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(Reaffirmed 2014) 

IS: 4669  -1968


(Reamrmed 20(3)
(Reaffirmed 2013) 
Indian Standard (Reaffirmed 2018)
 
METHODS OF TEST FOR
(Reaffirmed 2012) 
POLYVINYL CHLORIDE RESINS
Fourth Reprint MAY 2005  
(Incorporating Amendment No_ 1)
(Reaffirmed 2011) 
UDe 678.743.22: 543
 

(Reaffirmed 2010) 

(Reaffirmed 2009) 

(Reaffirmed 2008) 

(Reaffirmed 2007) 

(Reaffirmed 2006) 

 
© Copyright 1973
(Reaffirmed 2005) 
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN. 9 BAHADUR SHAH ZAF AR MARG
 
NEW DELHI 1lOOOl

Gr4 Alq.!u.\·, 1968


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11 . . . . ·1_

Indian Standard
METHODS OF TEST FOR
POLYVINYL CHLORIDE RESINS
Plastics Sectional Committee, CDC 17
CluJi,,,,.,, ~1iIIt
SH.. N. SIUNlVAI"N The PJuties IlIItitutc ( Indian Section), New Delhi
M""IJI"
SH.. C. I. AUlAtlLA Polychem Ltd, Bombay
Sual S. K. S""OHVI (AI,.,,,.,.)
SIUU K. J. SALAKallllNA Miniltry or Def'ence ( R It D)
SHIll K. K. GANOtlLl ( M,."..,. )
SHat G. BRAGAT or
The Metal Box Co India Ltd, Calcutta
0. S. S. MALHO'I'a" ( .A"""'" )
SHIll G. R.. BHIDJI Garware PJuties Pvt Ltd, Bombay
SHIll P. H. C"SHMAN PhiIi.,. India Ltd, Calcutta
SHaI S. S. CAaDMAI1'&R Hylam Limited, Hyderabad
SHRI S.J. HAIAN (.AI,."..,.)
SRRI K. G. CHANDRA.aKHAaAPP" Indian Telephone Induatrin Ltd, Baagalore
SNRI P. DAI Miniltry of Defence ( R It D)
DEPIlTY DrucroR STANDAJUlI Railway Board (Ministry of RailwaY' )
(CARRIAGa )
CHaM.... AI'fD METALLuaaT·2
( .AI,."..,. )
DR S. G"NOtJU I.C.I. ( India) Pvt Ltd, Calcutta
SIIRt D. K; RAiU ( .AlIn,.." )
S.... M. L. GANOtlU The Indian Cable Co Ltd, Calcutta
SlID I. P. GHOIH ( MImuII6)
Sa.. A. S. JUOHAH IDCliaD P_tics FederatioD, Calcutta
SHal V. V, KaTltAIl ( A"."",. ) .
DR S. L. KA..ua National ChemiCal Laboratory (CSlR), Pooaa
I5JW K. B. Kt/UAJUIII. Indo-Nippoa Chemic:al Co Ltd, Bombay
Sau N. I. BRuA ( .AI,.",.,.) .
SNRI S. M I T R A . CaUeo Milli ( Chemical Divwon), Bomba,
DR B. R. C. ANAlCD (M""'.") ..
SHat S. N. MuitHBIlJI Natioftal Tnt HoUie, Calcutta
. . ·SIW S. K. Boaa ( .AI""..,. ) .
SHU G. N. PARIKH . All·· India PJuties Manufacturen' A1IIoc:iadaD,
. .• Bc.nbay
s.aaIl'l'ARY ( .A"".".,. )
Saal ll. P....IICIHh' Direaoratc·· GCIler&l or. Technical DeveIopmeDt,
New Delhi
DaH. N. PATaL The Plastics It Linoleum Export Promotion CouaciI,
Bombay . .
SHal. R"IIAIC M. PAUL The Bhor IadUitrie. Ltd, Boaibay
SHill J.M. SHao,.. (
All"".,. )
Saw J. E. PalNaa National 0rpn1c Chemical Industries Ltd, Boaabay
8HRI'l'. ·G. PUNWANI Bript Brothen Pvt Ltd, Bombay
Sa.. T. W. BHOJWANI (.AI,.,...,.)
( C'MtIiItwtt .. ,.". 2 )

BUREAU OF INDIAN STANDARDS


MANAK SHAVAN, 9 SAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
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18,4669.1968

Mmtbm RlfJnsatinl
SHIll S. RAllAlWAIIY Chemical, aDd PlutiCllndia Ltd, Madru
SHIll R. KAuoAi ( AI"",.,. )
SIIRl D. A. Rua KOImek PlastiCi Manufacturing Ltd, Bombay
SHIll N. J. MllQ.UlTA (Mimi.,,)
SIIRl R. A. SHAH Union Carbide India Ltd, Calcutta
SHal I. M. MaRTA (AI""..,,)
SHU V. SUBaAMANIAN Heavy ElectricaIs ( India) Ltd, Bhopal
SHU R. C. MIIHaA ( AlImI." )
DR SAIKIOPAL, Director General, lSI (&-q/fidII Mlfflkr)
Director ( Chem )
Su"tGrWs
SHIll M. S. SAUNA
Deputy Director ( Chem ). lSI
Da G. M. SAXBNA
Deputy Director (Chem). lSI

Thermoplastics Subcommittee, CDC 17 : 3


Con_
Da S. L. KAPUIl National Chemical Laboratory (CSIa), Pooaa
M,mb",
SHaIB.A.CAJtp~a Eat Anglia Plastic. ( India) Ltd, Calcutta
Da D. CaOWOHual Un10n Carbide India Ltd, Calcutta
SHIll V. B. PATHAK (Aluf'ftIJU)
SHal C. R. DAI Shriram Vinyl lit Chemical Industrie., New Delhi
SYRI S. V. S. RATNAM ( AltmJ.u)
Da S. GANGUU 1.C.I. (India) Pvt Ltd, Calcutta
SHIll D. K. BAIU ( Allml4u )
SIUI R. A. MEHUDALE Garwarc PlastiCi Pvt Ltd, Bombay
SHIll B. M. JEOUUKAR ( Alllm.',)
SHU S. MITRA Calico MUll (Chemical Division ), Bombay
DR B. R. C. ANAND (.4111".,,11)
StuU K. K. MODY All India Pla.tia Manufacturen' Auociaticm,
Bombay
SECRETARY (AllmuJu)
DR C. K. PAUKH Tbe Hindustan Polymen Ltd, Bombay
SHIll MAHENDRA M. SHAn (AI,,,,,o")
SHRI RAMAN M. PATEL The Bhor Industries Ltrf, Bombay
SHIll K. S. DosHI (Alum.")
SHRIJ. E. PUNCE National Organic Chemical Industria Ltd, Bombay
SHU T. G. PUNWANI Bright Brothen Pvc Ltd, Bombay
S8R1 T. W. BHOJWANI (Alii,,,.,,)
SHIll D. A. Rlla KOImek Plutic. Manufacturing Ltd, Bombay
SHu N. J. MuQ,UITA (At"",.,,)
Da S. M. SHAH Polycbem Ltd, Bombay
SHaJ C. I. AuiAULA ( AltmJ.u)
SHRI P. S. SRlMIV""," Radion lit Electricall Mfg Co Ltd, Bangalore
SHRr L. R. Suo Mini,try of Defence (R lit D)
SHIll S. L. VaNKlTIIIWARAN MYlOre Acetate and Chemical Co Ltd, Bangalore
SHRI S. K. VEIUIA Caprihan. ( India) Private Ltd, Bombay
SRRr P. C. V ....A (AltmuIII)
SIIRl M. S. WOOD The Metal Box Co of India Ltd, Calcutta
SHIlr G. BHAOAT ( AI,."...)

2
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..... -1_
CONTENTS

O. FORBWOIlD ..

I. SCOPB ..

2. TBRMINOLOGY 4
S. SAMPLING... 5
4. QUALITY OF RSAGENTI 5
5. DETlUlMINATION OF Loss IN WBIGHT ON HBATING .5
6: SIBVB ANALYIU 6
7. DaTBIlMINATION OF ApPAllUIT DENim 7
8. DBTBRIIINATION OF VlICOSITY NUMBBR 8
9. DaT&IlMINATJON OF EUOTRICAL CONDUCTIVITY OF WATBR 12
EXTRACT ...

10. DETERMINATION OF PLAmCIZBR ABSORPTION NUMBER IS


11. DaTBRMIHATION OF SULPHATaD AsR 14
12. DaTBRMINATION OP TRBRIIAL STABIUTY BY CoNao RaD
METROD ••• 15

...
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11.468·1_

Indian Standard
METHODS OF TEST FOR
POLYVINYL CHLORIDE RESINS

o. FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards Institution
on 5 April 1968, after the draft finalized by the Plastics Sectional Commit-
tee had been approved by the Chemical Division Council.
0.2 The rapid increase in the use of polyvinyl chloride resins is the result
of their unique properties which vary from soft rubber-like products with
good tensile and elongation properties to rigid products with high struc-
tural modulus and excellent Impact resistance. Wide variation in hardness
combined with other properties, such as resistance to many chemicals,
oxygen and ozone, excellent dielectric strength, fire resistance and ease of
processing have promoted their use in a broad range of industrial and
domestic applications. These resins are used in the manufacture of wires
and cables for electrical purposes, film and sheeting, flooring tiles, PVC
coated fabrics ( teatherc10th ), pipes, injection moulded article!!; etc.
0.3 In this standard the corresponding methods of test given are essentially
the same as given in the following ISO Recommendations published on
this subject: •
ISO/R 60-1958 Plastics - Determination of apparent density of
moulding material that can be poured from a specified funnel.
ISO/R 174-1961 Plastics - Determination of viscosity number of
polyvinyl chloride resin in solution. '
0.4 In reporting the result of a test made in accordance with this standard,
if tbe final value, observed or calculated, is to be rounded off, it shan be
done in accordance with IS: 2-1960-.

1. SCOPE
1.1 This standard prescribes methods of test for polyvinyl chloride resins.
2.TBRMINOLOGY
2.1 For the purpose bfthis standard, the definitions given in IS: 2828-I964t
and the following shall apply.
-llula lor rouodiDt 0&" Dumerical vaiuel (mUitI).
tGloIIary 01 termI UIed in the plutica lDduatry.
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2.1.1 K- Val," - is obtained from the following formula :


I + ( 200 +-2 + 1·5;--;Ir-og-.t---')~i '5 log.t
e
A /

1'5 log.t - 1 + 'V


1 000 x -- 150 + 3 c - - - - - - - -
where
.t == relative viscosity. and
e = concentration in g/IOO ml.
2.1.2 Viscosity Numb" - The relative change of viscosity, divided by the
conctntration in g/l00 ml of the dissolved substance.

3. SAMPLING
3.1 Representative samples of the material shall be drawn as prescribed in
the relevant material specification.

4. Q.UALITY OF REAGENTS
4.1 Unless otherwise specified, pure chemicals and diJtilled water (I"
IS ~ 1070-1960-) shall be employed in tests.
NOTa - ' Pure cbemic:ab • iball mean chemicals tbat do not contain impwida wbicb
"eet the result. of analysis.

5. DETERMINATION OF LOSS IN WEIGHT ON HEATING


5.1 Proced.... -Weigh accurately about 5 g of the material in a tared
weighing bottle of about 50 ml capacity and 50 mm diameter. Place the
weighing bottle in an air circulatins oven maintained at 105 ± 2°C with
its cover half open for one hour. Remove the weighing bottle tiom the
oven, put t~e lid on and cool it to room temperature in a desiccator.
Weigh the bottle again. Carry out this determination three times. .
5.2 Calctalatloa
. .
Loss in weight on heating. .A _ B
percent by weight - A_ c x J00
where
.d =- wei~ht in g of the weighing bottle with material bd>re
drytng.
B - wei,ht in g of the weighing bottle with material after
drytng, and
C - weight in g of the weighing bottle.
----------------
.Speclfication for water. distilled quality ("I1iMl).

5
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5.3 Report - The mean of the three determinations shall be reported as


the representative value of the loss in weight on heating of the material.

6. SIEVE ANALYSIS
6.0 (hatHae of the Method - This method is used to determine the
particle size distribution and therefore is useful for determining lot-to-lot
uniformity of polyvinyl chloride resins. This method is applicable to the
powdered polymers of vinyl chloride having a particle size larger than
44 microns.

'.1 A......ta.
6.1.1 Sims - conforming to IS: 460-1962*.
6.1.2 Vibratift, D,viu
6.2 Proeedvre - Wei,h accurately about 25 ± 0'01 g of the sample.
Transfer the sample mto a set of sieves consisting of screens of 250,
200, 150, 100 and 75 microns along with a small quanti!}' of carbon
black (0'08 g is sufficient). The carbon black helps to ebminate any
Ita tic electricity. Shake the assembled sieves in the vibrating device
for 10 minutes.
Nora 1 - Check the tear or hole of IIC1'eeD or the aieve before teat.
Non 2 - The liae or openiDa or the lievealhall be examined periodically.
Nora S - 81eveiMould be 01 l1pt.CClDltnacUoA uadlO em in diameter to IacWtate
accurate welahJnl.
6.2.1 Mter screening, collect quantitatively the residue on each acreen
into separate bottles which have been weighed previously, using a funnel
and a gentle pat on the wall of the sieve. Weigh the bottles with thcae
residues.
6.3 C.Ica1.doa - The particle size distribution is indicated by the
percent quantity retained on each sieve. Let a"t J, e, d and I be the percent
weight in grams of the residue retained on ,,50, 200, 150, 100 and 75
micfon sieYts tfJIpeetiYlly:
a) Material retained on 250-micron sieve, =a
percent by weight
b) Material retained on 200-micron sieve,
percent by weight
c) Material retained on ISO-micron sieve.
percent by weight
*Sped8eadoD lor _linea ( ...... ).
6
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18.-'.1_
d) Material retained on lOO-micron sieve,
percent by weight
e) Material retained on 75-micron sieve, = a + b + c '.- d + ,
percent by weight
7. DETERMINATION OF APPARENT DENSITY
7.0 OatUae or the Methocl- This method of test describes the procedure
for determining the apparent density, for example, the weight per unit of
volume, of loose material that can be poured from a funnel of specified
design. The apparent density is to a certain extent a measure of porosity
of the resin particles which affect the resin dry blending characteristics.
When the method is applied to relatively coarse materials, rather variable
results may be obtained, owing to the error introduced when a straight-
edge blade is drawn across the top of the cylinder.
7.1 Apparatu.
7.1.1 Measuring Cylinder - smoothly finished inside, which may be
constructed of metal, of a capacity of 100'0 ± 0'5 ml and an internal
diameter of 45 ± 5 mm.
7.1.2 Funnel - of the form and dimensions shown in Fig. I.

"~
Ft ..I
METAL WITH
30 32 ---I SMOOTH INNER
SURFACES
~ ~~~~~~

r
t:=
1
~
--t- ----I - - - ---+-&

FlO. I FuNNaL
7.2 'PI'OCedan - Support the funnel ver~lr with its lower orifice 20 to
SO mm above the measuriDg cylinder and colllual with it. The IaDlple is
well mixed before test. With the lower orifice closed by any convenient
means, place a quantity of 110 to 120 mt of the resin in the funneL Allow.
the material to flow into the meaaurillJ cylinder. Ifnecessary, the material
may be assisted to flow by loosenins It with a rod. When the meaaurins
cylinder is full, draw a straight-edge blade across the top of the vaeel to
remove excea material. 'Weigh the contents of the measuring cylinder to
the nearest 0'1 g. Two determinations shall be made 'on the sample under
telt.
7
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11,"·1_
7.3 CalcaJadOD uti z.pn••OD oI ....Ju
7.3.1 Calculate the apparent density of the moulding material under
test by dividing by 100 the weight of the contents of the measuring
cylinder, in grams, and taking the arithmetic mean of the two
determinations.
7.3.2 Express the result in grams per millilitre ( glml ).
I. DETERMINATION or VISCOSITY Nt1MBER
1.0 O.tIlDe 01 the MetIaotl- The method of test describes the determi-
nation of the viscosity number of a solution in cycIohexanone of poly-
vinyl chloride resin. The times of Bow of the solvent and a solution ofreslll
are measured at 27°0 by conventional methods and the viscosity number
is calculated from these measurements and from the known concentration
of the solution. Density difference and kinetic energy corrections are small
in thi. method and are not applied.
1.1 Apparatu
8.1.1 Automat" Pi/JIlt, - of 50-ml and 150-ml capacity.
8.1.2 FIItIIIII- sintered glass filter funnel No. G 3.
8.13 Thmnoslalu: Balla - maintained at 27 ± 0'05°0.
8.1.4 Yisco",.'" - suspended-level Ubbelohde type of which the essential
dimensions are as shown in Fig. 2. Alternatively, any other vi~cometer
which can be shown to give the same results may be used.
8.1.5 Slop-Walth - reading to 0'1 second.
8.2 ReapDt
8.2.1 Redistilkd C"dohuano", - the fraction, distilling between J55
and 15600 at a pressure of 760 mm Hg, being collected in a brown bottle
and stored in the dark.
1.3 Procecl.... - Olean the viscometer with a mixture of equal volumes
of concentrated sulphuric acid and a saturated solution of potassium
dichromate in water. Rinse it then with water followed by acetone and
dry by drawing through it a stream of air free from dust. Weigh a quantity
of 0'500 ± 0'005 g of resin to the nearest 0'000 2 g and transfer quantita-
tively to the 50 ml glass-stoppered volumetric fluk. Add approximately
40 ml of redistilled cyclohexanone, care being taken to avoid the formation
of lumps, and insert the .topper. The mixture· is then warmed for. to
1 hour at a temperature of 80° to asoO and occasionally shaken gently
until the resin hal dissolved. The IOlution is then cooled to 27°0 and the
volume made up to the 50 m1 mark. Filter the liquid through the sintered
8
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1S ...,-I_
A 8

GRADUATION MARKS
DELIMITING A VOLUME
OF 4 T06ml

125 TO 135 CAftlLLARY OIl.


0'55 TO O'SSm",

as TO"

FILLING MARKS

All dimmaiona in millimetrc:a.


Flo.'2 UBBBLOHDB VISCOMBTER

glass filter funnel directly into Tube A of the viscometer, which should be
immened in the bath maintained at 27 ± 0'05°0, to a depth of approxi-
matel)' 20 mm above the upper graduation mark and supported so that
Tube A is vertical. The volume of liquid in the viscometer shall be such
that, after draininl5' the level shall lie between the two filling marks. After
not lest than 10 mm, the liquid is blown with dust-free air or drawn into
9
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18, . . ·1_
the upper bulb until it reaches approximately the centre of the bulb. Then
place the finger over Tube B until the liquid drops away ft'om the lower
end ofthe capillary. After removing the finger, measure the time interval
for the passage of the meniscus between the two graduation marks. Then
blow or draw the liquid into the upper bulb and measure again the time of
flow. The time of flow of the solution shall be the mean of the two deter-
niinationa, which should not differ by more than 0'4 second. The mean
time of flow of the redistilled cyclohexanone is determined in the same
manner.
8." Calca1.doD .ad £.p.....IOD of Renlt.
"
V 1SC000ty number' - '.
... ~
' . l.t
where
, = time of flow in leConds of the solution,
'. = time of flow in seconds of the redistilled cyclohexanone, and
C -= concentration in g of resin per millilitre of solution •
.....1 The viscosity number is reported to the nearest whole number. If
the samp'le has been dried or subjected to any other treatment before test,
the detads shall also be reported.
8 ....2 Table 1 provides a chart for interconversion of viscosity number
and K·value for one percent solution of PVC in cyclohexanone.

T.uLB 1 INTBRCONVEBSlON OP VISCOSITY NUMIIER. AND ~VA.LtJB


FOR ONE PERCENT IOLUTION OP PVC IN CYCLOIlEXANONB
V8ODIII'Y K-VALtIa VIIOOIITY K-VALtIa VIICOII'l'Y K·VALtIa
No•. No. No.
68 50·11 83 54075 98 58·75
69 ~3 84 5500S 99 59000
70 50·76 85 55·31 100 59015
71 51·09 86 55-59 101 59049
72 5H2 87 55·87 102 5907.
73 51-7. 88 56·1. 103 59098
7. 52·06 89 56·.2 10. 80022
75 52·37 90 56·69 105 6C)046
76 52·67 91 56·" 106 60-69
77 52·97 92 57·21 107 60-93
78 53·27 93 5H7 108 6 ... 7
79 53.57 9t 57-74 109 61-40
80 53·87 95 MJo()() 110 61 . .
81 5... 7 96 MJ'25 III 6NI5
82 5H6 97 58'50 112 62-07
(Cu.... ~)

10
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IS . . . . 1 "

TABLE I INTERCONVB1UJION 01' VISCOSITY Nt1MBD AND ~.vA.LtJE


-
1'0" ONE PDlc::DUn' 801.'UTl0" or
I'V'C IN CYCLOHEXA.NONE - rM/'d

VIIClOIITY K·VALtIa VIIOQIITY K·VALUI V.lOOIITY K,VALUI


No. No. No.
113 62·29 151 69.71 189 75-63
114- 62·51 152 69·88 190 75·77
115 62-73 153 70·05 191 75'91
116 62·94- 154 70·22 192 76·05
117 63·16 l.55 70·39 193 76'19

118 63-38 156 70·56 194- 76·32


119 63·60 157 70·73 195 76·46
120 63·81 1.58 70·90 196 76·60
121 64·02 159 71'07 197 76·73
122 64'23 160 71·23 198 76'87

123 64044- 161 71-40 199 77'00


124 64·64 162 71-56 200 77-13
125 64·84 163 71·71 201 77·27
126 65·04 164 71·87 202 77-40
127 65-25 165 72·03 203 77-53

128 65045 166 72'18 204 77·66


129 65·65 167 72-94 205 77-79
ISO 65·85 168 72.50 206 77·92
lSI 66004 169 72·66 207 78·05
112 66·24- PO 72·82 208 71·11
ISS 66·44 171 72·97 209 78·31
154 66·63 172 73012 210 78·44
155 66·82 173 73-27 :m 78'57
·156 67·00 174 73042 212 78·70
IS7 67-19 175 73·57 213 78·83

lSI 67-38 176 7S073 214 78·95


159 67·57 1'7 73·88 215 79-08
140 • 67-75 178 74·03 216 79'20
1+1 67·98 179 74-18 217 79'32
It~ ~'II Jl'O 7H2 218 79'f5
143 68·30 III 7·'-47 219 79',57
144 68·48 182 74·62 220 79'70
Its 68·66 183 74076 221 79'82
1. 68·84 184 7+91 222 79'M
147 69'Ol 185 75-06 223 80-06

148 69·20 186 75-20


149 &9'37 187 75-35
150 69·,54 188 15-49

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11 . . . . ·1_
•• DETERMINATION OP ELECTRICAL CONDUCTIVITY 01'
WATER EXTRACl
'.0 o.tUlie of the Method -This test is intended to distinguish
between electrical and non-electrical grades of unprocessed resin.
A water'
dispenion of the resin is prepared and the electrical conductivity of the
suspension measured. The conductivity of the water ~tract results from
iomc impurities in the resin which adversely affect its use for electrical
insulation.
'.1 Apparat••
9.1.1 IIC Wk4IJlstonl Brit/g, - having a range up to 250 000 ohms, a
1 000 ± 50 cycle oscillator, and a sensitive null point indicator, with
minimum accuracy ± 2 percent.
9.1.2 Condru:tivi9t C,U- having a cell constant of about 0'5 reciprocal
centimetre ( 0'5 cm- 1 ).
9.1.3 Wide-Moulk4d Flat Bottom,d Flask willa Ground-Glass SloPP", - 250 ml
capacity.
9.1.4 M,asuring Cylindm -10 ml and 100 ml capacity (mIS: 878-
1956- ).
1.2 ReageDt.
9.2.1 High Puri9t WaUT - having a conductivity of not more than 2'5
microhms per em.
9.2.2 M,thanol-mIS:517-1967t.
9.3 Procedure - Weigh accurately about' 5 g of the material, to the
neared 0'01 g, and transfer it to a wide-mouthed fiat bottomed flask with
ground glass-stopper which has been previously rinsed twice with high
purity water. Add 10 ml of methanol in the flask and swirl the mixture
until the resin is uniformly wet. Add 90 ml of high purity water in the
flask and close the flask with the stopper. Allow the resulting suspemion
to stand at 27°C ± I deg for 24 hours with frequent shaking. Measure
the conductivity of the suspension without filtration. Make blank defer.
mination using 10 ml of m<:thanol and 90 ml of high purity water.
Subtract the blank value from the value of the conductivity of the s~pen­
sion. Carry out the determination in duplicate.
9.4 Report - The mean of the two determinations shall be taken as the
representative value of the electrical conductivity of the water extract and
shall be expressed in microhms per centimetre. If the variation between
the two values is more than ±5 percent, then discard the values and
repeat the test.
·Specification (or graduatrd measurin, cylinders.
tSpeciJication for metbanol (metbylalcohol) (firsl rmriM).

12
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11 ..,.1_
10. DETERMINATION OF PLASTICIZER ABSORPTION ~VMBE1l
10.0 OatHae 01 dae Metlaocl - This method covtrs the measurement of
the amount of plasticizer that a resin can absorb at 27 ± 2·0. Plasticizer
absorption is one of the parameters for judging the dry blending properties
ofa resin.
10.1 Apparatas
10.1.1 Burette - 10 ml capacity (conforming to class A of IS: 1997.
196)· }.
10.1.2 Glass or Gla.:,£d Porcelain Tile -- about 250 X 250 X 6 mm size.
10.1.3 Mould - aluminium or brass, as shown in Fig. 3.

...u::=====~~
.....--100 ----l
PLATE (PORCELAIN OR GLASS)
Non. - Tolerance on all dimcnUoni Ihal,l be :!: 0'2 mm.
All dimc.wona in millimctrea.
F.o. 3 MOULD ,oa PLASTICIZBR ABSORPTION TEST

10.1." Stainltss Su,' Spatula - with width and shape to fit mould cavity
(St, Fig. 3 ):
10.2 Ilealcat
10.2.1 Plastick,n - ni-2~ethyl-.hex)-1 phthalate ( nop ), with a density
of 0'986 glml at 27°C (SIllS: 3672-1966t ). ' ,
10.3 Proceclare - Fill the bureUe with the plasticizer to the zero mark.
Weigh' 5'00 ± 0'01 g of the material and transfer it to the gtui or glazed
porcelain tile. Begin adding the DOP ~o the material from the burette in
.SPeci&cation for burette.. (Since revlaed).
tSpecification for octyf phthalate pluticii&en.

1.3
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11.4669.1968
0'5-ml increments using the spatula to distribute the plasticizer uniformly
in the resin. Continue adding plasticizer tiJl the mass shows indication of
becoming fluid. At this stage reduce the rate of addition of plasticizer to
0'05 ml at a time and make consistency determination until the end point
is reached. The consbtency determination is done by filling the mould, u
it rests on the plate, with a mixture and then sliding the spatula under the
charge. The charge is lifted above the mould cavity with a spatula
horizontal and the blade then rotated to a vertical position. The end point
is reached when the mixture fint slides off the blade. Carry out the
determination in duplicate.

10.t CalcaJadoD
Plasticizer absorption,
parts per hundred (phr) == 19'7 X v
where v is the total volume in rol of DOP plasticizer used in the teat.
10.5 Report - The mean of the two determinations shall be reported
as the plasticizer absorption number of the material.

11. DETERMINATION OF SULPHATBD ASH


11.0 OutllDe or the Methocl- The material is ignited in a mume
furnace after wetting with sulphuric acid.

11.1 RealeDt
11.1.1 Conc,n'rated Sulp"*rie Acid - reagent grade.
11.2 Procedure - Weigh accurately about 1 to 2 g of the teat aample in
a pofce1ain crucible of about 30 ml capacity, tared to constant weight
after ignition at about 800°C in a mufBe furnace. Add the minimum
possible quantity of concentrated sulphuric acid necessary to wet the
sample, evenly close the cover of the crucible and heat on the sand bath.
After cracking and carbonization is over ( lie Note), put the crucible in a
muffle furnace for igni tion at 800°0 for two houn. After ignition, cool the
crucible to room temperature in a desiccator and weigh to a constant
weight.
Non - Carbonization i. l'eC\uired Wore ignition .ince an explOlive combustion
takes place if the crucible ia put m a fW'D&Ce immtdiately after addition of lulpburic
acid.

11.3 Calca1adoD

Ash content, percent by weight - ~ ~=~ ~ X 100

If
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18, . . . 1_
where
A .... weight in g of the empty tared crucible,
B = weight in g of tbe crucible with the sample, anrf
C = weight in g of the crucible with the residue after ignition.

12. DETERMINATION OF THERMAL STABILITY BY CONGO


RED METHOD
12.0 OaillDe or the Methocl- By thermal stability or thermal life of
a resin of vinyl chloride polymer is meant the time, in minutes, from the
moment at which the material is exposed to a given temperature until
the first sign of decomposition is observed. The mode of decomposition
is the splitting off of hydrochloric acid. In this, the sample is heated in
an oil bath to a specific temperature and the time taken for the vapoun to
cauae a colour change in congo red paper is noted.
12.1 Apparata.
12.1.1 TId- Tubes - of diameter 16 ± 0'1 mm, wall thickness 0'4 ±
0'2 mm and length at leut 150 mm.
12.1.2 Glass Tubes -2 to 3 mm in internal diameter and about 100 mm
in length.
12.1.3 Oil Bath - fitted with stirrer and a thermostatic control, capable
of maintaining the temperature within ± 1°C in the range from 120 to
210°C. The bath shall also be fitted with suitable clamps for holding a
sufficient number of te<lt-tubes immersed to a depth of 50 mm.
12.2 RealeDt
12.2.1 Congo Red Indi&alor Paper Strips ~ 10 mm wide. The indicator
paper is prepared by immersing strips of filter paper in a 0'15 percent
solution of congo red in methanol ( see IS: 517-1967* ), and drying them.
12.3 Proced~re
n.3.1 For each sample, at least two determinations shan be carried out
in two separate test-tubes, which sball be immersed in the oil bath at the
same time. The preferred temperature of the oil bath is 180 ± 1°C.
Other temperatures may be wed provided that the duration of the test is
not less than 20 minutes and not more than 5 hours.
12.3;2 'Place the sample in the test tube and gently shake it down, taking
care to ensure that the pieces do not form a compact mass. Close the test
tube with a cork having at its centre the glass tube with a congo red paper
.SpeciflcatioD for metbaDol (mttbyl alcohol) (./irsl "lIiIiOII ).

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•. .,·1_
strip 30 mm long and 10 mm wide. The congo red strip i. folded or
rolled at one end, which is inserted into a glass tube. The tube is made
to slide in such a way that the lower edge of the paper is placed 25 mm
above the top of the specimen. Immerse the test tube thus prepared in
the oil bath which is already brought to the given temperature, up to the
level of the upper surface of the sample.
12.3.3 The time, in minutes, from the insertion of the teat tube in the
hot oil to the time when the indicator paper shows the first clear signa of
a change from red to blue, is recorded. Sometimes, with certain stabilizers
in the sample, the colour change is only slow and not very distinct; in these
cases, two different times shall be recorded, corresponding to the first lign
of colour changing from red to violet and to the permanent change from
violet to blue.
12.4 Report
12.4.1 Report the mean of the two determinations.
12.4.2 The report shall include the following information:
a) The complete identi6cation of the material tested and, if desired,
the formulation of the compound and the thermal t.reatment
during the preparation of thc test specimens;
b) Test tcmperatuTe; and
c) The time before the colour change of the indicator paper, ..
specified under 12.3.3 or in the case of a slow change of colour,
the two different times as specified under 12.3.3.

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BUREAU OF INDIAN STANDARDS


Headquarters:
Manak Bhavan, 9 Bahadur Shah Zalar Marg, NEW DELHI 11 0002
Telephones:23230131,23233375,23239402 Fax:91+01123239399,23239382
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Regional Offices:
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Bittan Market, BHOPAL 462016
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Pat1iputra Industrial Estate, PATNA 800013 2262808
First Floor, Plot Nos 657-660, MarketYard, Gultkdi, PUNE 411037 4268659
"Sahajanand House· 3'" Aoor, BhaktinagarCircle, 80 Feet Road, 2378251
RAJKOT 360002
lC. No. 1411421, University P.O. Palayam, THIRUVANANTHAPURAM 695034 2339174
1" Floor, Udyog Bhavan, VUDA, Sirlpuram Junction, VISHAKHAPATNAM-03 2712833

·Sales Otfice is al5 Chowrlnghea Approach, P.O. Prlncep Street, KOLKATA 700072 23553243
·Sales Office Is al Novelty Chambers, Grant Road, MUMBAI400007 23096528

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