.4.3.5 item i) and must be in
accordance
with the instructions for use of the equipment provided by the manufacturer.
When the cement peroxide solution is compared with a standard peroxide solution,
remember that this single standard solution cannot cover all areas of the required TiO2
content. The difference in volume or depth for the two liquids should not be more than 50% of
the smallest value.
All solutions must contain H2SO4, H3PO4, Fe2(SO4)3 and persulfate in the specified
concentrations, unless otherwise desired in the circumstances according to NOTE
10.
NOTE 10 Even though there is a small amount of TiO2 residue, it will not be a problem if this
procedure is carried out properly.
g) Kennicott type colorimeter

Using a piston (plunger) in a reservoir of standard peroxide solution, adjust the amount of
solution through which light passes until it gives the same color intensity as the sample peroxide
solution.
h) Colorimeter type Duboscq

Raise or lower the piston from the bowl so that the two solutions give the same color
intensity when viewed from above. Color comparisons can be made visually or
photoelectrically.
i) A colorimeter designed to measure light transmittance

Measurements must be made at a wavelength of 400 nm-450 nm can be done either visually
or photoelectrically. In most colorimeters of this type, the equipment is calibrated with a
standard solution and the calibration curve shows the relationship between light transmittance
or absorbance to TiO2 levels (which has been prepared beforehand).
7.1.4.3.6 Blank
Make a blank determination, following the procedure and the same number of reagents and
correcting the results obtained in the analysis.
Calculate the percentage of TiO2 to the nearest 0.01. If a colorimeter designed to measure light
transmittance is used: read the TiO2 percentage from the calibration curve showing the relationship
of light intensity to TiO2 content.
When the sample peroxide solution is compared with one of the reference standard solutions,
calculate the percentage of TiO2 as follows.
For a kennicott type colorimeter:
%TiO2 = (100 VE/S) x (D/C)
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For the duboscq type colorimeter:
%TiO2 = (100 VE/S) x (F/G)
Information:
V is milliliters of standard solution of Ti (SO4)2 in standard peroxide
solution; E is the TiO2 equivalent of standard Ti (SO4)2 solution, gram/mL;
S is the gram of sample used;
C is the total volume of the peroxide reference standard solution, mL ;
D is the volume of the peroxide reference standard solution in proportion to the sample peroxide
solution, mL ; is the depth of the reference standard peroxide solution through which light
passes;
FG is the depth of the sample peroxide solution through which the light passes.
NOTE The difference between D and C or between F and G must not exceed 50% of the least value.
7.1.4.4 Phosphorus pentaoxide

In this method, phosphorus is determined volumetrically by precipitating the phosphorus as

ammonium phosphomolybdate and titrating with NaOH and H2SO4.
7.1.4.4.2 Reagents
a) Ammonium molybdate solution
Prepare the solution according to 7.1.3.5.3 point a).
b) Ammonium nitrate (NH4NO3) c)

Potassium nitrate solution (10
gram/L)
Dissolve 10 grams of potassium nitrate (KNO3) in water which is free of CO2, dilute to 1 liter (water
is freed from CO2 by boiling).
d) Standard solution, sodium hydroxide (0.3 N)
- Dissolve 12 grams of sodium hydroxide (NaOH) in 1 liter of cold water that is free of CO2 (water
is freed from CO2 by boiling).
- Add 10 mL of fresh, saturated barium hydroxide (Ba(OH)2)

solution filtered.
- Shake the solution regularly for several hours, and strain.

- Keep CO2 contamination from the air.
- Standardize the solution for potassium phthalic acid (standard example No. 84) or benzoic acid
(standard example No. 39) provided by the National Berau Standards according to the
instructions accompanying the standard materials.
- Calculate the equivalence of phosphorus pentaoxide (P2O5) from the solution (gram/L), as follows:
E = N x 0.003 086
Note: E is the
equivalence of P2O5 with NaOH solution, gram/mL; N is the
normality of the NaOH solution; 0.003 086 is the equivalent
of P2O5 to 1N NaOH solution, gram/mL.
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NOTE The value of the solution is based on the assumption that the phosphorus in the
cement is precipitated as Ammonium phosphomolybdate (2(NH4)3PO4, 12 MoO3) and the
precipitate reacts with the NaOH solution:
2 (NH4)3 PO4, 12MoO3 + 46 NaOH = 2 (NH4)2 HPO4 + (NH4)2 MoO4 + 23 Na2MoO4 +

22 H2O.
The number 0.003 086 is obtained by dividing the molecular weight of P2O5 (141.96) by mm
46 (46 is the amount of NaOH in the reaction equation) and by 1 000 (the number of milliliters
in 1 liter). Since the actual composition of the precipitate is affected by depositional
conditions, it is therefore important to observe the sequence of procedures carefully as
described above.
e) Sodium nitrite (NaNO2 50 gram/L)
f) Standard solution, sulfuric acid (0.15 N)

Dilute 4.0 mL H2SO4 to 1 L with freshly boiled cold water. Standardize against standard
NaOH solution. Determine the ratio of the concentration of the standard H2SO4 solution to
the volume of the NaOH solution by dividing the volume of the NaOH solution by the
volume of the H2SO4 solution used in the titration.
7.1.4.4.3 Procedure
a) Weigh (1-3) grams of sample (NOTE 1) and 10 g of NH4NO3 into a 150

beaker mL.
Stir the mixture, add 10 mL HNO3, and mix rapidly, using a flat-tipped stir bar to break up
any lumps of cement, until the cement has completely dissolved and the viscous gel of
silica (SiO2) is broken up.
Cover the beaker with a watch glass, place it on a water bath or heating plate at
approximately 100 °C for (15-20) minutes, and stir the contents occasionally while heating.
Add 20 mL of hot water to the beaker and stir the contents.

If the cement contains sufficient levels of manganese to show a red or brown residue, add
a few milliliters of NaNO2 (50 g/L) to dissolve the residue.
Bring the contents of the beaker to a boil until all the nitrous vapor is gone.
This procedure must be carried out in no more than 5 minutes, and water must be
added to replace parts lost due to evaporation.

Filter, using medium-porous filter paper, into a 400 mL beaker under suction and with a
platinum cone to support the filter paper. Wash the SiO2 residue with hot water until
the volume of the filtrate and washing water is approximately 150 mL.
NOTE 1 The amount of sample and reagent used depends on the phosphorus content in
the cement. The minimum amount is required if the cement contains 0.5% P2O5 or greater.
The maximum amount is required when the specified P2O5 content is 0.1% or less.
b) Heat the solution at (69-71) oC, remove it from the heat source, and
immediately add (50-100) mL of ammonium molybdate solution.
Stir the solution vigorously for 5 minutes, wash the inside of the beaker with cold
KNO3 solution (10 g/L), cover the beaker with a watch glass and leave for 2 hours.
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Using a vacuum, filter the precipitate (NOTE 2) by decanting the solution while disturbing
the precipitate as little as possible. Stir the precipitate in the beaker with a stream of cold
KNO3 solution, decant the liquid, then wash off the precipitate on a filter.
Scrub the stirring rod and beaker with the policeman, wash them and pour the contents over
the filter. Wash off the precipitate until it is free of acid (NOTE 3), allowing each addition of
the washing solution to be completely sucked before further additions.
NOTE 2 The filter may be a medium porous filter paper supported on a platinum cone or a
small Hirsch funnel by means of a suitably cut filter paper and a thin layer of acid-free washed
pulp or asbestos pulp.
Screening should be done with care that has been washed free of acid. Screening must be
done carefully to avoid loss of precipitate. The filter must be perfectly precise, and suction must
be applied before filtering and maintained until the washing is complete.
NOTE 3 Estimated approx. 10 washes. Test the 10th washing water with drops of
phenophthalein indicator and half a drop of standard NaOH solution. If a pink color appears and
is visible for at least 5 minutes, the precipitate is truly acid-free, otherwise washing should be
continued.
c) Transfer the filter and precipitate to the beaker used for settling, use small pieces of damp
paper to clean the funnel and remove any sediment that may be in the funnel.
Add 20 mL of cold CO2 free water to the beaker and destroy the filter paper with the
policeman used to scrub the beaker.
Add excess 0.3 N NaOH solution, stir the contents of the beaker until the yellow spots
disappear, wash the policeman and the walls of the beaker with 50 mL of CO2-free cold
water, and add 2 drops of neutral phenolphathalein indicator solution.
Treat the solution with 0.15 N H2SO4 solution , in a measured quantity, sufficient to
remove the pink color completely.
Complete the titration with the NaOH solution until a slightly pink color persists for at least
5 minutes.
7.1.4.4.4 Blank
Make a blank determination, following the procedure and the same number of reagents, correcting
Calculate the percentage of P2O5 to the nearest 0.01 as follows:
% P2O5 = [E(V1-V2R)/S] x 100
Note: is the
milliliteerqsuoivf aNleanOtHofsPol2uOtio5ntousNeadO;
HV2soisluthtioenm, gill/iLlit;eErsVo1f is H2SO4 used; R
is the ratio of the strength of the H2SO4 solution to the
NaOH solution; S is the gram of sample used.
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7.1.4.5 Manganese oxide
In the test method, manganese oxide is determined volumetrically by titration with potassium permanganate
solution.
7.1.4.5.2 Reagents
a) Standard solution of potassium permanganate (0.18 N)
Prepare a solution of potassium permanganate (KMnO4) and standardize as described in 7.1.3.9.2

point b), except for manganese oxide (Mn2O3) the equivalent of the solution is calculated by the
equivalent of potassium oxide (CaO).
Calculate the equivalence of Mn2O in solution as follows:
E = (B x 0.353 4) / A
Note: E is the
equivalencoef Mn2O3 to KMnO4 solution, g/mL; B is the grams of
Na2C2O4 Nusae2dC;2AOi4s ttihtreatmioinlli;li0te.3rs53of4KiMs
tnhOe4msoolleuctiuolnarnreaetidoeodf in the 3Mn2O3 to 10
Na2C2O4.
b) Zinc oxide (ZnO) powder
7.1.4.5.3 Procedure
a) Place 2 grams of sample in a 250 mL beaker and add approximately 50 mL

water.
Stir the mixture until a suspension occurs and then add 15 mL HCl.
Heat the mixture carefully until the solution is as perfect as possible.
Add 5 mL HNO3 and 50 mL water to the solution and boil until some of the chlorine is released.
If necessary, add hot water to maintain the volume ÿ 100 mL.

Stop boiling and add ZnO powder to the solution until it is free of acid.
Add (3-5) grams of excess ZnO powder to the solution and boil for a few minutes.
b) Without filtering, and while keeping the solution heated (90-100)oC by heating intermittently or
continuously, titrate with 0.18 N KMnO4 standard solution, until the addition of 1 drop of KMnO4
produces a pink color that does not disappear anymore.
Approaching the end point of the titration, let the precipitate sink slightly, and observe the color of the
solution layer from the side of the beaker.
7.1.4.5.4 Blank
Make a blank determination, follow the procedure and the same number of reagents and correct the
results obtained in the analysis.
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Calculate the percentage of Mn2O3 to the nearest 0.01 as follows:
% M N O = EV x 50
2 3
Note: E
is
the equivalence of Mn2O3 and KMnO4 solution , gram/mL; V is
milliliters of KMnO4 solution used; 50 is 100 divided by the
weight of the sample used (2 grams).
7.1.4.6 Free calcium oxide
This test method is a quick way test for determining free calcium oxide in fresh slag.
If used for old cement or slag, one must keep in mind the possibility of calcium hydroxide, because
this method does not distinguish between free CaO and free Ca(OH)2 .
Two test methods are provided. First, alternative test method A is a modified Franke's procedure
in which free lime is titrated with an aqueous solution of perchloric acid after the solution is in ethyl
acetodetate-isobutyl alcohol.
Second, alternative test method B is titration of ammonium acetate–alcohol glycerin against free
lime with Sr (NO3)2 as accelerator.
7.1.4.6.2 Modified Franke test method (Alternative test method A)
a) Reflux apparatus
Consists of a flat-bottomed, short-necked Erlenmeyer flask, 250 mL capacity.
Water-cooled reflux condenser that is a minimum of 300 mm in length. The reflux flask
and condenser are connected by a glass connector.
The reflux condenser must be equipped with an absorbent tube containing a desiccant, such
as silica gel, and a material for separating CO2, such as ascarite.
The absorber tube is installed by making rubber on the top of the reflux column.
b) Burette
The capacity is 10 mL and the scale cannot be larger than 0.05 mL.
c) Vacuum filter equipment.
Consists of a cup of Gooch size No. 3, 25 mL capacity inside which is placed suitable filter
paper, size 21 mm, Walter cup holder, 500 mL suction flask and vacuum suction source. The
cup is half filled with compacted pulp.
d) Glass boiling stone granules.
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7.1.4.6.2.2 Required solvents
a) Ethyl acetoacetate–isobutyl alcohol solvent

Three parts by volume of ethyl acetoacetate and 20 parts by volume of isobutyl alcohol.
b) Thymol blue indicator
Dissolve 0.1 gram of thymol blue indicator powder in 100 mL of isobutyl alcohol.
c) Standard solution of perchloric acid
- 22 mL solution of perchloric acid (70 – 72) % to 1 Liter with
isobutyl alcohol.
- Standardize this solution as follows: Heat 0.100 0 gram of calcium carbonate

primary standard in a crucible at (900 – 1 000) oC.
- Cool the crucible and its contents in a desiccator and weigh accurately
0.000 1 gram to constant weight.
- Perform weighing quickly to prevent absorption of water and CO2.

- Immediately transfer the CaO without grinding into a clean and dry Erlenmeyer flask, and
re- weigh the empty crucible to the nearest 0.000 1 gram, to determine the amount of
CaO added. Then follow the procedure starting with "Add 70 mL of ethyl acetoacetate-
isobutyl alcohol etc" from 7.1.4.6.2.3 point a).
- Calculate the CaO equivalence to perchloric acid standard solution in grams per milliliter
by dividing the weight of CaO used by the volume of perchloric acid required for the
titration.
a) Weigh 1,000 grams of finely ground sample and transfer it to a dry and clean 250 mL
Erlenmeyer flask.
Add four to five glass boiling stones.
Add 70 mL of the prepared ethyl acetoacetate–isobutyl alcohol solvent.
Stir the flask until the sample is dispersed.
NOTE Accurate grinding of the sample is very important for the release of free lime grains
which are often entrapped in the tricalcium silicate crystals in cement.
However, sample contact with air must be kept as low as possible to avoid carbonation of free
lime. In particular, breathing directly into the sample should be avoided. The sample must be
fine
enough to pass through sieve no. 200 (75 µm) but filtering is not recommended. If samples are
not tested immediately, they should be stored in airtight containers to avoid unnecessary
contact
with air.
b) Connect the flask to the reflux condenser and treat the sample until it
boils. Reflux for 15 minutes.
c) Separate the condenser flask, plug it, and cool immediately to room temperature.
d) Filter the sample and solution using a vacuum apparatus. Wash the flask and residue bit by
bit (10-15) mL with isobutyl alcohol until the total volume of the washing solution is 50 mL.
e) Add 12 drops of thymol blue indicator to the filtrate and titrate with
acid perchlorate 0.2 N until a clear color change occurs.
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Calculate the percent free calcium oxide to the nearest 0.1%:
EV x 100
% free CaO = W
Note: E is
the equivalent of CaO to perchloric acid, gram/mL; V is the
milliliters of perchloric acid solution required for the sample; W is
the sample weight, grams.
7.1.4.6.3 Rapid test method of Sr(NO3)2 (alternative test method B)
a) Ammonium acetate standard solution (1 mL = 0.005 g CaO)

- Prepare a standard solution of ammonium acetate (NH4C2H3O2) by dissolving 16 grams of
ammonium acetate (which has been previously stored in a desiccator) in 1 liter of ethanol
in a dry and clean closed bottle.
- Standardize this solution using the same procedure as in 7.1.4.6.3.2 point a) except for
subsequent use as a sample replacement, heat it to a constant weight of ± 0.1 gram
of CaCO3 with a platinum crucible at a temperature of (900 – 1 000) oC.
Cool the contents in a desiccator and weigh to the nearest 0.000 1 gram.
- Perform weighing quickly to prevent absorption of water and CO2.
Immediately transfer the CaO without pulverizing it into a 250 mL boiling flask (containing
glycerin-ethanol and Sr(NO3)2 solvent, and weigh again the empty crucible to determine
the
weight of CaO to the nearest 0.000 1 gram.
- Continue according to point 7.1.4.6.3.2 point a) and 7.1.4.6.3.2 point b).
- Calculate the equivalence of CaO to ammonium acetate in grams per milliliter by dividing
the weight of CaO used by the required volume of solution.
b) phenolphthalein indicator
Dissolve 1.0 gram of phenolpthalein in 100 mL of ethanol (formula 2 B)
c) Glycerin – ethanol solvent (1 + 2)
- Mix 1 part volume of glycerin with 2 parts volume of ethanol (formula 2 B).
- For every liter of this solution, add 2.0 mL of phenolphthalein indicator solution.
NOTE Denaturalized ethanol according to formula 2B (99.5% ethanol and 0.5% benzol)
is preferable but can be substituted for reagent grade isopropyl alcohol.
d) Strosium nitrate Sr(NO3)2, reagent grade.
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a) Transfer 60 mL of glycerin-ethanol solvent into a 250 mL flat bottom boiling flask, clean
and dry.
Add 2 g of anhydrous strontium nitrate (Sr(NO3)2), and adjust the solvent to slightly
alkaline by adding dropwise a fresh, dilute NaOH solution in alcohol until a slightly pink
color forms.
Weigh 1,000 g of the finely ground sample into a flask, insert a magnetic stir bar, and
immediately connect it to the water-cooled condenser (using a 24/40 connecting glass).
NOTE Denaturalized ethanol according to formula 2B (99.5% ethanol and 0.5% benzol)
is preferable but can be substituted for reagent grade isopropyl alcohol.
Boil the solution in the flask on a hot plate with a magnetic stirrer for 20 minutes with
moderate stirring speed.
b) Remove the condenser and filter the contents of the flask with a polypropylene Buchner
funnel under suction, using a 250 mL flask having a tubular side for filtering.
Treat the filtrate to boiling and immediately titrate with standard ammonium acetate solution
until the end point of the titration is colorless.
Calculate the percent free calcium oxide to the nearest 0.1% as follows:
% free CaO = EV x 100
Note: E is
the equivalent of CaO to ammonium acetate solution, gram/mL; V is
the milliliters of ammonium acetate solution required for the sample.
7.2 Physics test method
7.2.1 Auxiliary materials and equipment
7.2.1.1 Auxiliary materials
a) The temperature of the test room is set at (23 ± 1.7) oC, while the humidity of the room
relative humidity test laboratory not less than 50%.
b) What is meant by a humid room is a room with a relative humidity of around 95%. c) If
water is used in the test, what is meant by water is distilled water. d) What is meant by
cold water, water that has room temperature. e) Measuring the amount of water is sufficient
to do with a measuring cup that has a size division of 1 mL.
f) Weighing with an accuracy of up to 0.01 gram must be carried out with a scale with a
maximum capacity of 500 gram.
g) Weighing with an accuracy of up to 10 grams must be carried out with a balance
the highest capacity of 5 000 grams.
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7.2.1.2 Equipment
a) Standard sieve size 150 um (No. 100) and 850 um (No. 20)
Wire mesh for standard screens shall be made of brass, bronze or suitable wire. The
wire is securely attached to the frame 50 mm deep from the top of the frame.
The connection between the frame and the wire mesh must be filled with solder to
prevent any cement from remaining in the connection.
The filter frame must be round with a diameter of 203 mm, equipped with a pan and cover.
b) Scales
Analytical balance has a capacity of not more than 200 grams with accuracy
0 . 0 0 0 1 o r a s c l e w it h a c o n
rT the h ae nd bin0ag .0lam 0n 0uc es2t mgh ruaasv m tesb aea s nceda npms ai tubiv sle
t a n t l a d a n d c a n b e r e a d d i
itty ho aof vfp enr ooad tnu mca oicn rcge uart ha race ynp oe0 fa.00t 0 .r00e 0a 10d gi2n r
e c tl y .
g ag mrwa .i mth sa. Sdcifafeleresnwceithodf inreoct tmore
Conventional scales with 2 pans must have a maximum difference of 0.000 3 grams
if weighing is done by exchanging pans.
c) Weights
The weights must be checked at least once a year or if necessary readjusted at least
within the tolerances permitted for class III. For this purpose, each laboratory must be
able to maintain accuracy or must have a standard weighing scale from 50 grams to
10 mg that conforms to a minimum class III specification and must calibrate it.
d) Brush
A soft-bristled brush is required for cleaning 150 um (No. 100) sieves.
7.2.2 Smoothness test with a blaine and turbidimeter
7.2.2.1 With a blaine tool
Testing with a blaine tool aims to determine the fineness expressed in the specific
surface area of portland cement, calculated as the total surface area of cm2/gram, or m
2
/kg portland cement.
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7.2.2.1.1 Equipment
(1) Blaine device
The blaine device basically consists of a device that draws a certain amount of air through a bed of portland
cement prepared with a certain porosity, which is a function of the particle size and determines the rate of
air flow through the bed.
This tool is shown in Figure 3 and consists of the following parts: a) Permeability cell
The permeability cell consists of a rigid cylinder with an inside diameter of (12.70 ± 0.10) mm
fabricated from austenitic stainless metal.
i. The inside of the cell must be smooth (0.81 um fineness)
The top of the cell must be perpendicular to the main axis of the cell.
The bottom of the cell shall be able to form an airtight connection with the upper end of
the manometer so that no air leakage occurs between the contact areas.
ii. The ledge (0.5–1.0) mm wide is the portion of the cell that is firmly attached to the cell, at a
distance (55 ± 10) mm, from the top of the cell to support the perforated metal disk.
The top of the permeability cell shall be provided with a protruding exterior, to facilitate removal
of the cell from the manometer.
b) Dish
i. The disc is made of stainless steel with a thickness of (0.9 ± 0.1) mm with as many as (30-40)
holes with a diameter of 1 mm and spread evenly.
ii. The disk must match the inside of the cell, the center of one side of the disk must be marked or
inscribed that can be read, so that the examiner always knows to stick that side on the
bottom when inserting it into the cell.
c) Thorax
i. The piston is made of austenitic stainless steel which must fit into the cell with a tolerance of not
more than 0.1 mm.
ii. The base of the piston must be completely flat and perpendicular to the
axis main.
iii. The piston must be equipped with an air vent in the form of a flat
part wide (3.0 ± 0.3) mm on one side.
iv. The top of the piston is equipped with a protruding outer part, so that when the piston is inserted into
the cell and the protruding part of the cell is in contact with the top of the cell, the distance
between the bottom of the piston and the top of the disc must be (15 ± 1) mm.
d) The filter paper must have medium airflow resistance, be circular in shape with flat edges and have
the same diameter as the inner diameter of the cell.
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e) Manometers
The manometer is made of U-shaped glass tube with an outer diameter of 9 mm, as shown in Figure 3.
The top of one of the arms must be able to form an airtight connection with the permeability cell. The
manometer arm connected to the permeability cell must be marked with a line encircling the tube at a
distance (125-145) mm below the top drain, as well as other lines at a distance of (15 ± 1) mm, (70 ±
1) mm , and (110 ± 1) mm above the line.
The exhaust shall be located at a distance (250-305) mm above the base of the manometer, used
for emptying the air in the manometer arm which is connected to the permeability cell.
The manometer shall be provided with a positive airtight valve or clamp located not more than 50
mm from the manometer arm.
The manometer must be securely attached so that the arms are perpendicular.
Figure 3 ÿ Blaine tool
f) Manometer fluid
The manometer must be filled up to the line in the center of the tube with a non-volatile, non-
hygroscopic, low-viscosity and low-density liquid.
such as dibutyl phthalate (dibutyl 1,2 benzene dicarboxylate) or light type mineral oil.
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g) Time keeping device
Timers shall be equipped with start and stop buttons, and shall be readable to 0.5 seconds or less.
For the time range from 0 seconds to 60 seconds. Timers must have a maximum accuracy of 0.5
seconds, and for times ranging from 60 seconds to 300 seconds must have an accuracy of 1% or less.
(2) Other equipment. a.
Suitable small funnel.
b. Small soft bristle brush (No. 7).
c. Weighing cup. d.
Analytical balance conforming to specification.
7.2.2.1.2 Equipment calibration
7.2.2.1.2.1 Standard cement samples
For calibration of the blaine tool, standard cement from NIST must be used, Standard Reference Material No.
114. The cement sample must first be adjusted to room temperature.
7.2.2.1.2.2 Determination of cement bed volume
Determination of the volume of the cement layer is done by moving the mercury as follows:
a) Put two pieces of filter paper in the shape of a circle in the cell with a slightly smaller diameter than the cell,
until all the filter paper is flat on the metal plate then fill the cell with mercury, ACS quality or better, to
remove air
bubbles adhering to the walls cell.
Use tongs (pliers) when carrying cells. If the cell is of a material to be amalgamated with mercury, the inside
of the cell must be treated with a very thin protective layer of oil before adding the mercury.
Then fill the cell with mercury.
Level the surface with the top edge of the cell using a glass plate that is pressed gently against the
mercury surface, making sure there are no air bubbles or voids between the mercury surface and the
glass plate.
Remove the mercury from the cell, weigh and record the weight.
Remove one of the filter papers from the cell, then on top of the filter paper that is left behind is filled with
a layer of cement made by inserting approximately 2.80 grams of cement (no need for standard cement)
then placing the filter paper that was removed earlier on top of the cement.
Then press the cement layer with the piston until the piston neck contacts the cell surface.
NOTE The cement paste preparation must be solid. If it is too loose or the cement cannot
be pressed down to the bottom with the desired volume, then in this case, adjust the
amount of
cement used in the experiment. The empty cell space above the cement layer is then filled with
mercury, and the surface is leveled in the manner above. Take out the mercury, then weigh it
and
record the weight.
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b) Calculate the volume of the portland cement bed to the nearest 0.005 cm 3 with the formula:
Wa - Wb................(1)
V=
D
Information:
V is the volume of the portland cement layer, cm 3;
Wa is the weight of mercury required to fill the cell without cement

coating portland, grams;
Wb is the weight of mercury required to fill the empty portion of the cell
occupied by a layer of portland cement, grams. 3
D is the density of mercury at the test temperature, gram/cm .
c) The determination of the volume of the portland cement layer must be carried out at least twice, and
for each determination the cement layer must be compacted separately. The cement layer volume
price used for the average calculation must be derived from two determination prices with a maximum
difference of ÿ 0.005 cm3. The room temperature around the cells should be recorded at the
beginning and end of the experiment.
7.2.2.1.2.3 Sample setup
Place the standard cement sample from the ampoule into a vial of approximately 120 volume, shake
3cm vigorously for two minutes to break up any lumps. Let the bottle stand and cover for two minutes,
then open the lid and stir gently, to distribute the particles which must be homogeneous.
7.2.2.1.2.4 Standard sample weight
The standard sample weight for calibration must be taken in such a way as to obtain a standard layer of
cement having a porosity of 0.500 ± 0.005 and calculated by the formula:
W = ÿ v (1 – e )….....(2)
Information:
W is the required standard sample weight, grams; ÿ
3
is the density of the portland cement test sample, the value used is 3.15 Mg/m or 3.15 g/
cm volume of sta3n; dard cement layer determined in the manner described in 7.2.2.1.2.2,
v cm is the desired standard cement layer porosity (0.530 ±0.005).
3;
NOTE Porosity is the ratio of the volume of voids to the total volume in the cement layer.
7.2.2.1.2.5 Preparation of cement layer

Place a metal disk on the bottom of the cell, place a piece of filter paper on top of the metal disk and then
press down with a rod slightly smaller than the diameter of the cell, so that the plate and the filter paper
are in proper position.
Weigh a quantity of cement with an accuracy of up to 0.001 gram whose weight is determined according
to the above calculation, in point 7.2.2.1.2.4, and put it in the
cell.
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Gently tap the outer cell wall to even out the cement layer inside.
Place a piece of filter paper on top of this layer of cement and then press it with the piston until the
piston neck contacts the cell surface.
Pull the piston slightly up, rotate 90 degrees, press again then slowly piston
pulled out of the cell.
7.2.2.1.2.6 Determination of the permeability of the cement

layer Each time the determination of the permeability of the cement layer must be used new
filter paper. a) Connect the permeability cell to the manometer tube with an airtight connection in
such a way that it does not interfere with the cement layer that has been prepared earlier
(NOTE 1).
NOTE 1 Apply a little grease to the manometer connecting valve, close one of the
manometer arms, open it slightly then close it again. The continuous pressure drop indicates
a leak in the system.
b) Slowly remove the air in one of the manometer tubes until the manometer fluid reaches the upper
line mark, then close the valve tightly.
c) Run the timekeeping device when the bottom of the liquid reaches the second mark from the top,
stop when the bottom of the liquid reaches the third mark. Record the observed time range
(seconds) and test temperature (oC). d) In calibrating the blaine tool, at least three times
determine the flow time, and each time use a different standard cement layer. Calibration should be
carried out by the old tester performing the smoothness test (NOTE 2).
NOTE 2 Samples are cleaned of brush hairs and reused, provided they are looked
after dry and all tests are carried out within 4 hours of opening the sample.
7.2.2.1.2.7 Recalibration The

blaine tool must be recalibrated if: a) At a
certain time interval, which is necessary for correction of possible wear of the piston or cell
permeability.
b) There is a loss of fluid in the manometer. c) If
required, another type and quality of filter paper.
N O T E I t i s a d vis a b l e to p re p a re a d u s e s e c o nd a r y st a n d a rd w h ic
t o c a lib r a t e th e a p p a ra tu s b e tw ee n ca l ib rati o n s w it h s ta n d a r d ce m e n
h is us e d a s a fineness standard
t s am p le s .
7.2.2.1.3 Procedure
a) The temperature of the cement sample being tested must be the same as the room
temperature at the time of the test b) The weight of the sample to be tested must be the same as
the weight of the standard cement for calibration as described in 7.2.2.1.2.4, unless time
determines the fineness of cement type III or other types the finer ones, whose bulk weight is
so great that pressure with the thumb alone cannot bring the piston neck into contact with the top of the cell.
The required sample weight must be such that the cement sample layer has a porosity of 0.530
± 0.005.
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c) Preparation of cement layer

Cement preparation according to 7.2.2.1.2.2.
d) Permeability testing
Permeability test in accordance with 7.2.2.1.2.6 except in determining the flow time only
once.
7.2.2.1.4 Calculation of specific surface area

a) Specific surface area is calculated using the following formulas:
S= Ss T .................................................. .(3)
Ts
S= Ss
ÿ s
Q .................................................. .(4)
Ts ÿ
S= Ss (b– 3
es) eÿ s
Q .................................................. (5)
3
es Ts (b–e)
S = Ss (b – es) 3
eÿ s
Q .................................................. .(6)
3
es Ts ÿ(b–e)
S = Ss ÿs (b – es) e T3 .................................................. .(7)

ÿ(b–e) 3
es Ts
S = Ss ÿs (b – es) e 3T .................................................. (8)

ÿ
s
ÿ(b–e) es Ts ÿ
3
Information:
2
S sis the2scpmecific surface area of the csteamnednatrdsacmempleenttessatemdp, lcemus/egdrainmc; alibration,

/grams;
Q is the time span of the pressure drop in the manometer for the Portland cement sample tested, seconds;
Ts is the time span of the pressure drop in the manometer for the cement sample
standard used in calibration, seconds; is the viscosity
of the air at the test temperature of the cement sample being tested, poise; is the viscosity of
ÿÿ b
s
e
ice
ÿ
ÿs
Ma c h i n e T9 ranslated
7 /1 7 / 20 1 16103_SNI 2049-
the air at calibration, poise; is the layer porosity of the cement sample being tested; is the porosity of the standard
the testing cement sample layer used in the calibration; is the density of the standard cement sample tested (the value is
temperature set at 3.15);
of the
standard
cement
sample is tgh/emd3ensity of the standard ce3m);ent sample used in calibration (assumed to be 3.15 or 3.15
used for gram/cm is a constant (0.9 for portland cement).
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NOTE Value ÿ , 3
e and T are obtained from Tables 9, 10, and 11, respectively.
1. Equation (3) and equation (4) are used to calculate the fineness of the portland cement sample which
is compressed to the same porosity as the cement sample
s t a n d a r d u s e d f o r
ef(r3 xo )pm ies rt iuhm se ecnd at ilft ibet hrmae p tioe
c a l i b r a ti o n . E q u a t io n
nxr ap ete u x rrpie me aer in md tea enl qtte utme am tpi oep nrea r(ta4ut)rueirfedt.hifefeersx
pbeyriammenatxaiml teumpoefr3atouCre fdroifmfertshebycamliobrreattihoann 3 oC
2. Equation (5) and equation (6) are used to calculate the fineness of the portland cement sample which
is compressed to a different porosity than the standard cement sample used for calibration.
Equation (5) is used when the temperature difference in the calibration experiment is a maximum of
3 oC and equation (6) is used when the temperature of the calibration experiment is different by more
than 3 oC.
3. Equation (7) and equation (8) are used to calculate the fineness of materials other than portland
cement. Equation (7) is used if the experimental temperature differs by ± 3 oC from the calibration
experiment temperature and equation (8) is used if the experimental temperature
differ by more than 3 oC with the experimental calibration temperature.
b) To calculate the specific surface area in units of m /kg, multiply the surface area
2
in cm /gram
2 with a factor of 0.1.
2 2
c) Round the price in cm /gram to the nearest tenth while for m /kg
rounded to the nearest union.
EXAMPLE 3 447 cm 2
/gram rounded up to 3 450 cm 2
/ gram or 345 m 2
/kg.
7.2.2.1.5 Reports
a) For cement and cement-based materials, one determination is sufficient. b) For

each material with high fineness over a long period of time, report the average fineness value
from the two permeability tests provided that the difference is not more than 2%. If the
difference is outside the provisions above, a retest is carried out until the price difference
meets the conditions.
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Table 9 ÿ Density of mercury, air viscosity (ÿ) and ÿ at certain temperature
Room temperature
Specific gravity of Air viscosity, ÿ (µPa.s)
(OC ) ÿ
mercury (Mg/m3 )
2108 13.55 18.08 4.25

22 13.54 18.18 4.26
24 13.54 18.28 4.28
26 13.53 18.37 4.29
28 13.53 18.47 4.30
30 13.52 18.57 4.31
32 13.52 18.67 4.32
34 13.51 18.76 4.33
Table 10 ÿ Cement coating porosity values
The porosity of the cement layer

3e
E
0.496 0.349
0.497 0.350
0.498 0.351
0.499 0.352
0.500 0.354
0.501 0.355
0.501 0.356
0.502 0.357
0.504 0.358
0.505 0.359
0.506 0.360
0.507 0.361
0.508 0.362
0.510 0.363
0.525 0.364
0.526 0.380
0.527 0.381
0.528 0.383
0.529 0.384
0.530 0.385
0.531 0.386
0.532 0.387
0.532 0.388
0.534 0.388
0.535 0.389
0.391 0.391
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Table 11 ÿ Airflow time range

Q Q Q
Q Q Q Q TT TT
T 26 5.10 51 7.14 76
8.77.21810716.1508.0.755115501.2101205.2.219072.120512711742.181,5.837337216212.05.33571.1205
0..21351512457.25 27.5 5.24
52.5 7.25 77.5 8.80 104 10, 20 154 12.41 204 14.28 28 5.29 53 7.28 78 8.83 105 10.25
155 12.45 205 14.32 285..5395.5344 75.355 779.35814.8.75987.15.03878,
178096.3.1540861.4591.7204.21303.805131506.24.03187925.145597.832.49102262.89510.745.8235.059
.484239109
10.44 159 12.61 209 14.46 30.5 5.52 55.5 7.45 80.5 8.97 110 10.49 160 12.65 210 14.49
31 7.48 81 9.00 111 101.5642 121.71322.6192
212141.53161434.52.53593.63162.5.555.167,01.7.5605828.17526.5749..7510.265.88118.3252.115940.90
.16.304381.6111362133413102.5.787
5.74 58 7.62 83 9.11 115 10.72 165 12.85 215 14.66 33 .5 5.79 58.5 7.65 83.5 9.14 116
10.77 166 12.88 216 145..7807 3549.5 873.751986740..65789.78.15498915.
198.2121073.18516.9051.185602.89.916116267.10961.65922.7191.3278.8021018475.27.1569493.17.524
35.83.19042.50
10.95 170 13.04 220 14.83 36 6.00 61 7.81 86 9.27 121 11.00 171 13.08 222 14.90 36.5
6.04 61.5 7.84 86, 5 9.3101.1029211713.0153.15122112.1364.
1157.204231431.14.59.9627.21382716652..0.1580762.971. 87.85799.3.363112243
5.57 56
38 6.16 63 7.94 88 9.38 125 11.18 175 13.23 230 15.17 38.5 6.20 63.5 7.97 88.5 9.41
126 11.22 176 13.27 232 15.23 39 6.24 64 8.00 89 9.43 127 11.27 177 13.30 234 15.30
39.5 6.28 64.5 8.03 89.1529
4161.1326811719.311131.13.4780821138380.311453.24.4321421045.450.356161.5348.6401966154.33.1
.5248586..1520249829.9011065.959..550964.9541.14139.15 0
6.44 66.5 8.15 91.5 9.57 132 11.49 182 13.49 244 15.62 42 6.48 67 8.19 92 9.59 133
11.53 183 13.53 246 154.3686.4526.5686.85.25679.35 98..6242 19325, 5119..6622 118354 1131..6508
215804 1153..8516 248 15.73
6.40 66
43.5 6.60 68.5 8.28 93.5 9.67 136 11.66 186 13.64 252 15.87 44 6.63 69 8.31 94 9.70
137 11.70 187 13.67 254 15.94 44.5 6.67 69.5 8.34 94.5 9.72 138 11.75 188 13.71 256
16.00 45 6.71 70 8.37
9.797.7154013191.1813.71910.18817931.179381.7215630.2851289626.16.52.09416.68.42615.917.54842
67..1571586.9..7482032.159796182..9541.038.0.9845616.451
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264 16.25 47 6.86 72 8.49 97 9.85 143 11.96 193 13.89 266 16.31 47.5 6.89 72.5 8.51
97.5 9.87 144 12.00 192471031.963.42364881.56.613.679.64987346.9.59738..075037
7894.1854.845..06940.929279.9419041.691654.155215.41047289.10.15249.761.2901541.91707340..952
672
8.63 99.5 9.97 148 12.17 198 14.07 276 16.61 50 7.07 75 8.66 100 10.00 149 12.21 199
14.11 278 16.67 50.5 7.11 75.5 8.68 100.5 10.02 150 12.25 200 14 .14 280 16.73
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7.2.2.2 With turbidimeters
7.2.2.2.1 Equipment
7.2.2.2.1.1 Standard equipment
The main Wagner turbidimeter consists of a light source maintained at a constant intensity and adjusted so that a
parallel beam of light passes through the cement suspension under test and strikes a sensitive photoelectric plate.
The electric current generated by the cell is measured by a micrometer and the reading indicated is a measure of the
turbidity of the suspension. The main estimates indicate that turbidity is an intermediate measurement of the surface
area of suspended cement samples. The apparatus shall consist of the specific parts described in 7.2.2.2.1.2 to
7.2.2.2.1.7 and shall be assembled in accordance with the complete design and dimensional requirements as shown
in Figures 4 through 7 and Table 12, except for those made of wood or metal.
Figure 4a ÿ Front view of the turbidimeter with the door open
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Perx,1atur Hn•J i ieci
0 0
3-6 CP
Tangki
Lanpu dengan tilanen ygng terkonssntrasi
se dimentasi dengan r etleMor 6 Ohm
Pelindung !ogam ’69¥ l9l
CATALAN Bagian luar laci dan bagian dalam lemari harus dicat hitam
Figure 4b ÿ Front view of the turbidimeter with the door open
RheosiMs
Tampa b beIaFang
Figure 5 – Rear view of the turbidimeter
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Rheostats
7ampa k belaksng
Figure 6 – Time burette
T ngki sedimentasi
Pelindung
FiHcr
Batere 6 V atau sumber Iain dengan emf

Tel air
konstan
3-6 CP lamp dan retlectcr
6 ohm r heoslat
Mikroameter
30 Ohm rheostat
Figure 7 – Turbidimeter electrical system
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Table 12 ÿ Dimensions of the turbidimeter apparatus

Units in millimeters
Caption Dimension
A 445
B 438
C 381
D 105
E 3.0
F 28.6
G 85.7
H 33.3
I 102
J 39.7
K 55.6
L 65.1
M 28.6
N 3.0
O 51
P 51
Q 3.0
R 61.1
S 69.8
Q 51
u 22.2
V 34.9
W 13
X 38
Y 15.9
Z 38 ± 0.76
AA 51 ± 2.5
AB 267
air conditioning
…..
AD ……
E 39.7
AF 55.6
AG 66.7
AH 203
AI 23.6 A
AJ 1.38
A
AK cm
NOTE A
The figure
is the actual number which is the part of the goal and the
number connecting the parts; consequently unrelated to column
headings.
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7.2.2.2.1.2 Turbidimeters
Installed in a wooden or metal box with the following features:
a) Light source
The light source in FIG. 4b consists of an electric lamp with filaments concentrated
between (3-6) candela operated by a source with constant emf. The lamp must be
firmly installed in the socket. A clean, shiny parabolic metal reflector must be mounted
firmly across from the lamp, focused so that an approximately parallel beam of light will
pass through the sedimentation tank and strike the photoelectric cell. The light intensity
shall be adjusted by means of two reastats of approximately 6 ohms and 30 ohms and
the reastat shall have such characteristic that a large uniform change in light intensity is
obtained over the full range of the resistance.
Reostats must be installed in parallel with each other and in series with the lamp.
b) Heat absorbing equipment
Light must pass through a device to absorb heat before entering the sedimentation
tank as long as the heat radiation from the light beam must be absorbed, the
equipment can be: i. water cell or; ii. heat-absorbing special glass filters.
The water cell shall be constructed of seamless brass tubing having an outside
diameter of 76 mm, a wall thickness of 3 mm and a length of 102 mm with a glass
window taped to the end. The cell must have an opening for distillation water filling. The
hole must be closed with a metal plug. The cell when mounted on a movable stand has
a cover in either the top or bottom position. The heat absorbing apparatus shall be
arranged so that all the light beam from the lamp entering the sedimentation tank
passes through the heat absorbing apparatus.
c) Tool for inhibition
Glass for reducing light shall be provided to reduce the light intensity from 100 µA to 20
µA to 30 µA. The light intensity shall be reduced uniformly in all parts of the cell
exposed to light during the test. The restraint device shall be mounted in a frame which
can be swung out of the way
light path by means of a holder.
d) Sedimentation tank
The sedimentation tank must be:
i. Cemented or bonded (5– 6) mm glass plates or borosilicate

glass together to form a square or tank; ii. A printed glass tank
having a wall thickness of approx. 5
mm with a flat surface.
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The dimensions of the tank must be 51 mm long, 38 mm wide and 203 mm high. The
allowable variations for the dimensions in the tank are ± 2.5 mm in length and ± 0.76
mm in width. The 51mm tank faces shall be evenly spaced by 0.25mm at all points. A
mark shall be placed on the side of the tank to indicate the fill volume of 335 mL which
is the limit for the tank's contents during the test. A tank filled with clear kerosene to the
mark and placed in a light beam turbidimeter will produce a uniform microameter
reading of
±0.1 ÿA, for the entire usable portion of the tank.
e) Photoelectric cell
The apparatus used to measure light intensity must be a sensitive photoelectric cell
connected directly to the micrometer. A cover with horizontal slots 13mm high, 35mm
wide shall be mounted over the photoelectric cell. The front of the cover should be (25
± 1) mm in front of the face of the cell.
The cell face shall be parallel to the tank face by 0.5 mm.
f) Protector
The metal guard uses a slot 16 mm high, 38 mm wide. It must be placed between
the heat sink and the sedimentation tank.
g) Lifting device
The light source, heat sink, photoelectric cell, filter block and shield shall be assembled
on a movable base which can be raised or lowered by two interconnected screws and
can be accurately adjusted so that the turbidity of the suspension can be determined at
the desired depth. wanted. The center of the light source, the heat sink, the photocell,
the slot
center of the metal shield, and the cover must be in a straight line parallel to the
mount. The sedimentation tank shall be mounted on a platform which is not affected
by the
equipment housing so that the tank is free from vibration caused by the movement of
the seat. The mounts must be level at all upgrade points and the tank must be normal to
the mounts. The distance between the tank and the seat opening surface shall not vary
by more than 0.4 mm between the “30 – 50” and “0” positions. The level of the light
beam with reference to the solution surface is indicated by a pointer that will move along
the scale attached to the box. Point 0 on the scale indicates the position where the
centerline of the hole for the light beam is at the same level as the liquid level in the tank
when it is filled to the limit of 335 mL. The lines on the scale are marked with 7.5; 10; 15;
20; 25; and
30 to 50 indicate the suspension depth numbers, h, in Table 13. The scale when
compared with a standard scale to the nearest 0.1 mm at all points shall not show a
deviation at any
point greater than 0.25 mm and indicate the position where the pointer is located at
the time the turbidity reading for the value h is taken.
Interiors of turbidimeter cabinets and outer mounting surfaces, parabolic reflectors, heat
absorbers, shields, photoelectric cell enclosures shall be painted solid black.
NOTE The 0-50 marking requirement on the scale is used only for new turbidimeters and not
for used equipment that meets the other requirements of this method.
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7.2.2.2.1.3 Microameters
a) D'Arsonval type micrometers have a range of 0 µA – 50 µA and must read up to 0.1 µA.
The new microammeter must be accurate to ±0.5% of the full scale value for the value
part of the scale on the part of the scale at 25 oC. For microameters that have been
used, the accuracy must be the same as the new instrument except that the accuracy at
40 µA and 50 µA must be ± 1% of full scale. The internal resistance of a micrometer is
between 50 ohms and 150 ohms. The micrometer shall not be installed on a work
surface containing or composed of iron or steel, or in close proximity to magnetic
influences.
b) Digital micrometer
NOTE An apparatus with a range of 199.9 µA can be used and allows the operator to read the
theoretical Io directly without the use of additional equipment. The high internal resistance of the digital
micrometer should not affect the linearity of the reading at light intensity levels encountered in fineness
determinations using a Wagner turbidimeter.
7.2.2.2.1.4 Current source
A 6V car battery and emergency light battery or emf source can be used as sources
current.
7.2.2.2.1.5 Sieve
The sieve must meet the requirements in the test method ASTM C 430-08, Standard
Test Method for Fineness of Hydraulic Cement by the 45-µm (No 325) Sieve.
Mixing
7.2.2.2.1.6 equipment
Mixing equipment shall consist
of:
a) A cylindrical brush, 19 mm in diameter and approx. 45 mm in length with a tip fitted
approx. around the bottom of a test tube with a diameter of 22 mm.
b) Other agitation equipment equally efficient in dispersing as measured using the
specific surface determination for a standard sample. The mixing equipment should
rotate at a speed of approx. 3 500 rpm.
7.2.2.2.1.7 Time burette
T he tt lin g ti m e o f p ar ti c le s o f d i f fe r e n t s i z e s
ke r osen e . Th e b u re t te s h a ll c o n s i s t o f a g l a s s
c a n b e o b ta in e d b y u s i n g b u re t te f il le d w it h
tu b e w it h a c a p ill a ry t u b e at th e l o w e r e nd . T he top of the
burette must be large to function as a funnel to put kerosene into the tube. The burette must
meet certain dimensions given in Table 14. The lines on the burette must be round (circular).
A 45 ÿm wire mesh (No. 325) may be used with the burette and the burette should be closed
when not in use.
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7.2.2.2.1.8 Scales
Must meet the requirements in 7.2.1.2 point b).

2
Table 13 ÿ h, d and h/d values used in the calibration of turbidimeter equipment
Particle diameter,d (µm)

Suspension depthof, h 2
h/d
50 45 40 35 (cm) 15 15 15
30 25 20 15 15 15 13.1 10 0.006 00
10 7,5 6.6 3.3 2.1 0.007 41
0.009 38
0.012 24
0.016 67
0.0210
0.0250
0.0293
0.0330
0.0373
Table 14 ÿ Burette dimensions
Dimensions, allowable Variation,

Description cm cm
Tube length (large) 38 ±4
Tube inner diameter (large) 1.9 ± 0.2
Capillary length 17.5 ± 2.5
Capillary diameter 0.09 ± 0.005
Mark 0 at the top of the burette 7 ±1
7.2.2.2.2 Materials
Clear kerosene
suspending liquid can be used for turbidimeter equipment. Kerosene cannot be reused.
7.2.2.2.3 Test object
Size of the test sample
Selselcigt hthtley bsieztewoefetnhe12ceµmA etont2s0aµmAp.le for testing so that the initial microameter reading
NOTE The following estimates will help quickly in sample size selection: 0.25 gram for normal
cement fineness and 0.2 gram for high fineness cement.
7.2.2.2.4 Calibration of turbidimeters
Calibrate the turbidimeter equipment according to the procedure below:
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7.2.2.2.4.1 Calibration of the burette
For burette scale calibration, use kerosene whose viscosity and specific gravity are known at
the temperature at which the calibration is carried out. Specific gravity and viscosity of kerosene
must be determined. Calculate the flow time from the burette in relation to the settling time for
different particle sizes using the following equation:
t = [1 837 000ÿ/(ÿ1- ÿ2)] x (h/d2)
Information:
t is the tsimetetlionrgflow time in seconds; is the viscosity of kerosene at
calibration temperature, p; is the specific gravity of 3the cement particles
ÿÿ1 _ (gram/cm (NOTE 1); ÿ2 is the specific gravity of kero)s=en3e.1a5t ftohreportland
cement calibration temperature, Mg/mh is the depth of suspension relative to
the light level in cm; d is the particle diameter, ÿm. ;3
2 2
Figures h/ given in Table Value h, d and h/d used in calibration
d Turbidimeter equipment (Table 13).
Fill the burette with kerosene at the calibration temperature, start timing as soon as the
kerosene in the burette passes zero, and mark on the burette the level reached by
decreasing the kerosene for each time interval, t, calculated as described above. For
these markings, give a permanent line and the number on the burette indicates the
corresponding diameter (NOTE 2). The construction and division of the burette must be
made in such a way that at the calibration temperature the time required for the kerosene
to pass through the line on the burette corresponds to the calculated settling time within
1%, except for variations which are allowed not to be less than 1 second.
NOTE 1 The specific gravity of portland cement should not vary too much and for this work it is
assumed to have a constant value of 3.15. A variation of 0.15 from this value when substituted
using Stoke's law gives a variation of 2.5% for the measured particle diameter.
NOTE 2 By using a calibrated burette the apparatus can be used within the normal range of
room temperature without further correction, the change in the kerosene flow rate from the
burette automatically compensates for the change in the viscosity of the suspension.
o
The temperature of the suspension and kerosene in the burette must be maintained the same C.
within 0.5. This condition will exist if the supply of kerosene is maintained in the same room as
the
equipment. It is necessary to ensure that only clear kerosene is used in the burette, and in addition
the capillary tube must be checked frequently to ensure that there are no pieces of gauze or other
material clogging it.
7.2.2.2.4.2 Calibration of 45 ÿm sieve (No. 325)
Calibration shall be made using ASTM C 430-08, Standard Test Method for Fineness of
Hydraulic Cement by the 45-µm (No 325) Sieve, which is based on correcting the percentage
of sieve on the difference between the test residue obtained and the resulting residual value
obtained indicated by electronically formed sheet sieves the fineness specified for the standard
sample, expressed as a percentage of the remaining test.
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7.2.2.2.4.3 Correct determination of light intensity, I a) b) For

turbidimFiell ttehres seeqduiimppeendtawtioitnh taandkiguitapltmo
itchreoammaerktewr iwthithcleaar kerosene.
range of 199.9 ÿA, place a sedimentation tank containing clear kerosene on a tank support in
the turbidimeter. Adjust the light intensity so that the microammeter reads 100.00 µA.
Adjust the light intensity again until a balance is reached at this reading. Place the blocking
filter in the beam path.
When equilibrium is obtained, record the reading of the measuring instrument as Ir.
The meter reading becomes the reference value for the light intensity. Measuring
instrument readings are also taken at the beginning and end of each test through its own
slow filter lamp to check the requirements of 7.2.2.2.5.2 point (3)h).
c) For turbidimeters equipped with a D'Arsonval type micrometer, place a sedimentation tank
filled with clear kerosene above the tank support in the turbidimeter.
Adjust the light intensity such that the microameter shows 50.0 µA with
the light blocking filter removed/moved out of the light path. Adjust the light intensity again
until a balance is reached at this reading. Connect a resistor or combination of resistors as
illustrated in Figure 4a so that the meter reading is reduced to an equilibrium value between
23.0 µA and 25.0 µA. Increase the beam intensity so that a balanced beam reading is
obtained between 23.0 µA and 25.0 µA exactly doubled. Adjust the light intensity again
until balance is reached at the level of the meter reading doubled. Place the light reducing
filter on the beam path. Remove the resistor from the measuring circuit. When the balance
is obtained, record the reading of the measuring instrument as Ir. This value becomes the
reference value for the intensity of the light. Adjust the reostat at the start of each test to
give the gauge reading through the filter plus a clean kerosene tank.
This gauge reading corresponds to a 100.00 µA gauge reading through a tank containing
clean kerosene using a lamp filter removed from the lamp path. The measuring instrument
readings are also taken at the beginning and end of each test by means of its own light to
check the requirements of 7.2.2.2.5.2 point (3)h).
NOTE 1 A ½ watt carbon resistance with a 5% tolerance limit can be used to obtain the
desired gauge reading. The shunt resistance or combination of resistors shown in Figure 4a
has a resistance value between 85% and 100% of the internal resistance value of the meter
printed on the card in the meter cover. The series resistance has a resistance value equal to
the difference between the internal resistance of the meter and the calculated resistance of the
gauge and shunt combination.
NOTE 2 Not quite certain but still acceptable test method for determining the setting of the
measuring instrument with respect to a current of 100.0 µA through the meter with the
beam
filter removed from the beam path can be obtained by removing the series resistance in the
measuring circuit. The internal resistance of the photocell is large enough to cause a small
error of about 0.5% of the desired setting when the series resistance of the circuit is neglected.
d) Example: If the internal resistance of the tool is 90 ohms, and the measuring tool is coupled
to a 470 ohm resistance in parallel with a 100 ohm resistance, the combined resistance of
the measuring device and displacement, will be reduced to 43 ohms. This will reduce the
meter reading, from 50.0 µA to the calculated value of 23.9 µA.
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7.2.2.2.4.4 Determination of the value of K in the specific surface equation
Determine the K value for the specific surface equation in 7.2.2.2.7 item (1) by dividing the
specific standard sample surface given by the value obtained for the statement in [ ]. Repeat this
calibration procedure 2 more times. The average of the three K values.
7.2.2.2.4.5 Calibration frequency
The turbidimeter must be calibrated 6 months before testing the semen sample.
NOTE The three K values (before averaging) set during calibration should not vary by more than
1.5% of their average values.
7.2.2.2.5 Procedure
7.2.2.2.5.1 Sieve determination

Place 1 gram of cement gradation sieve no. 325 (45 ÿm). Record the percentage of cement that
passes the sieve as r.
7.2.2.2.5.2 Suspension preparation
(1) Sample dispersion

a) Put the cement sample into the test tube together with (10-15) mL of kerosene and 5
drops of dispersing agent, namely oleic acid or lin oil which has been stored for a long
time (NOTE 1).
b) Stir the mixture for 1 minute with a stirrer. c) Then transfer

to sediment tank
d) Wash the stirrer and tube and tube with clear kerosene and put the wash in the sediment
tank.
e) Add kerosene in the tank to exactly 335 mL (NOTE 2).
NOTE 1 Oleic acid must have a grade with bj between (0.948 – 0.953) gram/cm affecting
the visco3s.itTyhoef kdeisrpoesresnineg. Daigsepnetrsminugstmbaetelirgiahltsawndill
hcahvaengliettlewhoer nnostionrfeludefnocrea long time or exposed to heat or light.
Therefore it must be stored in a dark glass bottle and tightly closed. Dropper bottles should
be emptied, cleaned, dried and refilled periodically. Where if oleic acid is less able to
disperse or if foam appears in suspension (there may be a little water in
the kerosene) then lye oil that has been stored for a long time should be used as a
dispersing agent. The same dispersing agent shall be used for instrument calibration
and
fineness determination.
NOTE 2 It is important that the limit of the liquid in the tank is equal to the 0 mark on the
apparatus, this corresponds to a volumeoobftasiunsepdeunsiinogn a
pgprarodaucahteindgc3y3li5ndmeLr .wThhicishcisan be calibrated to obtain 335 mL of
whole kerosene increasing the volume of the suspension; or by using a meter consisting
of a flat plate approximately (50 – 63) mm about center to which a metal pin of specified
length is attached vertically, when the plate is placed in position over the tank, the pin
point is at the 335 mL level. Both methods must ensure that the liquid limit is within 1/10
mm.
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(2) Mixing suspension

Just before the tank is put on the beam road, shake it first so that the suspension is even. Cover
the tank with a glass lid and move it 180° about the horizontal axis through the center of the
tank, rotating the tank up and down approximately every second for 1 minute (NOTE 3). Be
careful not
to let the kerosene run out (NOTE 4).
The suspension is ready to be put into place in the path of the light beam.
NOTE 3 The procedures described for actuating the suspension must be followed
carefully. Procedures for mixing drinks should not be followed.
NOTE 4 The tank cap must be tightly closed so that no kerosene flows out of the tank
surface. The surface of the glass tank must be clean when the suspension is added, and care
must be taken to avoid unnecessary cleaning until the determination is complete.
(3) Turbidimeter operating procedures
Operate the turbidimeter apparatus according to the following operating procedure: a)

Using an inert filter in a sedimentation tank containing approximately 100 mL of clear kerosene in
a light path, adjust the light intensity Ir as described in the light intensity setting procedure Ir
by repeating the reading at interval of 1 minute until there is no change in the number
indicating that the lamp and the photoelectric cell are in equilibrium. Move the tank, check
and record the light intensity.
NOTE 5 To protect the microameter, the lamp is only switched on when the suspension or
slow light intensity reducing filter is within the microameter range. The rechargeable
battery must be disconnected occasionally to reduce the voltage to a fixed value. If the
micrometer shows continuous fluctuation, check for broken lamp wires and photoelectric
cell circuits, make sure that the rheostat connections are clean, and ensure that the lamp,
socket and reflector are properly seated.
b) Weigh the cement sample with a certain weight, and record until the reading is to the nearest
value of 0.000 2 grams. Prepare the suspension according to the procedure above. c)
Place
the shelf limit pointer at the (30-50) ÿm position. d) Fill the burette to a certain height with
kerosene from the lot and the same temperature as the kerosene used in the manufacture of the
suspension,
and start moving the tank containing the suspension in accordance with 7.2.2.2.5.2 point (2).
Continue the oscillatory movement process until the kerosene in the burette reaches the
point zero and stop the agitation process. Immediately place the tank in the beam path
position.
e) Immediately remove the light reducing filter from the light path and close the box
door tool.
f) Read the microameter to the nearest value of 0.1 µA as the kerosene passes
through marks 50, 45, 40, 35, and 30.
g) Raise the rack successively to the 25, 20, 15, 10 and 7.5 marks on the scale, the
micrometer reading at each position being the reading when kerosene is emptied from
the burette.
h) Lower the rack to (30-50) ÿm. Replace the filter in the beam path, move the tank, and check the
intensity of the light. If the microameter reading shows a shift of more than 0.3 µA from
the initial setting through the filter alone, the test shall be repeated.
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7.2.2.2.6 Data recording
For data recording and specific surface calculations, it is recommended to follow Table 15.
(1) Specific surface calculation method
a) Calculate the specific surface using the following equation:
ÿ
S= K r ÿ 2 logs I ÿ
ÿ
ÿ I ÿ
logs ÿ logs I ÿ
5
ÿ ..... .. log I
ÿ
ÿ
9.5logs I
I
ÿÿ 1.5 0.75log 7,5 10 15 45 50 ÿÿ
Remarks: S
is the specific sample surface, m K is the
/kg; 2
calibration factor as described in section 7.2.2.2.4.4; r

is the weight percent of the sample corrected by the sample passing the 45 ÿm (No. 325) (NOTE 1) sieve and I7,5, I10, I 15,
….. I50 is the microameter reading corresponding to the particle diameter of 7.5 ÿm, 10 ÿm , 15 ÿm, ……50 ÿm, ÿA.
NOTE 1 The value of K determined using 7.2.2.2.4.3 is used only for materials having the
same specific gravity
3
as portland cement (approximately 3.15 gram/cm using the derivative
of the equation ,).wFhoicrhovthaerirems
ainteveriraslse,lyfigwuitrhesthaerepaorbtitcaleineddiambaester (ognracmaslcu/clamtions
with
3
).
b) To calculate the specific surface in m2/kg, multiply the surface area in cm

2
/gram with a factor of 0.1.
c) Round the number in cm 2 2
/gram up to 10 units (for /kg to
to the nearest value)
m
For example:
Sample identification: Example
Passes 45 µm (No. 325)r sieve, corrected, T X: 90.4
Calibration factor 33.9
M reading on filter, µA:

Before testing: 17.5
After testing: 17.5
Sample weight, grams 0.25
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Table 15 ÿ Example of recording turbidimeter test data and specific surface calculations
Particle size, ÿm Log I

I, ÿm
A
4550 …….
17.3 1,241 11,,224368
40 17.4 1,253 1,265
35 17.6 1,281 1,303
30 17.9 1,334 1,378
25 18.4 1,408
20 19.1
15 20.1
10 21.6 A
7.5 23.9 …….
25.6 0.75 x 1.408 = 1.056
1.500
Total = 12.857
9.5 x 1.238 = 11.761
Difference =
1.096 /
2
S = ( 33.9 x 90.4 x 0.762)/1.096 = 2131 cm gram
2 2
Round up to 2130 cm /g or 213 m / gram
NOTES:
A
For ease of calculation log I50 and Log I7.5 are recorded in separate columns
(2) Specific surface of the first turbidimeter reading I50.
This method can be used for successive determinations for the same manufacturer, with the same sample
size used, and no significant change in fineness, color or other cement properties. Under these conditions
the specific sample surface can be calculated from the first turbidity reading I50, using the following
equation:
S = c (2 – logI50 )
Information: 2
S is the specific sample surface, m /kg;
I50 is the microameter reading corresponding to a particle diameter of
50 ÿm;
c is the transmittance constant for a given plant.
NOTE 2 The transmittance constant can be evaluated by substituting the above equation given
the known values of S and 2 – log I50 as determined using a complete turbidimeter test.
Averages are
made with a minimum of 5 c values determined from exhaustive testing.
(3) If the fineness of the sample determined by 7.2.2.2.7(2) fails to meet the requirements for fineness, a retest
shall be carried out using the complete procedures of 7.2.2.2.5.2(3), 7.2.2.2.6 and 7.2. .2.2.7.
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7.2.2.2.8 Precision and bias
(1) Single operator precision
The variation of the single operator coefficient is 2.6%. Therefore, the results of 2 tests performed by the
same operator for the same sample, on average, should not differ by more than 7.3%.
(2) Multi-laboratory precision
The multi-laboratory coefficient variation is 3.8%. Therefore, the results obtained from two different
laboratories for the same sample should not average more than 10.6%.
NOTE The figures representing the limits for D1S% and D2S% are described in ASTM C 670-13,
Standard Practice for Preparing Precision and Bias Statements for Test Methods for
Construction Materials.
(3) When no acceptable reference material is suitable for determining the appropriate
bias with this method, it is not created.
7.2.3 Normal consistency test
This test method includes checking the normal consistency of hydraulic cement.
7.2.3.1 Purpose and use
This test method is used to determine the amount of water required to prepare a hydraulic cement paste for testing.
7.2.3.2 Equipment
a) Scales and weights must be according to specification
b) Measuring cup with a capacity of 200 mL or 250 mL, as specified
c) Vicat tool
Figure 8 – Vicat tool
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The vicat tool shall consist of frame A (Figure 8) having a movable rod B weighing 300 grams, one end of
a piston C 10 mm in diameter, spaced at least 50 mm, and the other end a disassembly D needle 1 in
diameter. mm and 50 mm long.
The B-bar is reversible and can be fixed in several positions by screw adjuster E and has an
adjustable, scale-movable F indicator (indicated in mm) which the scale is attached to the A frame.
The cement paste to be tested is inserted into the ring G, which is rigid in the shape of a cone, placed on
a flat plate H which does not absorb water, the width of each side is ± 100 mm.
Rod B is made of stainless steel having a hardness of not less than 35 HRC and must be straight with
the tip of the piston perpendicular to the axis of rod B. Rings made of non-corrosive, non-absorbing
materials have an inside diameter of 70 mm at the bottom and 60 mm at the top. with a height of 40 mm.
In addition to the provisions mentioned above, the vicat tool must comply with the following specifications:
a. Movable bar weight (B) b. Diameter of piston rod end (C) c. Needle diameter d. Inside diameter of bottom
ring e. Inside diameter of the top ring f. (300 ± 0.5) grams.
(10 ± 0.05)mm. (1 ±
0.05)mm. (70 ±
3)mm. (60 ± 3) mm.
(40 ± 1)mm.
ring height g.
The division of the scale
The division of the scale, when compared with a standard scale which is accurate to 0.1 mm at
each point, must not show deviations greater than 0.25 mm.
d) Mixing machines, mixers, mixing bowls, and rakes. e) Mixing knife,
triangular knife with straight edge size (100 – 150) mm
7.2.3.3 Temperature and humidity
a) The air temperature around the table where the dry cement is mixed, the mold and the base plate must
be maintained between (20 – 27.5) oC
b) Humidity of the damp room according to 7.2.1.1 point a) and b)
7.2.3.4 Procedure
7.2.3.4.1 Preparation of cement paste
Mix 650 grams of cement with water whose contents have been measured according to the procedure
described in Appendix C.
Place the stirrer and dry bowl in the stirring position on the
mixer. Then put the ingredients in a bowl and mix in the
following way:
Put all the mixed water in a bowl. Add the cement to the water and wait 30 seconds for the mixed water to
be absorbed. Run the mixer and mix at low speed (140 ± 5) revolutions per minute for 30 seconds.
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Stop the mixing machine for 15 seconds and during this time collect the paste adhering to the walls
of the bowl.
Run the mixer at medium speed (285 ± 10) revolutions per minute and mix for 1 minute.
7.2.3.4.2 Printing of test objects
Immediately form the cement paste that has been prepared according to the items as above, into a
ball with both hands (wearing rubber gloves) and throw it 6 times from one hand to the other with a
distance of approximately 15 cm.
Press the pasta ball resting in one hand into the large hole of the vicat ring, held in the other hand.
Take it with one movement of the palm. Place the ring with the large hole on the glass plate, remove
excess paste from the small ring hole in one motion using the edge of a triangular stirring knife, with
a slightly oblique motion towards the top of the ring, smooth the surface, tapping if necessary with
the tip of the mixing knife. slowly.
During cutting and smoothing operations avoid pressing on the paste.
7.2.3.4.3 Determination of consistency
Align the center of the paste in the ring under the slide rod B, stick the end of the slide rod C on the
surface of the paste and lock the screw E.
Then adjust the F indicator to the zero mark of the scale, and remove the slide rod at the latest 30
seconds after finishing making the paste.
The tool shall be free from vibration during the test.

The normal consistency of the paste is achieved when the slide rod penetrates (10 ± 1) mm below
the surface of the paste within 30 seconds of being released. Do the experiment above using different
percentages of water to achieve a normal consistency. Use new cement on each trial.
7.2.3.5 Calculation
The percent consistency is expressed in the water content of the paste and is calculated by the formula:
Wow
%W= Ws
Note: W
is
the consistency expressed in the water content of the paste,
%; Wa is the weight of water, grams; Ws is the weight of dry
cement, grams.
Calculate the amount of water required for normal consistency rounded up to 0.1% and report the
weight of dry cement rounded up to 0.5%.
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7.2.4 Testing of binding time
7.2.4.1 Equipment
a) Scales
Scales and weights must comply with specifications b) Measuring cups
with a capacity of 200 or 250 mL, according to specifications
The air temperature around the table where the dry cement is mixed, the mold and the base plate must be maintained
at (23 ± 3.0) oC. The temperature of the mixing water and the humid chamber was maintained at 23.0 ± 2.0 oC.
The humidity of the laboratory room and the damp room where the test specimens are stored is not less than 50%.
7.2.4.3 Preparation of cement paste
Mix 650 grams of cement with the required percentage of mixing water for normal consistency according to the
procedure described in Appendix C.
In testing it is recommended to use distilled water but in testing referees and joint testing must use distilled water.
The specimen used to determine normal consistency may also be used to determine the setting time with a vicat
needle according to the procedure described in 7.2.4.4.
7.2.4.4 Testing the binding time with a manual vicat tool (method A)
This method is intended to determine the setting time of hydraulic cement using a vicat needle.
7.2.4.4.1 Special equipment
Manual vicat tool (method A) in accordance with 7.2.3.2 point c) and Figure 8.
7.2.4.4.2 Procedure
7.2.4.4.2.1 Printing of test objects
Printing of test objects in accordance with 7.2.3.4.2. Immediately after printing, store the specimen in a damp room
and allow it to set until the setting time.
The specimen shall be in the printing ring based on the H glass plate during the test time.
Samples for setting time and autoclave tests can be prepared from these samples
same.
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7.2.4.4.2.2 Determination of the binding time
Leave the specimen in the damp chamber for 30 minutes after imprinting, then penetrate with a 1 mm
diameter needle and every 15 minutes thereafter (for type III cement every 10 minutes) until penetration is
achieved at 25 mm or less.
For the penetration test, lower the D needle until it is snug against the surface of the cement paste.
Tighten screw E, and set the F indicator to the upper end of the scale. Get it on the zero scale.
Unscrew the rod by quickly loosening the screw E and letting the needle down for 30 seconds, then read
the scale to determine penetration (if the paste looks watery, on the initial reading the descent of rod B
can be slowed down to prevent the needle from bending 1mm).
The distance between penetration points is not less than 5 mm against the inner wall of the mold and
the distance between 2 penetration points is not less than 10 mm. Record penetration testing results.
By interpolation determine the time for which the penetration was obtained by 25 mm. This is the
initial binding time. While the final binding time is when the needle does not appear to sink into the
paste.
Attention :
- During the penetration test the equipment must be vibration free.

- Keep the 1mm diameter needle straight and clean because lumps of cement sticking to the side of the
needle will slow down penetration, if cement sticks to the tip of the needle it will speed up
penetration.
- The setting time is not only affected by the percentage of water temperature used,
the amount of paste received, but also caused by the temperature and humidity of the air.
7.2.4.4.3 Precision
a) Based on the results of experiments by a single operator (within laboratory) standard deviation for initial
binding of 12 minutes in the range (49-202) minutes. The standard deviation for final binding was 20
minutes in the range (185-312) minutes. Therefore the results of tests carried out by the same
operator shall not differ by more than 34 minutes for initial setting and 56 minutes for final setting of
the paste used.
same.
b) Based on the results of a multi-laboratory experiment (between laboratory) the standard deviation for
ppeennggi ikkaat taann aakwhair l a1d6alamhen4i3t dmaelanmit draelnatmangren( t4a9n-

g20(71)85m-3e1n2it) . mSatannitd. aKrardeenvaasisit iu uhnatusikl tests carried out by 2 different
laboratories, the difference should not be more than 45 minutes for initial setting and 122 minutes
for final setting on the same paste.
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7.2.4.5 Testing the binding time with an automatic vicat device (method B)
a) Automatic vicat needle equipment

The apparatus must be equipped with a standard vicat needle. The needle must have a
diameter of (1.0 ÿ 0.05) mm and a minimum length of 50 mm. The total weight that can be
supported by the tip of the needle at the time of measurement is (300 ÿ 0.5) grams. The
instrument shall be capable of automatically completing and recording the penetration
measurement of a test sample at specified intervals of no more than 10 minutes and carry
out each penetration test at least 5 mm from the previous penetration and at least 10 mm
from the inside of the die.
b) Sample print
The cement paste is held in a conical ring with a height of (40 ÿ 1) mm and a
plate movable flat. The test surface has a minimum diameter of (60 ÿ 3) mm.
7.2.4.5.2 Working procedure
7.2.4.5.2.1 Printed sample
Formed rapidly from cement paste, prepared as described in the section on preparation of
cement paste into a ball shape by using gloved hands and tossed six times from one hand to the
other, keeping the hands 150 mm apart. Press down on the ball, hold it in the palm of your hand
until the big end of the conical ring, hold it with the other hand, completely filling the ring with the
paste.
Move the remainder on the larger end with a single movement of the palm. Place the larger
end on a flat plate. Use a sharp trowel and sharp edge to remove excess paste from the top of
the
mold. Holding the trowel at a 30° slope with the leading edge raised and starting closest to the
center of the mould, smooth the paste by pulling the trowel over the top of the mould with a
saw; repeat the procedure for the other half of the surface. Then smooth the surface all the way
to the
top of the omold making steady, complete strokes across the surface using the edge
the drag of the shovel. Repeat the cutting and smoothing steps but at 90° in the previous cut. o
Repeat these steps as needed to create a surface that is level with the top of the mold. Usually
the paste is leveled in two stages, but sometimes up to three if needed. Avoid excessive
pressure and compaction. Because the automatic vicat device refers to the top of the mold rim, it
is very important that the top of the paste surface is uniform and flush with the top of the mold.
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7.2.4.5.2.2 Timing of setup
By following the manufacturer's instructions and completing required instrument calibration

and zeroing procedures. Set the instrument to measure with no less than 10 minutes
(NOTE 1). Place the printed sample in the automatic vicat equipment and start
measurement (NOTE 2).
NOTE 1 Automatic equipment is usually capable of measurements more frequently than once
every 10 minutes and more frequent measurements minimize interpolation.
NOTE 2 The initial setting time according to method A is determined based on the elapsed time
required to obtain a penetration of 25 mm and the final setting as the total elapsed time by which
the needle does not enter clearly into the paste. The end point is determined using a quality
automatic vicat test method that deviates significantly from the end point specified in method A, and
requires standardization for the correct slope.
7.2.4.5.2.3 The range of applicability of a method shall be determined using the average
setting time range of cement used for qualification and standardization, and shall be limited
to
30 minutes greater than the maximum, and 30 minutes less than the minimum.
7.2.4.5.2.4 Calculation and reporting
Complete all calculations down to the closest value of 1 minute, and the report produces
a value that is closest to 5 minutes. The report must indicate that the test was carried out
by method B.
7.2.4.5.3 Performance requirements (qualification) for automatic vicat instruments
7.2.4.5.3.1 Scope
When the time set results of an automated vicat apparatus are used for acceptance or
rejection tests of cement, the method used shall comply with the qualification requirements of
this section. The estimated method consists of specific instrument procedures and printing
procedures meeting the requirements of this International Standard, which are used consistently
by a particular laboratory.
7.2.4.5.3.2 Samples of portland cement required Portland

cement that complies with the requirements specified in the quality requirements of this
standard and those samples when tested according to method A, shall include the
following:
a) Cement has an initial setting time of less than 110 minutes. b) Cement
with an initial setting time greater than 150 minutes. c) Cement with a
final setting time of less than 180 minutes. d) Cement with a final setting
time greater than 210 minutes
NOTE Laboratories are advised to stock up on sufficient cement for further qualification
and standardization.
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7.2.4.5.3.3 Testing
By using the method to be qualified and incorporating the standardized formula as described
in the standardization section, to obtain a single determination of the initial and final setting
times for each of the three cements. On the same day, take contiguous times for setting
determinations according to method A. Make a single determination of normal consistency
for each cement, and apply equal amounts of water to all batches of dummy. Complete three
sets of tests on different days, and repeat the steps in the method. Perform qualification
tests on samples prepared separately from standardization tests.
Calculate the average of three sets of initial and final setting times for each cement using
the method. A time-appropriate method
i n it ia l s e t ti n g q u a li f i c a
B qns euo i tats t iglnin frgio ec tati etm i ox recn tevhre aead lqnu u3e2 i 0r 5fe o m r
t i o n r e q u i r m e n t i f t h
i emni n nueu ttttehie fs ost.h dfLe oAi k deaifw nfeyid sr estha ,nem ac ec pm obl
i s a f f e r e n c e b t w
erertethawson ep ddeo cnthodtemhi n erp gal minea gsev ea wr noaitf fghitnehta hr vel
e n t h e a v ra g e i n it ia l
ea selfeuimnt etaion fl ocgsk retmitt meti esnettghs f otui drms miBen e gwt hmh oiec
dhthAiosd and the corresponding mean for method B is not greater than 45 minutes for any
instance, and the range of three mock tests by method B did not exceed 30 minutes. As an
example of qualification data is given in Appendix B.
7.2.4.5.3.5 Standardization
When standardization is required for the purpose of obtaining agreement between method
A and method B, this may apply to another initial setting time, final setting time, or both. A
standardization formula shall be based on a comparison of the test results obtained using
method A and the method selected using an automated instrument (method B). Test results
from a minimum of five different hydraulic cements are required for standardization. The
cement shall have a minimum range of 60 minutes initial setting time and a minimum range
of 90 minutes final setting time when tested according to method A. If desired, three
cements may be used for instrument qualification, but resulting in a new determination. Use
the same method as used in qualifying the instrument, including all the same steps. The
validation of standardization formulas must be derived mathematically and can be applied to
all examples.
NOTE In general, automated instruments are computer-operated devices, and can easily be
adopted for standardization calculations.
7.2.4.5.4 Re-qualification method
Requalification of a method is carried out at least once a year, and when the
following conditions occur:
a) The instrument is significantly modified
b) The instrument is substantially modified
c) The evidence substantially indicates that the method does not provide
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d) The averages of cement and concrete laboratory reference samples differ from the values obtained using the
method by more than 45 minutes for the initial time or final setting time.
7.2.4.5.5 Accuracy and bias
7.2.4.5.5.1 Accuracy
No precision data are available at this time. It is advisable for a laboratory to develop individual accuracy data for the
methods and instruments used. Based on the qualification requirements, the accuracy of a method should not be
greater than the accuracy of method A.
7.2.4.5.5.2 Bias
Since there is no suitable reference material for determining the bias for the procedure in this test method, no
statements of bias are presented.
7.2.4.6 Testing the binding time with gillmore needles
Gillmore needle kit
The gillmore tool must meet the following requirements: a) Pre-
engaging needle:
- Heavy : (113.4 ± 0.5) grams. :
- Diameters (2.12 ± 0.05) mm.
b) End binding needle:

- Heavy
: (453.6 ± 0.5) grams. :
- Diameters
(1.06 ± 0.05) mm.
The needle should be cylindrical and (4.8 ± 0.5) mm long. The point of the needle should be flat and aligned with the
axis and shaft (see Figure 9).
Figure 9 – The gilmore tool
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7.2.4.6.2 Procedure
7.2.4.6.2.1 Printing of test objects
Form the cement paste into plates of approximately 75 mm in diameter and 13 mm thick on a rectangular glass.
The surface is leveled and the edges beveled (Figure 10).
In making this slab, first place a lump of cement paste on the glass, level the surface then shape the slab by moving
the stirring spoon around in a direction from the outside edge, towards the center of the paste lump.
7.2.4.6.2.2 Determination of binding time
At the time of binding, hold the needle in a vertical position and penetrate the needle "initial" (vertical position).
If the "initial" needle has left no marks on the surface of the mold, record the time and count from the start of mixing
the cement and water as the initial setting time.
Do the above using the "final" needle and count as the final setting time.
Figure 10 – Cement paste slab shape
7.2.5 Expansion test with autoclave
This test method includes determining the autoclave expansion of portland cement by testing the specimen.
Expansion testing by autoclave to determine the potential index of slow expansion due to hydration of CaO,
MgO or both.
7.2.5.2 Equipment
a) Scales and weights, according to specifications. b) Measuring cup, 200 mL
or 250 mL capacity, as specified. c) Print size: (25 x 25 x 285) mm (Figure
11).
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Figure 11 – Prism print
d) Stirring knife, triangular blade with straight edge size (100-150) mm

e) Autoclave, consisting of a steam vessel with high pressure equipped with a wall
thermometer. The autoclave shall be equipped with an automatic pressure regulator and
a burst disc with a burst pressure of 2.4 MPa ± 5%. In locations where explosive
pressure is not allowed using breakable discs, the autoclave shall be equipped with a
safety valve. In addition, the autoclave must be equipped with a discharge valve which
can expel air during the initial heating period and release the remaining vapor pressure at
the end of a cooling period.
The pressure gauge must have a nominal capacity of 4.0 MPa (600 psi), must be
neither larger nor smaller, a dial with a nominal diameter of 115 mm and must
m0,0e3mpMuPnay.aiKseksaal laahdaanrip(a0d-4a,0p)eMngpuaku(( r0an–ti6d0a0k) bposl ie)hdemnegleabnihpie±m0b,a0g3iaMnPsakaplaadtaidatekkalenbaihn
2 MPa operation.
The capacity of the heating unit must be such that the maximum saturated vapor
pressure load in the autoclave can be increased until the maximum saturated vapor
pressure gauge in the autoclave can be increased until the pressure gauge shows
2 MPa for (45 – 75) minutes from the time the heating starts.
The automatic pressure regulator must be able to maintain the device pressure at (2 ±
0.07) MPa for at least 3 hours. The pressure of the autoclave device must be designed
so that the pressure drop from 2 MPa to less than 0.07 MPa within 1.5 hours after
heating is stopped.
Fragile discs must be made of a material that has a tensile strength that is
relatively insensitive to temperature (20–216) oC.
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f) Long comparison
Long comparators are used
right to measure change in the length of the test object and
memes according to amber 12).
s(pseeceifications
Image 1
– Comparator
7.2.5.3 temperature and humidity an
7.2.5.3.1 Rua temperature g
Keep room temperature, dry en and water per action, according to .2.1.1 but a).
se
7.2.5.3.2 Moisture an
Take care of the chapter in glue room chapter in accordance with 7. 2.1.1 item ).
cat
7.2.5.4
safety alert
a) Pressure gauges must be used ai capacity s 4.0 Mpa ( 600psi). have
Measuring devices with too small or too large a capacity may present a hazard. If the working pressureis
greater athlargtehreccaappaactcietiytsytoeofrftihtsheseiunmrseetrtauhsmautertinhtge,
tiphnoesitnrinutedmricedanottie,ostnhneoofitnj
pdbaiecscasotimtohnerosouftgojhoistshomeuatmlol.afFxsiocmraultehm,isasrncedaalescosnevcetthirosenec.lyu
arrwrueimtnht
arum
b) Pressure gauges must be

tested for proper operation.
used
The thermometer must always be used together with a pressure measuringdevice, the purpose of which
is to compolepteerathtieondaelt.ection of deviations by a pressure measuring device on a current that is
normally
c) Auto pressure adjustingtool tis should work all the time.
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d) Set the safety valve so that it will operate at a pressure of (6 – 10) % above the maximum
pressure of 2.1 MPa, the specifications specified in this test method are approximately
2.3 MPa (330 psi). If the manufacturer provides special instructions regarding maintenance
of the safety valve, follow those special instructions, otherwise check the safety valve 2
times per year. Check that the safety valve is open or set to open at ± 2.3 MPa (330 psi).
Keep the discharge direction of the safety valve away from the tester.
NOTE Unexpected circumstances may occur. For example, in one incident the automatic
pressure regulator failed, the safety valve became stuck and the pressure control indicator which
had shown O suddenly rose beyond the maximum level and stopped in the wrong position. The
condition of the pressure regulator is finally recognized and the pressure of unknown magnitude
is released before tool failure occurs.
e) The tester wears leather gloves to prevent burning of hands when removing the top of the
autoclave at the end of the test, keeping the discharge valve directed away from the
tester.
When removing the autoclave lid, tilt it so that the steam to be released is away from
the tester.
The tester must take care to prevent burns caused by hot water that has been used in
the autoclave.
f) It should be noted that in most autoclaves, the return of the needle to its original point or
to the starting point does not mean that the pressure in the autoclave is zero, there
may still be quite a dangerous pressure remaining.
7.2.5.5 Number of specimens
Make at least one test object.
7.2.5.6 Preparation of test object molds
Prepare the test object mold according to Figure 10.
7.2.5.7 Preparation of test objects
7.2.5.7.1 Mixing of cement paste
Prepare a paste consisting of 650 grams of cement and enough water to get
p a s t o f n
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o r l c o n s i s t e n c y . M i x t h
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e p a s t e m i x t u r e a c c o r d in
t tvdthiene tg tepe rtasmi m tsitcne eaaan ut inso b dene ds orpfef oean rcdo diimr lemy te epan r
g t o th e p r o c d u r d s c r
rlsmec pfoion an rarseta i sodu tntefor noc clm ays v,etehat testi nedp seatitsni mctgere icbt haies
i b e d i n
an d atb iinse as m tilpl le
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Immediately after completing the preparation of the test piece for the setting time test, print the test
piece in two stages. Each stage is compacted with the thumb or forefinger by pressing the paste
towards the corners of the mold and along the surface of the mold, until a well-mixed specimen is
produced.
The surface is compacted, the excess paste is cut flush with the surface of the mold using a stir
knife, and smooth the surface with a few strokes of the stirring knife.
During mixing and printing work both hands are protected with rubber gloves.
7.2.5.7.3 Preparation of test objects
Immediately place the mold filled with pasta in a damp room for at least 20 hours.
If removed from the mould before 24 hours, the specimen shall be kept in a humid room until the
time of execution of the test.
7.2.5.8 Procedure
a) At 24 hours ± 30 minutes after printing, the test specimens are removed from the humid chamber,
immediately measure the length of each test object with a length comparison device and put it
into the autoclave which must contain sufficient water at a temperature of (20 – 28) oC, to keep
steam remained saturated during the test.
b) To allow air to escape from the autoclave during the preheat period leave the discharge valve
open until moisture begins to escape (see safety warning).
Then the valve is closed and the autoclave temperature is increased gradually until a vapor
pressure of 2 MPa is obtained during the time (45 – 75) minutes since heating begins. The
pressure was maintained at (2 ± 0.07) MPa for 3 hours.
At the end of the 3 hour period, the heating was stopped and the autoclave was gradually
cooled down to a pressure of less than 0.07 MPa in approximately 1.5 hours. At the end of the
1.5 hour period, the remaining pressure is gradually released by opening the relief valve until
atmospheric pressure is reached.
Then the autoclave was opened, the test object was removed and then immersed in hot water at
a temperature above 90 oC.
Within 15 minutes, gradually cool the water around the specimen with the addition of cold
water until the water temperature drops to 23 °C.
Keep the water around the specimen at 23 oC for 15 minutes, then dry the surface of the
specimen and measure its length again with a length comparator.
NOTE If a reading is desired at 27 oC it is recommended that the specimens after being removed
from the humid chamber be placed in water whose temperature is maintained at 27 oC for at
least 15 minutes, removed and measured the length of each specimen with a length comparator,
then heated in the autoclave . When finished, remove from the autoclave and cool the specimen
with water to 27 °C in 15 minutes.
Keep the specimens at this temperature in water for as long as then measure the length of
each specimen with a length comparator.
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7.2.5.9 Calculation
Calculate the change in the length of the test object before and after the autoclave test in % (percent)
with an accuracy of 0.01.
Report the percentage increase in length as autoclave expansion. Express long subtraction with a
minus sign in front of the percent.
7.2.6 Determination of the compressive strength of hydraulic cement mortar
This test method covers the determination of the compressive strength of hydraulic cement mortar
using a 50 mm sided cube die.
7.2.6.1 Summary of test method
The dough used consists of 1 part by weight of cement and 2.75 parts by weight of sand.
Portland cement is mixed with water at a certain water-cement ratio.
The dough that has been put into the cube is compacted by stacking when the cube is half filled and
full, the test object is left in the mold in a humid room for 1 day, open the mold in a humid room for 1
day, open the mold and the test object is immersed in water containing lime until the time of testing.
This test method is used to determine the compressive strength of hydraulic cement mortar and the
results can be used to determine whether the cement meets specifications. Furthermore, the test
method is used as reference by a number of specifications and other test methods. Be careful when
the results of this mortar test will be used to predict the compressive strength of the concrete.
7.2.6.3 Equipment
(1) Weights and scales

Scales must comply with specifications. The balance should be evaluated for accuracy and
deviation at a total load of 2 000 grams.
(2) Measuring cup

A graduated cylinder of the specified capacity (preferably one large enough to measure the
water mixture in a single operation) to produce the indicated volume at 20 C. The allowable
variation is ÿ 2 mL. o
The measuring cup can be divided by at least 5 mL, except for the line which can be ignored
for the smallest volume of 10 mL for a 250 mL measuring cup and the smallest volume of 25
mL for a 500 mL measuring cup. The main indicating lines should encircle the measuring cup
and be numbered.
(3) Sample print

For cube molds with a side of 50 mm it must be securely mounted. Prints may not have more
than 3 compartments and be separated into no more than two parts. The parts of the mold
when assembled into one strong unit. The molds are made of strong metal which is not
affected by cement mortar. For new castings the Rockwell Hardness number of the metal shall
not be less than 55 HRB. The sides of the die must have a rigidity that prevents splaying or
bending. The inside of the die must be flat and comply with the tolerances in Table 16.
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Table 16
Variation required out of mold(mm)
print
Print n cubes 5 mm
P ramer Recently used < 0s.u0d2a5 < 0.05 5 0 ÿ n
Flatness of the 0.13 5 ÿ 0.50 50 + 0.25 – 0–.10.5308 +0 00.205
sides
The distance between the sides of opposite sides
0 9 ÿ 0.5 90
Foreign height-each compa mates
Angle an*) between adjacent
ÿ 0.5
surfaces
NOTE N:
*) Measured at the point where even a little from persi food. Measured apart from h for each
the compartmeanllt the inside and adjamceonldt .faces and the bottom right between
twheasinmneorveadnpdabreuttsp m
plane of the
wpdeeern
(4) Mixing machine, stirrer and mang uk stir
De- and bowl-driven mixing machines. Bro, the electric power is equipped only pen stir
See with
Figure 13, Gam DAR 14 and Figure 15 .
Figure 13 Stirring machine
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1 – Eccl duk
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Figure 15 – Bowl
(5) Flow table and flow mold (see Figure 16)
Figure 16 – Flow table
(6) Collider
Made from non-absorbent, non-abrasive, non-brittle materials, such as rubber
compound which has a hardness of 80 ÿ 10 on the Shore A scale or teak wood which is
made non- absorbent, non-abrasive, by immersing it in paraffin for 15 minutes at ÿ 200
oC and must have a cross-section of (13 x 25) mm, a length of approximately (5 – 6)
inches or
(120-150) mm. The face of the pounder must be flat and perpendicular to the handle.
(7) Mixing knife, triangular knife with straight edge size (100-150) mm.
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(8) Engine compressive strength
A compressive strength machine, either hydraulic or screw type, having sufficient opening between
the top compression plane and the bottom anvil to permit testing of various sizes of specimens. The
load used on the specimen must show an accuracy of ± 1.0%. The upper compression plane shall
have a circular seat, a hard metal block firmly attached to the center of the top of the machine.
The center of the circle must be located in the center of the surface of the block when in contact with
the test object. The blocks must fit securely in the circular holders, but must move freely in each
direction.
The diagonal or diameter of the anvil surface should be slightly larger than the cube diagonal of the
specimen to facilitate proper placement of the specimen in the center of the anvil. Hard blocks shall
be used under the specimen to reduce wear on the machine plate.
The ground surface of the block in contact with the specimen shall be numbered
Rockwell hardness of not less than 60 HRC.

The base surface of the block must be completely flat with a slope of not more than 0.013 mm if the
block is new and must be maintained with a permissible variation of 0.025 mm
NOTE The diameter of the base block is 79.4 mm, which is wide enough for testing a cylinder 75 mm x 150 mm,
provided that the base block has a diameter greater than the diagonal of the 50 mm cube but is not larger than 74 mm
and is perpendicular to the base block above and is fixed with the right position.
7.2.6.4 Standard sand
The sand used must meet the requirements contained in Table 17 which aims to assess the source of the
sand and the loss of the characteristics of the air in it which is not desirable.
Table 17 ÿ Standard sand requirements

Assessment
Characteristics, the percentage that passes the Sand 20-30 Graded sand
No. sieve. 16 (1.18mm) 100 100
No. 20 (850 ÿm) 85 – 100
No. 30 (600 ÿm) 0-5 96 – 100
No. 40 (425 ÿm) 65 – 75
5 (3 0 0 ÿm ) 20 – 30
No. 100 ( 1 50 ÿm ) 0–4
Difference in air content of mortar made using 2.0 A) 1.5
washed and unwashed sand, % maximum air
Sand source
Ottawa, 1 L or Ottawa, 1L
Les Suer, Mn
NOTE A)
Compressive strength of portland cement prepared to mixed portland cement specifications, cement reduced
by approximately 4% of each percentage of air in the compacted cube. A total of three washed and three
unwashed sandboxes is required to detect a strength difference of 7% between washed and unwashed mortar
sand.
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7.2.6.5.1 Temperature
The temperature of the air surrounding the mixing board, dry ingredients, moulds, flat plate and mixing bowl shall
be maintained between 20 oC and 26 oC. The temperature of the mixing water, room humidity and water in the
storage tank must be set at (23 ÿ 2) oC.
7.2.6.5.2 Humidity
The relative humidity of the laboratory should not be less than 50%.
7.2.6.6 Test object
For each test, 3 or more specimens shall be made.
7.2.6.7 Preparation of test object molds
a) Using a cloth that has been smeared with grease or oil, make a thin layer on the inside of the mold and the
bottom of the plate that is non-absorbent. Wipe the face of the mold and the bottom of the platen with the
cloth as necessary to remove excess coating and to lighten the inner surfaces. When using sprayed
lubricant, spray
it directly on the mold face and plate bottom with a distance of (150-200) mm to obtain perfect sealing
power. After spraying, if necessary wipe the surface with a cloth to remove excess sprayed lubricant. The
layer that sticks is considered sufficient if the pressure with the finger leaves an impression.
b) Cover the surfaces of the parts to be joined with grease while the two dies are joined. There should be enough
of it when the two halves are held together firmly. Remove excess grease with a cloth.
c) After attaching the mold to the base plate (if the clamp type is bolted) carefully remove with a dry cloth any
excess oil or grease from the surface of the mold and the base plate using a waterproof coating, as a
coating is paraffin, microcritaline wax, or a mixture of 3 parts paraffin and 5 parts by weight of rosin. Melt
the coating by heating between (110 - 120) oC. The outer contact area between the die and the plate base
is made watertight by means of a coating that has been melted.
NOTE 1 Since spray lubricants evaporate, molds should be checked for coating just before use. If
spraying has been a long time, it needs to be sprayed again.
NOTE 2 The use of straight paraffin is permitted if a watertight connection is guaranteed, due to
the low strength of paraffin, if the mold is not bonded to the bottom of the plate, a mixture of paraffin
and rosin must be used. The paraffin and rosin mixture may be difficult to remove when the mold is
cleaned and the joint is watertight, which can be guaranteed with paraffin alone, by slightly heating
the mold and the bottom plate before scrubbing the joint.
The mold mentioned above must be allowed to stand to return to its original temperature.
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7.2.6.8 Procedure
7.2.6.8.1 Mortar composition
a) The proportional ratio of standard mortar is one part by weight of cement to 2.75 parts by
weight of graded standard sand. The water-cement factor was 0.485 for all types of
Portland cement and 0.460 for air-containing Portland cement. The amount of mixing
water for other types of cement is such that it produces a flow rate of 110 ÿ 5 and is
expressed as a weight percent of cement.
b) The quantities of the ingredients to be mixed at the same time in a batch of mortar to
make the six and nine test samples are as follows:
Table 18 ÿ Mortar composition
Material Number of test objects
Cement (grams) 6 9
Sand (grams) 500 1 375 740 2 035
Water (mL)
-Portland 242 359
- Airborne Portland 230 340
- Others (with a flow rate of 110 ÿ 5) --- ---
7.2.6.8.2 Mortar preparation
Mixed mechanically according to Appendix C procedure.
7.2.6.8.3 Flow determination
Wipe, clean and dry carefully the top of the flow table, and place the flow mold in the center.
Place a layer of mortar ÿ 25 mm thick in the mold and pound it 20 times with the hammer.
The crushing pressure shall be such that it fills the uniform portion of the mold sufficiently.
Then fill the mold with mortar and mash as in the first layer. Slice the mortar to obtain a
flat surface, leveling the top of the mold using the straight side of a trowel knife (almost
perpendicular to the mold) in a sawing motion across the top of the mold.
RoWfeitpmheeotvmheeotlfhdloe. wmtoalbdlefroclmeatnheanmdodrtrayr,
1bemininguctearaefftuelrtoworerkmiosvceoamnpylewtea.ter from around the corners
Immediately lower the table 13 mm high 25 times in 15 seconds. Flow is the result of
increasing the average diameter of the mortar pile, measured at least 4 measuring points,
expressed as
a percentage of the original base diameter.
Experiment with mortar varying the percentage of water until the desired flow is
obtained. Every time you do the experiment, use a new mortar.
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a) Leave the mortar in the mixing bowl, mix for 90 seconds uncovered.
During the first 15 seconds, quickly wipe off any mortar adhering to the walls of the bowl.
Then stir again for 15 seconds at medium speed.

As soon as the mixing is complete, shake the mixer to remove the adhering mortar
and place it in the bowl.
b) If duplicates are desired, return the mortar from the running table to the bowl.
Immediately lower it against the wall of the bowl and then mix the whole mixture again
for 15 seconds at medium speed.
After mixing is complete, the mixer should be shaken to remove excess mortar in
the bowl.
c) If duplicate batches are required for additional tests, the flow test is omitted and the tart is left in the mixing bowl for
90 seconds without cover. During the last 15 seconds, quickly wipe off any mortar adhering to the walls of the bowl.
Then mix again for 15 seconds at medium speed, when mixing is complete, agitate
the mixer inward dropping any adhering mortar into the mixing bowl.
d) Start printing the test object with no more than 2 minutes and 30 seconds after finishing
mixing. Place a ÿ 25 mm thick layer of mortar (approx. ½ the depth of the mold) over all
spaces of the cube mold. Impact the mortar in each cubical space as much as (4 X 8)
collisions within ÿ 10 seconds, the collisions in the 2nd round of the next round, must
be perpendicular to the previous collision round and consist of 8 collisions adjacent to
each
other on the surface of the object test, as described in Figure 17. The impact pressure
shall be sufficient to ensure uniform filling of the mold. The collision which consists of
4
rounds (32 collisions) must be completed for one cube before proceeding to the other
cubes. When the mashing of the first layer in all the spaces of the cube has been
completed, fill the cube with the remaining mortar and then pound it as in the first layer.
During pounding layers, try to ensure that the mortar that is sticking out of the mold, is
returned to the mold after each round of pounding is complete, by using gloves. After
each pounding is complete, the top of the cube should be slightly higher than the top of
the mold. Pick up the mortar sticking out of the mold with the trowel knife and level the
mold with the even part of the stirring knife, one time over the top of each cube in a
motion perpendicular to the length of the mould. Then, for the purpose of evening out
the mortar sticking up and making it uniform in thickness, slice the flat part of the stirring
knife again along the length of the mold. Slice the mortar back flat to the top of the mold
by cutting the straight side of the trowel knife (almost perpendicular to the mold) in a
sawing motion along the length of the mold.
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A. First collision sequence B. Tum sequence is not the second a

and third and fourth at
G mbar 17 – That order no
e) Penyi pan the test object
As soon as the printing of the test object is complete, place the test object in the guard
room so that bthoettotemstoofbthjeemctpoilisasttiemaiimnr
beaudhtiaumtmeuliysdtarbofteeormptrhofoeterpcartei(nd2ti0nfr- chapter, an di kaan
go7mi)shdinoriutphrpsei,nmbgyowlpdalatwechrin.icghitisinsctoornetdacotnwtihthe
When the test object is removed from

n before 24 hours, if always
the mold it is in a humid chamber until u
thehteosutrso.btjeesctteirsTshtiellnn 24 hour
test) in saocahkatmhebemr
m(eaxdcepotffmorattheeria2l4that
is not rruosotmy awnadtefirlleydesw. ith saturated lime water, keep it clear if necessary to replacaefrtheesh
store of
water in nature
,
f) Pene Tuan keku tan press
Immediately carry out tests After the test object was removed from the special damping chamber, the 24-
for
hour
spectiemsetsn, stimfoirnogthae
dampingctoemstpfrreosmsivtheeswtraetnegrthatatenndubartiooknefowritthhea
srfaoglloews:
tceesrttawinasamteostuendt foofr
Table 19 ÿ Time tester

tolerance
Examiner age 24 n tolerance give it

required ÿ
hours 3
0.5 hours
ÿ
days 7 1 hour ÿ 3
days
hours ÿ
28 days
12 hours
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If more than one specimen is removed from the damp room at the same time, for a 24
hour test, protect each specimen with a wet cloth until the test is carried out. For tests
with other test ages, if more than one specimen is removed from the immersion water
at the same time
Wtesteipd,ekeeepathce hspescipmeencinimwateernat u(23nÿti2l) tchomeplesteulyrsfuabmceergeidsundtirl

tyheatenst dis craerrimed oouvt. eoaCnaynlodoesaecshatnedstoorbcjeocatrse coating from
the surface which will be in contact with the base of the testing machine block.
Check the surface using a straightedge (NOTE 1). If there are indentations, rub the
surface flat or discard the test piece, periodically checking the cross-section of the
test piece.
NOTE 1 The surface of the test object will be lower than the actual test result if the surface is not
completely flat. Therefore, the mold of the specimen must be kept clean, otherwise an irregular
surface will form. To prevent wear, use a mold cleaner that is softer than the metal of the mold.
In terms of
The surface
object of the
with fine test object
sandpaper or aneeds
cloth to be smoothed,
attached this canusing
to the surface be done bypressure.
a little rubbing the
It istest
difficult
to scrub
the uneven surfaces of specimens larger than a few hundredths of a mm, in which case
the specimens should be discarded.
Apply a load to the surface of the specimen which is in contact with the flat surface of
the mold when printing.
Be careful to place the specimen in the testing machine just below the center point of
the upper block base. Before testing each cube, make sure that the circular seat block is
free to move. Cannot use pads.
The initial load, at the desired compression rate, may be applied up to half of the
maximum load of the specimen which is expected to have a maximum load greater
than
13.3 KN.
Do not apply an initial load to a specimen that is estimated to have a maximum load
of less than 13.3 KN.
Set the compression rate such that the remaining load (or the entire load in the case of
an estimated maximum load of less than 13.3 KN), is applied without interruption, until it
breaks at a compression rate such that the maximum load will be achieved, not less
than 20 seconds, nor more than 80 seconds since pressing started.
Do not make changes to the adjusting device of the compressive strength testing machine
while the test piece is being pressed and has not broken.
NOTE 2 It is recommended to apply a light coating of good quality light mineral oil to the
annular seat of the top block base.
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7.2.6.9 Calculation
Record the total maximum load indicated by the testing machine, and calculate the compressive
strength according to the formula below:
Fm = P/A
Information:
Fm is the compressive strength in psi or
MPa; P is the total maximum load in N;
A is the area of the loaded surface in mm 2
.
For 50 mm cube molds used for determining compressive strength, either using inch-pound units or
International System units. However, the specified units for load and area must be used to calculate
the compressive strength in the units selected. If the cross-sectional area of a die varies by more than
1.5% of the figure, use the actual area for the compressive strength calculation. compressive strength
of
All mold acceptance
averaged tests
and reported made
to the from the
nearest same
10 psi (0.1sample
MPa). and tested over the same period shall be
7.2.6.10 Test object failure and retest
a) In determining the compressive strength, do not worry about prints that are manifestly faulty. b)
The maximum allowable range between dies of the same mortar bath, at the same test time is 8.7%
of the mean value when three cubes represent an age test and 7.6% when two cubes represent
an age test .
NOTE The possible increase in the range is 1 in 100 when the body coefficient varies within
2.1%. The value of 2.1% is the average value for laboratories participating in the portland cement
and cement masonry reference sample program from cement and concrete reference
laboratories.
c) If the range of the three prints exceeds the maximum specified in 7.2.6.10 item b), discard the
results that differ the most from the average and check the range of the remaining printed boxes.
Make a retest of the sample if less than two prints remain after discarding a defective print or
discarding a test that failed to comply with the maximum allowable range of two prints.
7.2.6.11 Accuracy and deviation
The accuracy of this test method is shown in Table 20 and is based on the results of the cement and
concrete reference laboratory of the reference sample program. This precision was developed from
data in which a test yielded the average compressive strength test of three cubes molded from a
single mortar bath and tested at the same age. A real change in accuracy cannot be obtained when
the test results are the average of two cubes, unlike when an average of 3 cubes is used.
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Table 20 ÿ Accuracy
Coefficient
Acceptable range of the test
Portland cement with Age of test of variation 1 sec result in 2 seconds
Water factor: fixed cement (days) %A %A
Lab. Single 3.1 8.7

1 3.9 10.9
3 3.9 10.9
7 28 3.8 10.6
Multi Lab 3.7 10.4
Average. 7.3 20.4
1 6.8 19.0
3 6.6 18.5
7 28 6.5 18.2
Average 6.6 18.5
Mixed Portland cement
Lab fixed mortar flow rate.

Single 3 4.0 11.3
7 3.8 10.7
28 3.4 9.6
Multi Lab 3.8 10.7
Average. 3 7.8 22.1
7 7.6 21.5
28 7.4 20.9
7.6 21.5
Mansory cement
Fixed mortar flow rate
Lab. Single 7.9 22.3
7 28 7.5 21.2
Multi-lab 7.7 21.8
average. 11.8 33.4
7 28 12.0 33.9
Average 11.9 33.7
A NOTES
represent each of (1S %) and (d2s %) as explained in ASTM Practice C 670
The precision statement applies to mortars prepared from cement admixtures, and tested at the ages recorded. The
appropriate limits are usually greater for tests of age
younger and slightly smaller to test at older ages.

The deviation of the procedure in this test method has no deviation, because the values of compressive strength are
defined in the requirements of the test method.
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7.2.7 Rapid stiffness test of portland cement (paste method)
This test method covers the determination of the quick setting of portland cement.
7.2.7.1 Limitation
Fast stiff development occurs early in the working characteristics of portland cement paste, mortar
or concrete. This limitation includes pseudo binding and fast binding.
a) Pseudo-bonding: the expansion to stiffness that occurs early in the working characteristics of
portland cement paste, mortar or concrete without much heat evolution, the stiffness of which
can be removed and plasticity regained by further mixing without addition of water.
b) Rapid setting: expansion to rigidity which occurs early in the working characteristics of portland
cement paste, mortar or concrete, usually with a rather large evolution of heat, the stiffness of
which cannot be removed and the plasticity cannot be regained by further mixing without
addition of water.
7.2.7.2 Summary of test method
The paste is prepared from the cement to be tested, using a quantity of water sufficient to provide
the required initial penetration, as measured by means of a vicat, within a specified amount of time
after mixing is complete.
The second penetration, which is also called the final penetration, is measured in a specified
amount of time later.
The comparison between final penetration and initial penetration is calculated in the presentation.
a) This test method is used to determine the degree of quick stiffening of the smeen paste or
to determine whether the cement meets the specification limits for quick stiffening or
not.
b) When used to ensure cement meets specified specification limits, the required specification
is usually stated in the minimum permissible final penetration price, in percent, calculated
in accordance with 7.2.7.8.
When used to estimate the relatively quick tendency to stiffen cement, additional information can be obtained if
the re-mixing procedure described in 7.2.7.7 is carried out.
In some conditions, to distinguish the less persistent and less pronounced tendency
towards rapid setting with the cement which has a more consistent and more obvious
appearance by comparing the properties of the mixing conditions of the two cements.
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c) Very fast apparent fixation of cement can cause difficulties in handling and placing, but this will not happen if the
concrete is mixed longer than usual, this is usually done during transporting the mixed concrete or if it is
mixed before placing it, as usually done in foundries.
The stiffness of the cement due to its rapid apparent setting is immediately apparent when the concrete is
stirred for a short time in a stationary mixer and brought to the place of placing without any means to
provide mixing, as in road pavement works.
d) Cements with very fast apparent setting usually require slightly more water to produce the same consistency,
which can result in slightly lower compressive strength and increased shrinkage.
e) Fast setting will cause difficulties in handling and casting
concrete which would normally cause the cement to fail to meet setting time requirements.
7.2.7.4 Equipment
a) Vicat tool, in accordance with 7.2.3.2 point c).
b) Knife, triangular blade with straight edge measuring (100-150) mm.
c) Mixing machines, bowls, mixers, rakes. d) Measuring cup,
according to specifications.
7.2.7.5 Reagents
Mixing water, distilled water
a) Room temperature, dry ingredients, stirrer, bowl, ebonite ring and base plate is 23.0 ± 3 oC. Mixed
water temperature is conditioned at 23.0 ± 2.0 oC.
b) Humidity of the damp room must comply with 7.2.1.1 point b).
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7.2.7.7 Procedure
7.2.7.7.1 Preparation of cement paste
Cement paste mix Mix 500

grams of cement with enough water to produce a paste with initial penetration (32 ± 4) mm using the
following procedure: a) Install the stirrer and dry bowl in the mixing machine. b) Put all the mixing
water
in a bowl. c) Add cement and leave for 30 seconds so the water is absorbed. d) Run the mixer and
stir at low speed (140 ± 5) rpm for 30
second.
e) Stop mixing for 15 seconds and during this time remove any mixture that may stick to the walls of
the bowl.
f) Run the mixer at medium speed (285 ± 10) rpm and stir for 2.5 minutes.
Immediately form the cement paste into balls with gloved hands. Press the ball that is in the palm of
one hand, insert it into the larger end of the G ebonite ring, which is held in the other hand, continue to
fill the paste into the ring.
Remove excess paste on the larger end of the ring with a single palm motion. Place the larger end
of the ring on the glass plate, H, and slice off the excess paste on the smaller end on the top of the
ring with a single motion of a sharp triangular knife held at a slight angle to the top surface.
ebonite ring.
If necessary, smooth the top of the specimen, with one or two touches with the tip of the mixing
knife. During cutting and smoothing do not press the paste.
7.2.7.7.3 Determination of initial penetration
Place the paste in the ebonite ring on the glass plate H, under the rod B (Fig. 8), approximately 1/3
the diameter from the edge of the tip of the slide, C, should it contact the paste chamber and tighten
screw E.
Then set the F indicator to the zero mark at the top of the scale, and launch the rod exactly 20
seconds after the end of stirring.
The tool shall be free from vibration during the test. If the rod has slid (32 ± 4) mm below the surface
of the paste within 30 seconds of sliding, the paste has reached the proper consistency. Experiment
with varying the percentage of water in the paste until you get the right consistency.
This consistency is initial penetration. During the 30 second interval for the initial
penetration determination return the excess paste to the bowl and then cover the bowl and
stirrer.
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7.2.7.7.4 Final penetration determination
Upon completion of the initial reading, remove the launcher from the paste, clean it and
then adjust the ring and plate back to their new position.
This operation shall be carried out with as little disturbance as possible to the paste in the vicat
ring. Then touch the slide to the surface of the paste, tighten the screw and set the F indicator
to
the right on the top of the scale.
Release the launcher a second time 5 minutes ± 10 seconds after completion of mixing
and record the final penetration 30 seconds after the rod is launched.
7.2.7.7.5 Determination of re-mixing penetration
If the penetration has been determined by the procedure above it turns out that the cement
becomes stiff immediately, information about the quick setting properties can be obtained by
the following tests:
a) After completing the 5 minute penetration measurement, immediately return the paste
inside bowl.
b) Start the mixer, raise the bowl to the stirring position and
stir refill bowl at medium speed, (285 ± 10) rpm for 1
minute.
c) Fill the ring and record the penetration following the procedure specified in items
Imprinting the test piece and determining initial penetration 7.2.7.7.2 and 7.2.7.7.3.
7.2.7.8 Calculation
Calculate the final penetration percent, based on the ratio of the final penetration to the
initial penetration, as follows:
B
%P = x100
A
Note: P
is
the final penetration percent; A
is initial penetration, mm; B is the
final penetration, mm.
7.2.7.9 Reports
Report the test results as follows:

Initial penetration…...........................mm.
Final penetration…..........................mm.
Percent of final penetration…..................%.

Re-mixing penetration…......mm.
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7.2.8 Determination of the heat of hydration
This test method covers the determination of the hydration heat of hydraulic cement by measuring the heat of
dissolution of dry cement and the heat of dissolution of cement which has been hydrated for 7 days and 28 days,
the difference between these values is the heat of hydration during the respective hydration time.
7.2.8.1 Equipment
(1) The calorimeter (see Figure 18) consists of
a) Calorimeter, consisting of a wide-mouth flask, with a cork lid, the inner wall of which is coated with a
hydrofluoric acid resistant material. The temperature of the contents of the flask should not
change more than 0.001 oC/minute for each degree of difference in room temperature if it is filled
with 425 grams of acid as specified in 7.2.8.3 point (2), closed and left without stirring for 30
minutes.
The temperature at the check must be close to the initial temperature at the determination. b)
The insulation box contains an insulating layer of cotton or similar material, which must be at least 25
mm thick and enclose the walls and bottom of the flask, but permit easy removal of the flask.
c) Differential thermometer and comparator adjustable differential thermometer of the Beckmann type,
with a scale division of 0.01 oC and having a range of 6 oC .
The thermometer must be adjusted so that the limit of the scale is close to room temperature.
The part of the thermometer that will enter the calorimeter must be protected with a coating
resistant to hydrofluoric acid.
The thermometer is equipped with a special reading lens.

The Beckmann thermometer at zero can be determined by immersing it in a liquid and comparing
it with a reference thermometer.
An accurate reference thermometer with a range of 0.1 °C is placed near the calorimeter and is
used to read the temperature and to set the zero point of the Beckmann thermometer.
d) Funnel
The funnel used to enter the sample into the calorimeter is made of glass or plastic and has a rod
with a length of ± 76 mm with an inner diameter of not less than 6 mm.
e) Stirrer
The stirrer consists of a three-bladed vane made of polyethylene having the dimensions shown in
Figure 19 and shall enter the calorimeter as close as possible to the bottom of the calorimeter.
The motor must have a constant speed of at least 1/20 hp (37 W) and must be equipped with a
speed- reducing gear so that it can set a constant speed between (350 – 700) rev/min.
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Fig
r 18 – calorimeter er
Ala
Image 1 9 – Calorie ether

mixer
NOTES a
Figucroem1mTehreciballpamodleayetaetshriyasllhesoncwedoinnabsmlianisdeptetienasrg.
w9oofitfish43mpmramodp,eedlflireaormmeter of ether shaft having 6 mm, tank length 455 mm.
The function of the stirrer is to maintain the temperature of all
uniform liquiidssimanpdorptaronvt
ifndoaertumsruaefifnoictfiaetihniisnmgstixtirhirneingsgtpogeemendaeiornafttatehinse
htaheceaidts.umsipxetunrdee. dcosnoslitdasntinstihrreinmg ixbteucraeu, swehitchhe
(2) Pe gaduk machine
Mixing machine that has a have a moderate speed, can be used for
stirrer
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and cement
and water k forms an all-purpose paste.
for
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(3) Mortar, ± 200 mm in diameter, and pounder to grind partially hydrated samples.
(4) Plastic bottles, ± (80 x 25) mm in size, with covers.

(5) Drying oven, which can maintain a temperature of (100 – 110) oC.
(6) Weighing bottle, ± 40 mm high and ± 25 mm wide, with lid.
(7) Timer device.
(8) Sieve No. 100 ( 150 µm) and No. 20 ( 850 µm).
(9) Crucible, 30 mL capacity, with lid for determining flash loss.
(10) Furnace that is suitable and capable of maintaining a temperature of (900 – 950) oC.
(11) Scales and weights according to specifications.
7.2.8.2 Reagents and materials
a) Hydrofluoric acid (bj 1,15)

b) Nitric acid (2.00 N) c)
Nitric acid ( 2.00 N HNO3) is used for the calorimeter, must be prepared and standardized in
large quantities, alternatively dilute HNO3 can be prepared by dissolving 127 mL of
concentrated nitric acid per liter of solution, provided that any determination of the heat
capacity is carried out with the prepared HNO3.
d) Candle
Paraffin wax or other suitable wax, for sealing bottle caps. e) Zinc oxide
(ZnO) must be heated at (900-950) oC for 1 hour then cooled in a desiccator, puree until it passes
through sieve No. 100 (150 µm) and stored before determining the heat capacity,
immediately heat 7 grams of ZnO at (900-950) oC for no more than 5 minutes, cool to room
temperature
in a desiccator, and weigh carefully to put into the calorimeter.
7.2.8.3 Procedure for determining the heat capacity of the device
(1) To determine the heat capacity of the system (ie the number of calories I or Joules required to
raise the temperature of the calorimeter and its contents by 1 oC), measure the corrected
temperature rise obtained by dissolving 7 grams of ignitable ZnO in the acid mixture
specified in 7.2. 8.3 point (2) to 7.2.8.3 point (5).
(2) Transfer into a vacuum bottle ± 400 grams of HNO3 2 N, which has been cooled to the lower
temperature indicated on the Beckmann thermometer (usually around (4 – 5) oC below
room temperature), add 8 mL of HF (bj 1.15 ), weigh and add enough HNO3 2 N to make
the total weight of the solution 425 grams.
Then install the calorimeter and run the stirrer motor. Take care that the impeller or the
wall does not touch the thermometer.
The bottom funnel shall be ± 6 mm below the bottom surface of the enclosure and at
least 12 mm above the liquid level.
The top end of the ball of the Beckman thermometer must be at least 38 mm
below liquid surface.
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This condition must be the same in all determinations. After an initial stirring period of at least 20
minutes to bring the temperature of the system to the same, record the room temperature to the
nearest 0.1 oC, the acid temperature to the nearest 0.001 oC record the time and then enter the
ZnO through the funnel at the same speed (NOTE 1).
In no less than one minute and not more than two minutes enter ZnO. Brush with a brush any ZnO
attached to the funnel rod into the acid mixture.
NOTE 1 The temperature of the sample must correspond to the room temperature when the sample is placed in the
calorimeter.
(3) After the sample is added, the temperature is taken to the nearest 0.001 °C at 20 minutes and then at
40 minutes. The first 20 minute period includes a dissolution period which is a temperature rise
without correction, while the second 20 minute period is a continuation period. The temperature
difference between 20 minutes and 40 minutes is a necessary correction
is added or subtracted from the temperature rise, according to whether the calorimeter temperature rises or falls during the continuation period.
a) Calculate the corrected temperature rise as follows:
R0 = Q 20 – Q 0
R = R0 – ( Q40 – Q20)
Description: is
the tempertahteuroebsoef rtvhe ctaelomrpimeerateturraet rtihse,eonCd; oRf
0thQe20 is dissolutionwpheerniodth;eQs0aims pthlee
itseamdpdeerda;tuisrethoef tchoerrceacltoerdimteemtepr erature rise, oC; R
Q40 is thpeertieomd.perature of the calorimeter at the end of the
continuation
b) Calculate the heat capacity of the calorimeter and its contents as follows (NOTE
2):
W [ 1072 + 0.4 (30 – t ) + [ 0.5( T – t ) ]

C=
R
Note: is the
weight of ZhneOa,t gcarapmacsi;tyT,
iksJt/hoeC;finCaWl teismthperature of the final
calorimeter, (Q zero Beckmann + temperature at the time of reading
thermomet(eror)o, moCte; mis
ptheeratteumrep),ewrahtuerneitoifsZinserted into the
20
calorimeter, oC; is the corrected temperature rise,
Q oC.
R
NOTE 2 The heat of ZnO solution is 256.1 cal/g at 30 oC. This value increases by 0.1 cal/g for each degree of
decrease in temperature below 30 oC. The heat capacity of ZnO 0.12 cal/g oC the heat required to bring ZnO to the
final temperature of the calorimeter must be included in the effective heat of solution.
(4) If enough ZnO is found attached to the funnel or lid when the calorimeter is opened, the test is cancelled.
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(5) Re-determine the heat capacity of the calorimeter at the following times:
a) When the Beckmann thermometer is reset.
b) When a fresh coating is applied to a thermometer, stirrer or flask.
c) If a new thermometer, new flask and or new stirrer is used. d) When a new
acid solution (HNO3) is used. e) If deemed necessary by the operator.
7.2.8.4 Procedure for determining the heat of hydration
a) Preparation of cement paste

Before preparing the paste, place the cement and water mixing at room temperature at constant
temperature, at (23 ± 2) oC, until the cement and water are at room temperature.
Mix 150 grams of cement and 60 mL of distilled water with a spatula, and stir the mixture
vigorously with a mechanical stirrer for 5 minutes.
Put the same amount of paste into four or more plastic bottles evenly until it reaches approximately
13 mm from the top and immediately close tightly (preferably the closed bottle is sealed with
melted wax).
The bottles were stored in an upright position in a water bath at room temperature (23 ± 2) oC
until the test was carried out.
b) Preparation of partially hydrated sample material for testing the heat of solution. At the specified
age of the test, remove from the reservoir a vial containing the partially hydrated sample. For 20
minutes the initial stirring of the calorimeter, plastic bottle
solved
passedand
the the
850sample
micron was
sieveimmediately crushed in put
(No. 20), immediately a mortar
it in awith a pounder
closed until
weighing the sample
bottle.
c) Be careful, especially for partially hydrated sample material for 7 days, so that the influence of air
is as small as possible, so that the influence of CO2 or loss of moisture from the sample is as
small as possible.
7.2.8.5 Determination of the hydration heat of dry cement by calorimetry
Determine the hydration heat of the dry cement sample as done in 7.2.8.3 item (1) but use 3 grams
of sample (weigh to the nearest 0.001 gram) of dry cement as
replacement for ZnO.

Calculations and results reports are stated based on samples that have been determined by the loss
of glow. Perform a 7-day partially hydrated sample test.
NOTE The heat of ZnO solution is 256.1 cal/g at 30 oC. This value increases by 0.1 cal/g for each
degree of decrease in temperature below 30 oC. The heat capacity of ZnO 0.12 cal/g oC the heat
required to bring ZnO to the final temperature of the calorimeter must be included in the effective
heat of solution.
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7.2.8.6 Determination of the heat of hydration for partially hydrated samples
For the determination of the heat of partially hydrated sample solution follow the dry cement procedure as
in 7.2.8.5 but use (4.18 ± 0.05) grams of partially hydrated cement sample.
Weigh to the nearest 0.001 gram. Calculations stated are based on a predetermined sample of the loss of
glow.
7.2.8.7 Loss of glow
Immediately before and after the sample for the determination of the hydration heat by calorimeter is
weighed, weigh the same number of samples in the crucible for the determination of the loss of glow.
The value of the loss of glow used is the average of the two determinations.
For the determination of the flash loss of dry cement, heat a sample of the dry cement at room temperature
o
(950 ± 50) k
desiccator, in Camsek ka un rah nin gg -g kua rsau nh gu ny raua 1n ,5g, jadmsaene,ms urda iatinmsb ea tn eg.h immediately move it inside
When determining the glow loss of hydrated cement, first dry the weighed sample in the oven at (100-110)
oC for 1 hour, transfer it to the furnace at (950 ± 50) oC for 1 night, or above suitable heating for not less
than 5 hours, cool in a desiccator until room temperature then weigh.
Calculate the weight of the incandescent base sample included in the calorimeter as follows:
AxW
Wi = B
Note: Wi is
the of the sample calculated on the basis of the glow entered in the calorimeter, grams; A is
the sample weight after ignition, grams; B is the weight of the sample before ignition, grams;
W is the sample weight included in the calorimeter, grams.
In addition to the glow loss procedure for portland cement, the determination of glow loss can be determined
using the referee's method as given in the test method in 7.1.3.12 for portland slag cement and cement
slag.
a) Determine the SO3 content using the referee method according to the test method in 7.1.3.11.1. Also
determine the SO3 content of the unsanded cement using the same method.
b) Calculate the percentage by weight of the sulfur sulfide as follows:
G = 0.8 (S1 – S2)
Note: G is
the weight percent obtained in the sample that was ignited; S1 is SO3 in
the ignited sample; S2 is SO3 in the unfired example; 0.8 is the
molecular weight ratio of 4(O)/ SO3.
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c) Calculate the weight of the dry calorimetry sample on the basis of annealing as follows:
(A-BG/100) W
Wi =
B
Note: Wi is
the weight of the dry sample, on an incandescent basis,
grams; A is the weight of the burnt dry sample, grams; B
is
the weight of the dry sample before annealing, grams; G is the
percentage by weight of the sulfur sulfide recovered, and; W is the
weight of the dry calorimetric sample, grams.
d) Calculate the weight of the partially hydrated calorimetry sample on a glow basis as in
below:
AW (1-G/100)
Wi =
B
Note: Wi is
the weight of the dry calorimetric sample, on an incandescent basis,
grams; A is the weight of the partially hydrated sample after agitation, grams;
B is the weight of the partially hydrated sample before annealing, grams; G is
the percentage by weight of the sulfur sulfide recovered; W is the weight of the
dry calorimetric sample, grams.
NOTE An assumption is made in the calculations that the percent sulfide is the same as
before annealing for the partially hydrated sample as determined in the cement.
7.2.8.8 Calculation
7.2.8.8.1 Heat of dissolution of dry cement
Calculate the corrected temperature rise as in 7.2.8.3 point (3)a) and 7.2.8.3 point (3)b). Also correct
the calorific value of dissolution if the temperature is different from the calorimeter temperature when
the sample is added. So, for dry cement which has a specific heat of about 0.8 kJ/kg.K, if the final
temperature of the calorimeter exceeds the temperature of the cement sample after it has been
introduced, add a correction of 0.8 kJ/kg.K, to that temperature when calculating the heat of
dissolution . Calculate the heat of dissolution of dry cement as follows:
H1 = (RC/Wi) – 0.8 (T – td)
Note: H1 is
the heat of dissolution of dry cement, kJ/kg; R is
the corrected temperature rise, oC; C is the heat
capacity, kJ/°C; Wi is the sample weight
calculated
on the basis of glow, grams; T is the room temperature at the
time the sample was added, oC; is the final temperature of
the
calorimeter at the end of the dry cement measurement, oC. td
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7.2.8.8.2 Heats of dissolution of partially hydrated materials
Calculating the heat of dissolution of the partially hydrated sample is the same as for dry cement, except that
corrections are made as follows: For every 1 °C increase in temperature during the heat of dissolution test,
the
heat of solution decreases by approximately 1.3 kJ/kg. Thus if the temperature of the partially hydrated heat
dissolution test exceeds the determination temperature for dry cement, add a correction of 1.3 kJ/kg to the calorific
value of dissolution obtained for the partially hydrated sample.
Also, correct the calorific value of the solution if the final calorimeter temperature is different from the
calorimeter temperature at the time of the test.
For the partially hydrated cement example, luminous cement has a specific heat of about 1.7 kJ/kg. If the final
calorimeter temperature exceeds the sample temperature at the time of insertion, add a correction of 1.7 kJ/kg
oC when calculating the heat of dissolution.
H2 = (RC/Wi) – 1.7 (T-yr) – 1.3 (td – yr)
Information :
H2
is the heat of dissolution of the partially hydrated sample,
R,C,Wi,T and
kJ/kg; is as in 7.2.8.8.1; is the temperature of the calorimeter at
td th
the end of the measurement of the partially hydrated sample,
oC.
7.2.8.8.3 Heat of hydration
The final calorimeter temperature of 25 oC shall be considered as the basic reference heat of hydration, and it
is important to bear in mind the influence of variations in this temperature in considering the test results.
The final increase in temperature increases the heat of hydration by approximately 0.4 kJ/kg.K, of the hot cement.
For example, if the final temperature is 27 oC, 0.8 kJ/kg must be subtracted from the heat of hydration in order
to refer to the 25 oC result.
Observation for the final calorimeter temperature is around 25 oC, be careful in observing the final
temperature. Accurately calculate the hydration heat of cement as follows:
H = H1 – H2 – 0.4 (years – 25.0)
Note: H is the
hydrationohfehaott cement, kJ/kg; H1 is the heat of dry
cement sohlyudtiroante, d7.c2e.8m.8e.n1t;
sHo2luitsiotnhe7.h2e.8a.t8o.2f ;ptahrtiisaltlhye same value as
in 7.2.8.8.2.
7.2.8.9 Retest
In case of failing to meet the 28-day hydration caloric requirement, the reserve paste sample can be tested at a
later age and corrected by 2.1 kJ/kg per day for each additional age. To bring the results of the calculation of
the heat of solution at 28 days.
The excess period in which this correction is made should be limited to 4 days. In case of failure to comply
with the 7 day requirement, retest entirely including the manufacture of the paste mix.
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7.2.8.10 Accuracy and bias
7.2.8.10.1 Accuracy
7.2.8.10.1.1 Single operator precision
The standard deviations of the single operator are 12.2 kJ/kg (1 second) and 14.8 kJ/kg (1
second) for the heat of dissolution and heat of hydration respectively. Accordingly, the
results of two tests performed by the same operator for samples of the same cement shall
not differ
by more than 34 kJ/kg in determining the heat of dissolution or 42 kJ/kg in determining
the heat of hydration.
7.2.8.10.1.2 Accuracy of multiple laboratories
The standard deviation of the multi-laboratory is 18.5 kJ/kg for the heat of dissolution and 16.9 kJ/kg for the heat of
hydration. Therefore, for two tests performed for two
Different
heat laboratoryorsamples
of dissolution 48 kJ/kgoffor
thethe
same cement shall
determination notheat
of the differofby more than 52 kJ/kg for the determination of the
hydration.
7.2.8.10.2 Bias
No statement of bias is made as there is no acceptable reference material.
7.2.9 Sulfate expansion test
This test method is only used for Portland cement, including determining the expansion of mortar made from a mixture
of Portland cement and gypsum in certain proportions so that the sulfur trioxide (SO3) content in the mixture is 7.0%
by weight. Values are specified in mm per gram and are expressed as standards.
This test method is intended primarily for use by those interested in research on methods for determining the sulfate
resistance potential of portland cement. This method is also used to ensure that the sulfate resistance of portland
cement meets the requirements in Table 4.
7.2.9.2 Equipment
a) Scales and weights must be according to specifications.

b) Flow table, must meet the specification requirements (See Figure 16).
c) Mixing machines, bowls and stirrers must comply with the specifications in the Appendix
C.
d) Knives stirring, triangular knife, pounder must meet specifications. e)
Measuring cups, molds and length comparisons must comply with
specifications.
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a) The temperature of the molding chamber, dry ingredients and mixing water shall be maintained at 23.0
± 4 °C.
b) The humidity of the printing room shall not be less than 50%.
7.2.9.4 Ingredients
a) The sand used to make the test mortar must meet the quality requirements
sand according to 7.2.6.4.
b) Gypsum used for addition to portland cement must be high quality natural gypsum with 100% passing 150 µm (no.
100) sieve, at least 94% passing 75 µm sieve (no. 200) and at least 90% passing 45 µm sieve (no. 325).
Calculate the required percentage of cement and gypsum so that the mixture is
contains 7.0% by weight SO3 as follows: % cement = [ ( g

– 7.0 ) / ( g – c ) ] x 1x0010%0 gypsum = [ (7.0 – c ) / ( g – c ) ]
Note: is the
c SO3 content in portland cement, %; is the
SO3 content in gypsum, %; is the SO3
g 7.0 content of the cement-gypsum mixture,
%.
7.2.9.5 If the SO3 content of gypsum is not known, the gypsum shall be analyzed for SO3 content using the
SO3 chemical analysis method of cement. The SO3 level must be determined
with an accuracy of 0.1%.

7.2.9.6 Number and size of test objects
a) For each cement sample, two mortars are made, each of which is mixed for 3 test objects. The size of each
specimen is (25 x 25 x 285) mm. b) In routine testing, specimens with a size of (25 x 25 x 160) mm can
be
used, but in the case of disputes, the results obtained must be based on the size of the specimens (25 x 25 x
285) mm.
7.2.9.7 Procedure
7.2.9.7.1 Preparation of test object molds
a) The mold must be prepared according to Figure 11.
b) The amount of dry ingredients needed for each mortar should be 400 grams (cement plus gypsum) and 1
100 grams of sand. The amount of mixing water must be 194 mL for all types of portland cement.
c) Mix the mortar according to the mortar mixing procedure of Appendix C, except after placing the mixing water in
the bowl, add the gypsum and mix at low speed for 15 seconds, then stop mixing, add the cement, and
proceed as described in Appendix C.
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As soon as the flow test is complete, transfer the mix back to the bowl, lower the mix against
the bowl wall, and mix again at medium speed (285 ± 10) rpm for 15 seconds. Remove the
mixer and bowl from the mixer and pour excess mortar from the mixer into the bowl. Fill the
mold in two layers, each layer compacted with the pounder.
Push the mortar into the corners, around the bolts, and along the surface of the mold by
pounding until a homogeneous specimen is obtained.
After the top layer is compacted, cut off the excess mortar until it is flush with the top surface of
the mold and smooth the surface of the mold several times with a triangular stir knife.
7.2.9.7.3 Place of storage of test objects
7.2.9.7.3.1 Initial storage
Moisten the specimen in the mold in a damp cupboard at (23 ± 2) oC for (22-23) hours, then
remove the specimen from the mould, mark accordingly and place it in water at (23 ± 2) oC for
at least at least 30 minutes before the initial measurement.
7.2.9.7.3.2 Advanced storage
After the rod has been removed from the mold and has been measured, place the specimen
horizontally in water at a temperature of (23 ± 2) oC. The placement of each specimen shall be
at least 6 mm on the sides except for supports where necessary.
All specimens shall be submerged in water to a depth of at least 13 mm. The ratio of the volume
of water to the volume of the specimen should not be more than 5 : 1 to prevent excessive lime
dissolution.
Replace the soaking water with fresh water every 7 days for the first 28 days and every 28 days
thereafter.
7.2.9.7.4 Length gauge
Measure the length of the specimen using a length comparator. Remove the specimens from
the water bath one at a time, and wipe with a damp cloth before measuring.
Take the first measurement at 24 hours ± 15 minutes from the time the cement and water were
mixed. Re-measure the specimen at the age of 14 days.
NOTE Add data from the price of the measurement results can be obtained by re-soaking the
test object after the 14-day age test and taking additional measurements at a later age.
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7.2.9.8 Calculation
Calculate the difference in the length of the specimen at 24 hours and 14 days with an accuracy of 0.001% of
the effective length and report it as the expansion of the specimen in that period.
All specimens remaining for 14 days of age must consist of 1 set of at least three specimens with the
permissible stretch depending on the number of specimens remaining, as follows:
Table 21 ÿ Deviation
Maximum allowable length deviation

Number of test
objects (%) 0.010 0.011 0.012 0.012
3
4
5
6
7.2.9.9 Reports
Report the average length of a set of specimens meeting the above conditions with an accuracy of 0.001%.
7.2.10 Testing the air content of mortar
The purpose of testing with this method is to determine the air content in the mortar.
7.2.10.1 Equipment and materials
a) Flow tables, dies and calipers, according to 7.2.6.3. b) The measuring

instrument is a cylinder with an inner diameter of (76 ± 2) mm and a depth of 88 mm which is standardized
with water (400 ± 1) mL at a temperature of (23 ± 2) oC .
c) For the purpose of this test the capacity of the measuring instrument is stated in mL which is the weight of water
divided by 0.997 6. There is no correction for weight due to foam occurring. The gauge must have an even
wall thickness, wall and base thickness of not less than 2.9 mm and a total empty weight of not more than
900 grams. Measuring tools must be made of metal that is not damaged by the cement.
d) Mixing machine, mixing bowl. e) Slicing
and leveling knife.
Slicing and leveling blades are made of steel with a length of not less than 200 mm with a thickness of 1.5
mm to 3.5 mm with a straight edge.
f) Scales that have a capacity of 2 kg with an accuracy of 1 gram. g) 250 mL measuring
cup with a measurement accuracy of 2 mL.
h) Collider. i) A
metal spoon has a length of 230 mm and a bend length of 100 mm.
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The room and dry materials are maintained at a temperature of (23 ± 4) oC with a humidity
of not less than 50%. Stirring water conditions and measurements at (23 ± 2) °C.
7.2.10.3 Standard sand
The standard sand used is Ottawa sand (standard sand 20-30) with the following
grain gradations:
Table 22 ÿ Ottawa sand grain gradations

Sieve hole diameter 1.18
mm 850 micron Pass the sieve, (%)
100 (85 –
600 micron
100) (0 – 5)
7.2.10.4 Procedure
7.2.10.4.1 Arrangement of mixed mortar
Portland cement : 350

Standard sand gradation 20-30 grams : 1 400 grams
Enough water to provide a spread of the mix (87.5 ± 7.5) %
7.2.10.4.2 Mixing mortar
iPT(n1hlta4oe0cnteh±pethu5bet)
otrdhpwremyl.isnbfotg)irrrAre3edd0rdieascneedcsmomfneoidnrxstion.tnogetbhtoiemwwel
oamnteixtrh,inetghmei nixoreurtnhinethtbehoemwsilxtiaerrsrinfaognlldpoowwsshit:ioaen) s.Ptiurrtinthgeamt
lioxwingspweaetder
c) Add all the sand slowly in 30 second intervals, while stirring

at low speed (140 ± 5) rpm.
d) Stop the mixer, change to medium speed (285 ± 10) rpm, and stir for 30 seconds. Stop
the mixer and let the mortar sit for 1.5 minutes.
During the first 15 seconds of this time interval, immediately clean the mortar attached
to the inside wall of the bowl, then cover the bowl.
e) Continue the final stirring for 1 minute at medium speed (285 ± 10) rpm. f) If necessary,
at any intervals it is necessary to re-mix, any mortar attached to the inner wall of the bowl
must be cleaned immediately with a rake before re-mixing is carried out.
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7.2.10.4.3 Determination of mortar mix distribution
Place the mold in the middle of the flow table which is wiped dry beforehand. Fill the mold with
a height of 25 mm. Compact the mixture with the pounder 20 times. The impact pressure must
be sufficient so that the filling is completely level.
The mold is filled again to the brim and compacted like the first layer. Then level the top of the
mortar with a leveling knife in 2 mutually perpendicular directions.
Clean and dry the surface of the flow table on the outside of the mould. Remove the mold from
the mortar 1 minute after finishing work, tap the flow table from a height of 12.7 mm 10 times in
6 seconds. The average dispersion that occurs is measured with calipers from 4 measurements
at different angles.
The measurement results are expressed in percent of the initial diameter. Repeat the work as
above with different amounts of water, until the desired distribution is achieved. Each repetition
uses a new mix.
7.2.10.4.4 Determination of air content
If the intended distribution has been obtained, weigh the remaining 400 mL of the mixture. Enter
the mixture with a spoon into the measuring tool in 3 layers. Each layer is compacted by pricking
it with a leveling knife 20 times along the inner side of the mould. In stabbing the first layer,
don't puncture the bottom of the mold. In the second and last stabbing, it is enough to penetrate
the layers of each mixture. To remove air trapped in the mix, gently tap the side of the gauge
with the pounder at 5 different points around the gauge, each batch. To remove air trapped in
the mix, gently tap the side of the measuring tool with a pounder at 5 different points around the
measuring tool, 1 time each tap.
Level the surface of the mortar in the measuring tool with a leveling knife in 2 perpendicular
directions. If during leveling there are grains of sand that come out of the mortar and cause
scratches, the equipment must be repeated. This whole job should be completed within 1.5
minutes. Clean the mixture and water that comes out of the measuring tool.
Weigh the measuring instrument and its contents then calculate the weight of the mixture in grams.
7.2.10.5 Calculation of air content
Calculate the air content of the mortar with the formula below:
Air content = 100 – W [(182.7 + P)/(2 000 + 4 P)]
Note: W is
the weight of 400 mL of mortar, grams; P
is the ptoertche wtaegigehot fowf atht e
cferommentht eusmeidx.
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8 Requirements to pass the test
Portland cement being tested is declared ineligible if: a) Cement fails

to meet one of the quality requirements as stated in Article 5. b) Retests can be carried out
on cement stored in silos that will be shipped for a period of more than 6 months. If the
results of the retest fail to meet one of the quality requirements as stated in Article 5, the
cement is declared to have failed the test.
c) Portland cement test results certifying that it fulfills the requirements only applies to
the sample group.
9 Packaging
9.1 Portland cement can be traded in packaged and bulk forms. If there are no other provisions,
packaged portland cement must be packaged in bags with a net weight of 25 kg and/or 40
kg and/or 50 kg for each bag.
9.2 Underweight should not be more than 2% of the weight stated on each package.
10 Terms of marking
The packaging must include the code, brand/trademark, type, company name and net
weight. For bulk portland cement, the marking shall be stated on the shipping document.
11 Storage and transportation
a) Cement when stored or transported must be maintained in such a

way for easy inspection and identification.
b) Bulk cement is stored in a building/storage that is weather-tight, so it will protect

cement from moisture and prevent cement from clumping during storage and
transportation.
c) Storage and transportation of cement in bags is carried out in such a way as to avoid the effects of weather.
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Appendix A
(informative)
Example of chloride determination record form
Table A.1 - An example of an equivalence point determination form for chloride determination
Column 1 Column 2 Column 3 Column 4

AgNO3, mL Potential, mV mV A 2mV B
1.60 125.3
5,8
1.80 119.5 1,4
7,2
2.00 112.3 1,3
8,5
2,20 103.8 1,3
2.40 94.0 9,8 0.6
9,2
2.60 84.8 2,3
6,9
2.80 77.9 0.8
6,1
3.00 71.8 1,3
4,8
3,20 67.0
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Appendix B
(informative)
Example of qualifying results
Table B.1 - Initial setting

time units in minutes
Initial binding Average

Cement Suite method B difference
Initial binding
method A (max. spec. 45)
A 1 95 105 …
A 2 90 105 …
A 3 95 90 …
range
5 15 …
(spect. 30 Max)
Average 93,3 100.0 6,7
B 1 100 120 …
B 2 105 95 …
B 3 85 95 …
range
20 25 …
(Spec. 30 Max)
Average 96.7 103,3 6,7
C 1 155 170 …
C 2 155 160 …
C 3 145 155 …
range
10 15 …
(spect. 30 Max)
Average 151.7 161.7 10.0
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Table B.2 - Time of final setting
units in minutes
Final binding Difference

Cement The final binding series of method method B average
A (max spec. 45)
A 1 150 150 …
A 2 145 150 …
A 3 170 125 …
range
25 25 …
(spect. 30 max)
Average 155.0 141.7 13,3
B 1 185 180 …
B 2 200 180 …
B 3 185 155 …
range
15 25 …
(spect. 30 max)
Average 190.0 171.7 18,3
C 1 235 225 …
C 2 240 220 …
C 3 240 215 …
range
5 10 …
(spect. 30 max)
Average 238.3 220.0 18,3
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Appendix C
(informative)
Mechanical mixing of hydraulic cement paste and
plastic consistency of mortar
C.1 Scope
This practical method includes mechanical mixing of the cement paste, hydraulic and
plastic consistency of the mortar.
C.2 Purpose and use
This method is intended for use in mechanical mixing of pastes and mortars for
hydraulic cement testing.
C.3 Equipment
C.3.1 Mixing machine
The mixer shall be a mechanical mixer of the epicyclic type, having an electrically
actuated drive capable of moving the mixer horizontally and rotating.
The mixer shall have two mechanically adjustable speeds.

T h e f i rs t s p e e d, l o w sp e e d w h ic h c a n m o v th e s
c i rc u l a r m o t io n o f t he s tir r er b la d e s a t a sp ee d o f
t i rr e r a t a s p e ed o f (1 40 ± 5 ) m w it h a
( 2 8 5 ± 1 0 ) rp m w i th a cir cu l ar m o tio n o f the stirrer rod of
approximately 125 rpm. Electric motor power must be at least 124 watts (1/6 hp).
The mixing machine shall be provided with a spacer retaining device as shown in figure
12 which shall be used to maintain that the distance between the bottom of the mixer and
the bottom of the bowl is not greater than 2.5 mm, but not less than 0.8 mm (approx. with
a diameter of Ottawa sand (20 – 30) when the bowl is in the stirring position.
C.3.2 Mixer
The stirrer must be easy to assemble and disassemble, made of stainless steel, and have
a basic design as described in Figure 13. If the stirring position follows the shape of the
bowl used, the shortest distance between the tip of the stirrer and the inner wall of the bowl
is ±
4.0 mm but not less from 0.8mm.
C.3.3 Mixing bowl
The removable mixing bowl shall have a nominal capacity of 4.73 L. It shall comply with the
dimensions and appearance as shown in Figure 14, and shall be made of stainless steel.
The bowl is equipped with a part that can be attached properly to the mixing equipment in a
firm position while the stirring is running.
Must be equipped with a lid made of non-absorbent material and not damaged by cement.
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C.3.4 Scraper
The scraper shall consist of a semi-rigid rubber blade fitted with a handle ± 150 mm long.
The blade is ± 75 mm long, 50 mm wide and tapers to a thin side of ± 2 mm.
C.3.5 Additional equipment
Scales, weighing stones, measuring cups and other tools used in measuring and
preparing mortar materials prior to mixing must meet the appropriate requirements.
C.4 Temperature and humidity
C.4.1 One chamber, dry ingredients, mixer and bowl shall be kept between
(20 - 27.5) oC. Mixing water temperature should be (23 ± 1.7) ÿC.
C.4.2 Laboratory humidity of at least 50%. Temperature and humidity according to 7.2.1.1.
C.5 Ingredients, proportions and consistency
C.5.1 Requirements
The ingredients, their proportions and consistencies as well as their quantities must comply with
the requirements contained in the particular method by which the paste or mortar is prepared.
C.5.2 Procedure for mixing pasta
C.5.2.1 Place the stirrer and dry bowl on the stirrer in the stirring position. Then put
the ingredients for one time stirring into the bowl as follows:
a) put all the mixing water in a bowl;

b) add cement to the water and let it sit for 30 seconds, for water absorption;
c) run the mixer at low speed 140 rpm ± 5 rpm for 30 seconds.
fCro.5m.2a.2nySstotipckthyepamsitxee.r for 15 seconds and during this time clean the inner walls of the
bowl
C.5.2.3 Run the mixer at medium speed at (285 ± 10) rpm and mix for 1 minute.
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C.5.3 Procedure for mixing mortar
C.5.3.1 Place the dry stirrer and mixing bowl on the stirrer in the stirring position. Then put
the ingredients one time stirring into the bowl as follows: a) put the mixing water in the
bowl;
b) add cement to the water, then run the mixer while stirring on
low speed 140 rpm ± 5 rpm for 30 seconds;

c) add all the sand slowly in 30 second intervals, while stirring at a low speed of 140 rpm ±
5 rpm.
C.5.3.2 Stop the mixer, switch to medium speed (285 ± 10) rpm, and stir for 30 seconds.
C.5.3.3 Stop the mixer and allow the mortar to set for 1.5 minutes. During the first 15 seconds
of this interval, quickly clean off any mortar adhering to the inside walls of the bowl,
then cover the bowl.
C.5.3.4 Continue final stirring for 1 minute at moderate speed (285 ± 10)rpm.
C.5.3.5 If necessary, at any intervals where re-mixing is required, any mortar adhering to
the inner walls of the bowl shall be removed immediately with a rake prior to re-mixing.
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Bibliography
ASTM C 150/C150M-12, Standard Specification for Portland Cement

ASTM C114-13, Standard Test Methods for Chemical Analysis of Hydraulic Cement
ASTM C109/C109M-13, Standard Test Method for Compressive Strength of Hydraulic Cement
Mortars (Using 2-in. or [50-mm] Cube Specimens)
ASTM C 151/C151M-09, Standard Test Method for Autoclave Expansion of Portland Cement.
ASTM C 186-13, Standard Test Method for Heat of Hydration of Hydraulic Cement.
ASTM C 187-11e1, Standard Test Method for Amount of Water Required for Normal Consistency
of Hydraulic Cement Paste
ASTM C 191-13, Standard Test Method for Time of Setting of Hydraulic Cement by Vicat Needle
ASTM C204-11, Standard Test Methods for Fineness of Hydraulic Cement by Air
Permeability Apparatus
ASTM C115/C115M-10e1, Standard Test Method for Fineness of Portland Cement by the
turbidimeter
ASTM C 266-13, Standard Test Method for Time of Setting of Hydraulic Cement Paste by
Gillmore Needles
ASTM C 451-13, Standard Test Method for Early Stiffening of Hydraulic Cement (Paste Method).
ASTM C185-08, Standard Test Method for Air Content of Hydraulic Cement Mortar

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Ma c h i n e T ranslated by

Indonesian National Standard

ICS 91.100.10 National Standardization Body

3 Terms and definitions............................................................................................................ 1

4 Types and uses................................................................................................................... 2

7.1 Chemical test method......................................................................................................... 10 7.1.1

7.1.3.1 Insoluble part.................................................................................................14 7.1.3.2

7.1.3.9 Calcium oxide (CaO)..........................................................................................26 7.1.3.10

7.1.3.12 Loss of glow......................................................................................................... 34

7.1.3.14 Manganese oxide................................................................................................. 39

7.1.3.16 Organic compounds that dissolve in chloroform......................................................45

7.1.4 Alternative test method (Optional)...............................................................................48

7.1.4.3 Titanium dioxide.............................................................................................. 52 7.1 .4.4

7.2 Physics test method.............................................................................................................. 64 7.2.1

7.2.9 Test for expansion due to sulfate...........................................................................126 7.2.10

8 Requirements for passing the test................................................. .................................................. ...............

10 Terms of marking.......................................................................................................................... 132

11 Storage and transportation........................................................................................................... 132

Appendix A........................................................................................................................... 133

Appendix B........................................................................................................................... 134

Appendix C............................................................................................................................. 136

Table 1 ÿ Main chemical terms..................................................................................................... 2 Table 2 ÿ

Additional chemical terms...................................................................................................... 3

Table 3 ÿ Main physics requirements..................................................................................................... 4

Table 4 ÿ Additional physics requirements................................................................................................ 4

Table 5 ÿ Test time interval after sampling...................................................6

Table 6 ÿ Permissible difference in test results.............................................................................11

Table 7 ÿ Comparison of MgO levels with the required amount of reagent................51

Table 8 ÿ Comparison of MgO levels with the amount of standard solution...............................................52

Table 10 ÿ Cement coating porosity values............................................................................73

Table 11 ÿ Airflow time range.......................................................................................... 74

Table 12 ÿ Dimensions of the turbidimeter apparatus............................................................................. 78

Table 13 ÿ h, d and h/d

Table 14 ÿ Burette dimensions......................................................................................................... 82

Table 15 ÿ Example of recording turbidimeter test data and calculations

Table 16 ÿ Allowable variation of die casting (mm).............................................104

Table 17 ÿ Standard sand requirements......................................................................................... 106

Table 18 ÿ Mortar composition.................................................................................................. 108

Table 19 ÿ Test time tolerances.......................................................................................... 110

Table 20 ÿ Accuracy........................................................................................................................ 113

Table 22 ÿ Ottawa sand grain gradations......................................................................................... 130

©BSN 2015 iii

Figure 1 ÿ Cement sampling pipe.................................................................................... 8 Figure 2 ÿ Packaged cement

Figure 3 ÿ Blaine tool................................................................................................................ 67

Figure 4a ÿ Front view of the turbidimeter with the door open..................................................75

Figure 4b ÿ Front view of the turbidimeter with the door open..................................................76

Figure 5 – Turbidimeter rear view................................................................................. 76

Figure 6 – Time burette.............................................................................................................. 77

Figure 7 – Turbidimeter electrical system.............................................................................................. 77 Figure 8 –

Figure 9 – Gilmore tool............................................................................................................... 97

Figure 10 – Cement paste slab shape............................................................................ 98

Figure 11 – Prism print..................................................................................................... 99

Figure 12 – Comparator........................................................................................................... 100

Figure 13 – Stirrer machine................................................................................................... 104

Figure 14 – Mixer............................................................................................................ 104

Figure 15 – Bowl.............................................................................................................................. 105

Figure 16 – Flow table................................................................................................................ 105

Figure 17 – The sequence of collisions................................................................................................. 110