KENYA STANDARD KS 1180: 2012

Specification for ethyl methyl ketone

(butanone for industrial use)

© KEBS 2012
 TECHNICAL COMMITTEE REPRESENTATION

The following organizations were represented on the Technical Committee:

Agrochemical and Food Company

University of Nairobi
Kenyatta University
KIRDI
Government Chemist
MOR – Materials Dept.
Consumer Information Network
Spectre International
Marshall Fowler
Kel Chemicals
Associated Battery Manufacturers
Unilever (K) Ltd
Pan African Chemicals
Athi River Mining
Ministry of Medical Services
Galaxy Paints and Coatings
Agricultural Association of Kenya
Betachem Chemicals
TATA Chemicals Magadi
Kenya Bureau of Standards Secretariat

REVISION OF KENYA STANDARDS

In order to keep abreast of progress in industry, Kenya Standards shall be regularly reviewed. Suggestions
for improvements to published standards, addressed to the Managing Director, Kenya Bureau of Standards,
are welcome.

© Kenya Bureau of Standards, 2012

Copyright. Users are reminded that by virtue of section of the Copyright Act, Cap. 12 of 2001 of the Laws of Kenya, copyright subsists
in all Kenya Standards and except as provided under section 26 of this Act, no Kenya Standard produced by Kenya Bureau of
Standards may be reproduced, stored in a retrieval system in any form or transmitted by any means without prior permission in writing
from the Managing Director.
KENYA STANDARD KS 1180: 2012

Specification for ethyl methyl ketone

(butanone for industrial use)

KENYA BUREAU OF STANDARDS (KEBS)

Head Office: P.O. Box 54974, Nairobi-00200, Tel.: (+254 020) 605490, 602350, Fax: (+254 020) 604031
E-Mail: info@kebs.org, Web:http://www.kebs.org

Coast Region Lake Region Rift Valley Region

P.O. Box 99376, Mombasa-80100 P.O. Box 2949, Kisumu-40100 P.O. Box 2138, Nakuru-20100
Tel.: (+254 041) 229563, 230939/40 Tel.: (+254 057) 23549, 22396 Tel.: (+254 051) 210553, 210555
Fax: (+254 041) 229448 Fax: (+254 057) 21814
DKS 1180: 2012 ©KEBS

Preface

This Kenya Standard was prepared by the Technical Committee on Industrial solvents and chemicals under
the authority of Kenya Bureau of Standards.

This second edition of the standard has put into consideration revision of parameters including the distillation
o o
range at 77 C to 81 C; refractive index to 1.370 to 1.380 since butanone is for Industrial use. The
determination of color has been done using Lovibond Scale instead of platinum – cobalt scale.

Butanone is a colourless liquid ketone with a sharp sweet odor reminiscent of butter scotch and acetone. It is
completely miscible with many organic liquids. With resins, it produces low viscosity and high solids content
solutions.

It is mainly used as a low boiling solvent for nitrocellulose, acrylic, vinyl, alkyd and other natural and synthetic
resins; and as a denaturant.

This Kenya Standard specifies important characteristics such as distillation range, water content, acidity
among others.

During the preparation of this standard, reference was made to the following publications and
acknowledgement is made for its assistance with thanks:

• BS 1940:87, Specification for Butanone for Industrial use.

• Laboratory tests from different industries

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©KEBS DKS 1180: 2012

KENYA STANDARD

SPECIFICATION FOR ETHYL METHYL KETONE

(BUTANONE FOR INDUSTRIAL USE)

1. SCOPE

This Kenya Standard specifies requirements and methods of test for butanone suitable for industrial
use.
It has a chemical formula of C 4H 8O and a chemical structure as below.

2. REQUIREMENTS

Butanone shall satisfy the requirements specified in the Table below:

SL.NO Characteristics Requirements Method of test

1 Appearance Clear and free Visual
from suspended
matter
2 Colour, Hazen units 10 max Appendix A
0
3 Density g/ml at 20 C 0.803-0.806 Appendix B

4 Distillation range at 1013 mbar, ºC Appendix C

IBP 77.0
D.P 81.0
5 Residue on evaporation % (m/m) 0.002 max Appendix D
6 Water content % (m/m) 0.15 max Appendix E
7 Acidity calculated as acetic acid % (m/m) 0.004 max Appendix F
8 Alcoholic impurities calculated as butanol 0.7 max Appendix G
% (m/m)
9 Refractive index at 20ºC 1.370-1.380 Using a refractometer
10 Flash point, ºC -5.0 to -3.0 Appendix I
11 Evaporation rate (n-BuAc=1) 3.7 Appendix J

4. MARKING AND PACKING

Butanone shall be packaged in suitable and serviceable containers and marked indelibly with the
following information:

(a) Manufacturer’s name and/or registered trade mark; and address

(b) Net weight;

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DKS 1180: 2012 ©KEBS

(c) The words ‘inflammable’ and its Standard Symbol;

(d) Precautionary measures i.e. may cause irritation to the eyes, respiratory system and skin.

(b) Country of origin.

APPENDIX A

DETERMINATION OF COLOUR IN HAZEN UNITS

(LOVIBOND SCALE)
A.1 PRINCIPLE

Visual comparison of the colour of a sample with that colour of standards, and expression of the
result in terms of hazen

Note:For routine control purposes an instrument such as a comparator, colorimeter or

spectrophotometer may be used, provided that it has first been established that the results so
obtained are identical with those obtained by visual comparison.

A.2 REAGENTS

Distilled water, or water of equivalent purity, shall be used in the test.

A.3 APPARATUS

Ordinary laboratory apparatus and the Lovibond comparator

A.3.1 Two colorimetric tubes, flat based if possible, with a graduation mark at least 100 mm above the
base and matched especially with respect to colour of glass and height of graduation mark above the
base. Suitable tubes are available commercially as 50 mL or 100 mL Nessler Cylinders.

For the measurement of low colorations (less than 50 Hazen Units), the height of the graduation
mark above the base must be greater than for the measurement of deeper colours and must be
sufficient that, on looking through this greater depth of liquid, clear distinction between the standard
Hazen matching solutions can be observed.

NOTE: 1. For routine control purposes, a colorimetric or spectrophotometer may be used, the
instrument being standardized by means of the standard colorimetric solutions
provided that it has been confirmed that the use of that instrument gives the same
results as does visual comparison.

A.4 Expression of Results

Express the colour of the sample as the number of Hazen colour units

A.5 TEST REPORT

The test report shall include the following particulars:

(a) the reference of the method used

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(b) the result, expressed in Hazen colour units

(c) any unusual features noted during the determination

(d) any operation not included in this standard or regarded as optional.

APPENDIX B

DETERMINATION OF DENSITY
B.1 PRINCIPLE
B.2 Determination of the mass at 20ºC of a volume of the material contained in a pyknometer flask, and
determination of the volume of the latter by determining the mass of a corresponding volume of
water at 20ºC calculation of the density is done by dividing the mass of the material by the volume of
the flask.

B.3 APPARATUS

Ordinary laboratory apparatus, and the following in particular:

*
B.3.1 Pyknometer flask — type 3 (Gay-Lussac) (see ISO 3507) , made of glass and of a size and type
suitable for use with the material under test, preferably 25 or 50 mL (see Fig. 1)
0
B.3.2 Water bath —capable of being controlled at 20 ± 0.1 C.

B.4 PROCEDURE

Clean and dry the flask (B.3.1) and weigh it, with its stopper, to the nearest 0.001 g. Fill the flask with
freshly boiled and cooled distilled water, and determine the apparent mass of the contents,
0
previously brought to 20 ± 0.1 C. in the water bath (B.3.2)

Empty, clean and dry the flask, fill it with the sample under test, and determine in a similar manner
0
the apparent mass of sample contained in the flask at 20 C.

NOTE: With volatile liquids, it is essential that suitable precautions be taken to avoid loss by
evaporation.

*
Pyknometers
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FIG. 1 — 50 PYKNOMETER FLASK, TYPE 3 (GAY – LUSSAC)

B.5 EXPRESSION OF RESULTS

0
The density of the sample at 20 C, in grams per millilitre is given by the formula:

m1 + A
Xp
m2 + A

Where,

0
m1 is the apparent mass in grams of sample required to fill the flask at 20 C,

0
m2 is the apparent mass, in grams, of water required to fill the flask at 20 C,

0
p is the density of water at 20 C = 0.9982 g/mL,

A is buoyancy correction = pa x m2

Where pa is the density of air approximately 0.0012 g/mL.

Calculate the result to three decimal places.

B.6 Other suitable methods for determination of density may be used such as use of hydrometer,
densimeter, provided that the results so obtained are identical with those obtained above.

B.7 TEST REPORT

The test report shall include the following particulars:

(a) the reference of the method used;

(b) the results and method of expression used;

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©KEBS DKS 1180: 2012

(c) any unusual features noted during the determination;

(d) any operation not included in this standard or in the standard to which reference is made or
regarded as optional.

APPENDIX C

DETERMINATION OF DISTILLATION RANGE

C.1 PRINCIPLE

Distillation of a test portion, under carefully defined conditions in order to determine either.

C.1.1 The temperature corresponding to the condensate volumes defined in the standard for the product
under test, these temperatures shall be corrected as indicted in 6.7. Unless the nature of the product
provides only for a difference of temperature between two volumes of condensate (plotting
temperature as a function of volume) or

C.1.2 The volume of condensate when the thermometer indicates each of the distillation temperatures
(previously adjusted as indicated in C.6) specified in the standard for the product under test (plotting
volume as a function of temperature).

C.2 APPARATUS

Ordinary laboratory apparatus and the following in particular:

C.2.1 Distillation apparatus — as shown in figure 2 comprising.

C.2.1.1 Distillation flask — available capacity 100 ml of borosilicate glass as shown in figure 3.
0
C.2.1.2 Thermometer — use a thermometer designated F 100 C /100
*
C.2.1.3 Receiver — 100 mL capacity graduated as shown in figure 4, complying with BS 593 .

C.2.1.4 Condenser of the Liebig/West type — of borosilicate glass as shown in figure5. The inner tube shall
have the following dimensions:

Internal diameter 14.0 ±1.0 mm

Wall thickness 1.0 to 1.5 mm

Length of straight portion of longer limb 600 ± 10 mm

Length of shorter limb 55 ± 5 mm

Angle included between longer and shorter limb 97 ± 3 ºC.

The inlet of the inner tube of the condenser shall be finished square with its axis and its outlet,
smoothly ground at an angle of approximately 45ºC to the axis of the tube at that point as shown in
Figure 5.

*
Laboratory thermometers.
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FIG. 2 — ASSEMBLY OF DISTILLATION APPARATUS

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FIG. 3 — DISTILLATION FLASK

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FIG. 4 — DISTILLATION RECEIVER

The length of the central straight portion of the water jacket shall be 450 ± 10 mm, and its external
diameter 35 ± 3 mm.

C.2.1.5 Draught Screen — Rectangular in cross-section and open at the top and bottom. It shall have the
dimensions shown in Figure 6 and shall be made of sheet metal, 0.7 mm thick.

In each of the two narrower sides of the draught screen are two air-vent holes 25 mm in diameter
situated below the heat-resistant shelf, as shown in figure 6.

In each of the four sides of the draught screen are three air-vent holes with their centre 25 mm
above the base of the draught screen. These holes occupy the positions shown in Figure 6, the
diameter of the holes situated centrally in the wider side being 25 mm and the diameter of the
remaining 10 holes 12.5 mm.

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©KEBS DKS 1180: 2012

At the middle of each of the wider sides, a vertical slot for the side tube of the distillation flask
dimensioned as shown in Figure 6, is cut downwards from the top of the screen. A removable shutter
conforming to the dimensions in figure 6 is provided for closing whichever vertical slot is not in use.

A shelf of hard heat-resistant board 6 mm in thickness and possessing a centrally cut circular hole
110 mm in diameter, is supported horizontally in the screen and fits closely to the sides of the screen
to ensure that hot gases from the source of heat do not come into contact with the sides ore neck of
the flask. The supports for shelf may consist of triangular pieces of metal sheet firmly fixed to the
screen at its four corners.

FIG. 6 — DRAUGHT SCREEN

In one of the narrower sides of the screen, a door is provided having the dimensions shown in figure
6 and overlapping an opening in the screen by approximately 5 mm all round.

In each of the narrower sides of the screen, a mica window is placed centrally with the bottom of the
window level with the top of the heat-resistant shelf. The dimensions and the positions of the
windows are shown in figure 6.

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DKS 1180: 2012 ©KEBS

C.2.1.6 Heat-resistant board — In addition to the heat resistant shelf referred to in C.2.1.5, a heat resistant
board 150 mm square and 6 mm in thickness is required. It has a central hole 50 mm diameter,
unless otherwise stated in the specification for the material under test.

C.2.2 Assembly of apparatus — Assemble the distillation apparatus as shown in figure 2.

C.2.2.1 Position of thermometer — The thermometer shall be held in the neck of the flask by means of a well
fitting stopper of a material which is not attacked by the liquid under test. The junction of the capillary
tube and the main bulb of the thermometer shall be maintained level with the lower edge of the joint
between the side tube and the neck of the flask. The stopper shall project about 10 mm above the
top of the neck of the flask.

When the thermometer is fixed in position as indicated above, the immersion line on the
thermometer will be in the neighbourhood of the top of the stopper holding the thermometer in
position in the neck of the flask.

C.2.2.2 Support for flask — The heat resistant board (C.2.1.6) shall be placed on the top of the heat-
resistant shelf of the draught screen so that the two holes are approximately concentric. The flask is
then placed in position so as to close the hole in the heat-resistant board completely.

C.2.2.3 Connection of flask to condenser — The flask shall be connected to the condenser so that the end of
the side tube projects at least 25 mm into the condenser and is coaxial with it.

C.3 Sample size — To carry out this test a laboratory sample of 500 mL is recommended.

C.4 PROCEDURE

C.4.1 Test Portion — Using the receiver (C.2.1.3) take 100 ± 1 mL of the laboratory sample.
0
If the expected distillation temperature lies below 70 C, adjust the temperature of the sample before
taking it, to the appropriate value shown in Table 1.

TABLE 2: SAMPLING TEMPERATURE

Values in degrees Celsius

Initial boiling point Condenser Sample

Below 50 0 to 3 0 to 3
50 to 70 0 to 10 10 to 20
70 to 150 25 to 30 20 to 30
Above 150 35 to 50 20 to 30

C.4.2 Distillation

WARNING – Carry out the distillation in a well ventilated fume cupboard.

Transfer the test portion (C.4.1) as completely as possible to the distillation flask and add a few small
pieces of clean, dry porous pot. Place the flask and its contents, the thermometer and the receiver in
position and ensure that the condenser has a steady supply of water.

NOTE: For materials expected to boil below 70 ºC, the temperature of the water supply of the
condenser and the temperature of the receiver should be adjusted to the values indicated in
table 2. In this case, immerse the receiver in a transparent cold water bath maintained at the
values of temperatures indicated in Table 2.

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©KEBS DKS 1180: 2012

Regulate the rate of heating so that the first drop of distillate falls from the end of the
condenser after 10 to 15 min.

Again adjust the flame so that the condensate is collected at the rate of 3 to 4 mL/min
corresponding to approximately 2 drops per second,

This can be achieved by adjusting the distance between the bottom of the flask so that the
flame of minimum size only is necessary.

Record as appropriate,

— temperature as a function of volume (C.1.1)

— Volume as a function of temperature (C.1.2)

In addition, record the atmospheric pressure and the temperature of the barometer on taking the
reading.

C.5 CORRECTION TO BAROMETER READINGS

Atmospheric pressure is generally measured by means of a mercury barometer (Fortin type), having
a brass scale calibrated in millibars (mbar). A standard atmospheric (atm) = 1 013.25 mbar = 101
325 Pa (see ISO 31/3).

NOTE: If the barometer is calibrated in millimetres of mercury, multiply the observed value by 1.332
89 (rounded up to 1.333) in order to obtain the corresponding value in millibars.

If however, the pressure reading is given in pascals (Pa) note the following equivalent
values:
5
1 bar = 1 000 mbar = 10 Pa = kPa = 0.1 Mpa (see ISO 31/3)

C.6.1 Index Correction

C.5.1 Index correction — Initially correct the observed barometer reading in accordance with the
inspection certificate issued with the instrument. The reading thus corrected gives the atmospheric
pressure as would be indicated by a correctly adjusted barometer at the temperature and at the
latitude of the place of observation.

C.5.2 Temperature correction to 0ºC — Correct the value obtained in C.5.1 to 0 ºC, taking into account
the temperature at which the reading was taken and the type of barometer used.

If the mercury barometer is of the Fortin type, of any other type in which the mercury is set to a
fiducial level when the barometetric reading is taken, apply the correction given in Table 3.

If the barometer used is of Kew type, i.e. one which the barometric reading is taken without adjusting
the level of the mercury in the reserviour, the temperature correction will differ somewhat from that
given in Table 2. The temperature coefficient of a Kew pattern barometer depends to a small extent

on its dimensions, but sufficient accuracy will be obtained in general, if the temperature correction to
a reading of a Kew pattern barometer is taken to be 5 % in excess of that given in Table 3.

C.5.3 The barometric pressure — As corrected in accordance with C.5.1 and C.5.2 is given in standard
millibars at 0 ºC, at the place of observation. However, if the distillation is carried out in latitudes
where the value of gravity differs from the standard value, a third correction is necessary to obtain
g
the equivalent value under standard gravity. Multiply the value obtained as above by
9.806 65
where g acceleration of free fall,

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TABLE 4: CORRECTION OF BAROMETER READINGS TO STANDARD GRAVITY

Latitude
degrees Barometer reading. bar
925 950 975 1000 1025 1050 1075 1100
0 -2.48 -2.55 -2.62 -2.89 -2.76 -2.83 -2.90 -2.97
5 -2.44 -2.51 -2.57 -2.64 -2.71 -2.77 -2.84 -2.91
10 -2.35 -2.41 -2.47 -2.53 -2.59 -2.65 -2.71 -2.77
15 -2.16 -2.22 -2.28 -2.34 -2.39 -2.45 -2.51 -2.57
20 -1.92 -1.97 -2,02 -2.07 -2.12 -2.17 -2.23 -2.28
25 -1.61 -1.66 -1.70 -1.75 -1.79 -1.84 -1.89 -1.94
30 -1.27 -1.30 -1.33 -1.37 -1.40 -1.44 -1.48 -1.52
35 -0.89 -1.81 -0.83 -0.95 -0.97 -0.99 -1.02 -0.05
40 -0.48 -0.49 -0.50 -0.51 -0.52 -0.53 -0.54 -0.55
45 -0.05 -0.05 -0.39 -0.05 -0.05 -0.05 -0.05 -0.05
50 +0.37 +0.39 -0.05 +0.41 +0.43 +0.44 _0.45 +0.46
55 +0.79 +0.81 +0.40 +0.86 +0.88 +0.91 +0.93 +1.95
60 +1.17 +1.20 +1.83 +1.27 +1.30 +1.33 +1.36 +1.39
65 +1.52 +1.68 +1.60 +1.65 +1.69 +1.73 +1.77 +1.81
70 +1.83 +1.87 +1.92 +1.98 +2.02 +2.07 +2.12 +2.17

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1
Temperature Barometer reading.mbar
of 925 950 975 1000 1025 1050 1075 1100
Barometer
1.51 1.55 1.59 1.63 1.67 1.71 1.75 1.79
1.66 1.70 1.75 1.79 1.84 1.88 1.93 1.97
1.81 1.86 1.90 1.95 2.00 2.05 2.10 2.15
1.96 2.01 2.08 2.12 2.17 2.22 2.28 2.33
2.11 2.16 2.22 2.28 2.34 2.39 2.45 2.51
2.26 2.32 2.38 2.44 2.50 2.56 2.63 2.69
2.41 2.47 2.54 2.60 2.67 2.73 2.80 2.87
2.56 2.63 2.70 2.77 2.83 2.90 2.97 3.04
2.71 2.78 2.85 2.93 3.00 3.07 3.15 3.22
2.85 2.93 3.01 3.09 3.17 3.25 3.32 3.40
3.01 3.08 3.17 3.25 3.33 3.42 3.50 3.58
3.16 3.24 3.33 3.41 3.50 3.69 3.67 3.78
3.31 3.40 3.49 3.58 3.67 3.76 3.85 3.94
3.46 3.55 3.85 3.74 3.83 3.93 4.02 4.12
3.61 3.71 3.81 3.90 4.00 4.10 4.20 4.29
3.78 3.86 3.96 4.06 4.17 4.27 4.37 4.47
3.91 4.01 4.12 4.23 4.33 4.44 4.55 4.66
4.06 4.17 4.28 4.39 4.50 4.61 4.72 4.83
4.21 4.32 4.44 4.55 4.66 4.78 4.89 5.01
4.36 4.47 4.59 4.71 4.83 4.95 5.07 5.19
4.51 4.63 4.75 4.87 5.00 5.12 6.24 5.37

Table 3. Correction of barometer readings to 0 0C Fortin barometer with brass scale (subtract the
correction from the barometer reading)

1
If the barometer is calibrated in millimeters of mercury, see the note in 8.

Expressed in metres per second squared, at the place of observation. The correction to standard
gravity is carried out by reference to table 4 which gives the appropriate corrections for different
latitudes. According to whether the sign of the correction in table 4 is positive or negative, add or
subtract the value shown.

Variations in gravity due to causes other than change in latitude, e.g. height above sea level, may be
neglected.

C.6 TEMPERATURE CORRECTIONS

C.6.1 For temperature readings as a function of volume (see C.1.1) — These corrections shall be
applied after the distillation.

C.6.1.1 Corrections for thermometer error — If the thermometer gives incorrect readings at the observed
initial boiling point or dry point, correct the readings by subtracting the amount of error if the
thermometer is reading high, or adding the amount of error if the thermometer is reading low.

Also make corrections for the emergent stem of the thermometer when using a thermometer
calibrated for total immersion.

C.6.1.2 If the corrected barometric pressure deviates from 1013 mbar apply corrections to the observed
temperatures by subtracting 0.028 ºC for every millibar above 1013 mbar, or adding 0.028 ºC for
every millibar below 1013 mbar,

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NOTE: These corrections are valid only for pressures above 933 mbar.

C.6.2 For volume readings as a function of temperature (see C.1.2) — These corrections shall be
applied before commencing distillation.

C.6.2.1 Correction for thermometer error — If the thermometer gives in correct readings at the specified
distillation temperature, corrected in accordance with C.6.2.2, correct the readings by adding the
amount of error if the thermometer is reading high, or subtracting the amount of error if the
thermometer is reading low.

Also make corrections for the emergent stem of the thermometer when using a thermometer
calibrated for total immersion.

C.6.2.2 Correction for barometric pressure — If the corrected barometric pressure deviates from 1013 mbar
apply corrections to the observed temperatures by subtracting 0.028 ºC for every millibar above
1013 mbar, or adding 0.028 ºC for every millibar below 1013 mbar.

C.7 EXPRESSION OF RESULTS

Apply the corrections specified in C.5 and C.6 to the barometric pressure and temperature readings,
respectively. In order to calculate the correction which is to be applied to the coefficient of variation
of boiling point of a given product as a function of pressure (C.6.1.2 and C.6.2.2) apply the following
formula, adding algebraically the result obtained to the temperatures.

CV (1 013.25 – p) ºC

Where,

CV is the rate of change of boiling point with pressure in degrees Celsius per millibar of
the material under test.

P is the atmospheric pressure in millibars, taken during the test, corrected in

accordance with C.6.

1 013.25 I is standard atmospheric pressure in millibars

NOTE: If the overall distillation range of the test portion does not exceed 2 ºC, combined corrections
for thermometer error and barometric pressure may be made on the basis of the difference
between the observed 50 percent boiling point and the true boiling point at 1 1013.25 mbar
(see ISO 4626, Table 3).

Report the characteristics required for the product under consideration.

C.8 TEST REPORT

The test report shall include the following particulars:

(a) an identification of the sample;

(b) the reference of the method used;

(c) the results and the method of expression used;

(d) any unusual features noted during the determination;

(e) Any peration not included in this standard or in the standard to which reference is made, or
regarded as optional.

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APPENDIX D

DETERMINATION OF RESIDUE ON EVAPORATION

D.1 PRINCIPLE

Evaporation of a test portion on a water bath, and drying the residue, if any, in an oven at 110 ºC ±
2ºC to constant mass.

D.2 APPARATUS

D.2.1 Dish, of platinum, silica or borosilicate glass, of capacity about 150 mL.

D.2.2 Water bath, maintained at a temperature appropriate to the boiling point of the product under
examination.

Warning: The heating system shall be designed so as to avoid all possibility of a fire hazard.

D.2.3 Electric oven, capable of being maintained at 110 ± 2 ºC.

D.3 PROCEDURE

D.3.1 Test Portion — take 100 ± 0.1 ml of the test sample.

D.3.2 Determination — Introduce the test portion (D.3.1) into the dish (D.2.1) previously heated for 2 h in
the oven at 110 ± 2 ºC, cooled in a desicator and weighed to the nearest 0.0001 g.

Place the dish and its contents on the water bath (D.2.2) maintained at the appropriate temperature
and operating in a well ventilated fume cupboard, evaporate to dryness.

Remove the dish from the water bath, wipe the outside with a tissue and continue heating in the
oven (D.2.3) maintained at 110 ± 2 ºC for about 2 h. Remove the dish from the oven, allow it to cool
to ambient temperature in a desiccator and weigh to the nearest 0.000 1 g. Repeat the operations of
heating, cooling and weighing until constant mass is attained i.e. until the difference between two
consecutive weighing does not exceed 0.000 2 g.

D.4 EXPRESSION OF RESULTS

Percentage residue on evaporation

m1 − m o
V× ȡ
Where

mo is the mass, in grams, of the empty dish (D.1.1)

m1 is the mass, in grams of the dish plus residue

V volume in ml of test portion

ȇ is the density of butanone

The value of density used to calculate the results as a percentage by mass shall be that determined
by the method specified in Appendix B.

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DKS 1180: 2012 ©KEBS

D.5 TEST REPORT

The test report shall include the following particulars:

(a) an indication of the sample

(b) the results
(c) any unusual features noted during the determination

(d) Any operation not included in this standard or in the standard to which reference is made, or
regarded as optional.

APPENDIX E

DETERMINATION OF WATER CONTENT

E.1 APPARATUS

Complete sets of apparatus for determination of water by the Karl Fischer method are available from
the trade. These are of different types designed to meet different requirements as to sensitivity and
accuracy. In order to avoid unnecessary restrictions the apparatus is described in general terms,
except where strict adherence to a particular type or size is considered essential.

E.1.1 Reaction Vessel — The reaction vessel (see Fig. 7) has a working capacity of not less than 60 mL.
The wide neck has an airtight detachable head fitted to accommodate two burette jets (extended to
suitable length) and tubes for entry and exit of nitrogen. An additional hole, protected by a suitable
seal, accommodates the spindle of a stirrer (unless magnetic stirring is provided). Two platinum wire
electrodes extending nearly to the bottom of the vessel are either fused in through the side of the
vessel or inserted through the head, if preferred. A drain cock is provided. A side tube closed by a
translucent latex vaccine cap, provides for insertion of liquid samples without exposing the contents
of the vessel to atmospheric moisture during the operation.

NOTE: Care should be taken in the construction of the vessel to avoid excessive ‘dead space’ in the
region of the drain cock.

E.1.2 Two Burettes — The two burettes are of 25 mL capacity (or other capacity as preferred). All are
*
class A, complying with BS 846

*
Burettes and bulb burettes
18
©KEBS DKS 1180: 2012

FIG. 7 — SUGGESTED ALTERNATIVE FORMS OF REACTION VESSEL

E.1.3 Two reagent reservoirs — These are suitably connected to the burettes for gravity, suction or
pressure feed. Provision is made for drying the air used for blowing or displacing the reagents.

E.1.4 Glass stirrer — The stirrer is either mechanical driven from the above or magnetically driven from
below.

E.1.5 Electrical equipment — This is to provide for the application of not more than 20 mV to the
electrode when there is an excess of 0.2 mL of Fischer reagent. Suitable circuits are shown
diagrammatical in Figures 8 and 9.

E.1.6 Galvanometer — This has a sensitivity such that full scale deflection is obtained by a current of not
more than 100 uA. The galvanometer may be in a series with the reaction vessel or in a shunt
position. In the former case, the galvanometer will give a ‘null’ reading at the end point and in the
latter case a positive reading. For use in the series position the galvanometer should have a
resistance not exceeding 100.

E.1.7 Tapping key or switch

*
E.1.9 Pipettes* — Pipettes are of 10 mL and 20 mL capacity, fitted with hypodermic needles of about 1
mm bore (1.5 mm for use with the more viscous liquids such as the higher alkyl phthalates) and
provided with suitable protection against atmospheric moisture.

19
DKS 1180: 2012 ©KEBS

FIG. 8 — SERIES CIRCUIT FOR DOUBLE BURETTE APPARATUS

FIG. 9 — MAINS OPERATED SHUNT CIRCUIT FOR DOUBLE BURETTE APPARATUS

E.1.9 The additional hypodermic needles — These are of about 1 mm bore.

E.1.10 Weighing pipette — This is fitted with a hypodermic needle, of about 1 mm bore, in place of the
usual jet.

E.1.11 Three drying bottles — The bottles are for drying the nitrogen supply, one containing concentrated
sulphuric acid and two containing freshly activated silica gel, in that order.

20
©KEBS DKS 1180: 2012

*
E.1.12 One-mark volumetric flask — These are 100 ml capacity closed with translucent latex vaccine caps.

NOTE 1: All possible points of entry of atmospheric moisture into the apparatus (including the
suction end of the pipettes) are protected by guard tubes filled with freshly activated silica
gel or other efficient desicant. On safety grounds the use of granular magnesium
perchlorate is recommended.

NOTE 2: Silicon grease is used for lubrication of stopcocks. Petroleum jelly is not suitable owing to
its reactivity with Fischer reagent.

E.2 REAGENTS

The following reagents are required:

**
(i) Methanol, complying with KS03 and dried as described in E.3.4 or anhydrous methanol
denatured with pyridine.

(ii) Nitrogen, from a cylinder of compressed gas.

(iii) Bischer reagent, having a water equivalent 3.0 – 4.0 mg/mL. This may be prepared as described
in E.3.4.

E.3 PREPARATION OF REAGENTS

Prepare reagents by the following methods:

(i) Methanol – Dry methanol, if it is not already anhydrous by distillation over magnesium turnings
and a little iodine, or by fractioning through a 1.6 mm rectifying column and distil it into a receiver
protected from atmospheric moisture by a guard tube. Methanol dried in this manner will contain
not more than 0.03 percent of water.

(ii) Water/Methanol – To approximately 900 mL of the methanol in a 1 litre one-mark volumetric

flask add 1.5 mL of distilled water. Make up to the mark with the methanol, mix thoroughly and
transfer to the appropriate burette reservoir.

(iii) Pyridine-Distil the pyridine, collecting the fraction boiling between 114ºC and 116ºC at
2*
101.3kN/m (760 mmHg) pressure, the receiver being protected from the atmospheric moisture
by a guard tube.

(iv) Fischer reagent – Measure 800 mL of the methanol into a dry 150 mL glass stoppered flask.
Add 160 g of pyridine. Exchange the glass stopper for a two hole rubber stopper fitted with an
inlet tube reaching nearly to the bottom of the flask and a short outlet tube protected by a guard
tube. Weigh the flask with its fittings and contents and cool in ice water.

Connect the inlet tube to the siphon of sulphur dioxide and allow the gas to pass into the mixture with
continuous agitation until the total mass of the flask and its contents is increased by about 50 g. The
remove the rubber stopper and delivery tubes and add 90 g of iodine. Replace the glass stopper,
shake to dissolve the iodine and allow the mixture to stand for 24 h. Finally, transfer the prepared
reagent to the appropriate burette reservoir bottle. The water equivalent of the Fischer reagent to the
appropriate burette reservoir bottle. The water equivalent of the Fischer reagent thus prepared will
be about 3.5 mg/mL.

*
Flasks complying with BS 1972 – One-mark volumetric flasks, are suitable.
**
KS 03 — under preparation
* 2
1kN/m = 10 mbar = 7.5 mmHg.
21
DKS 1180: 2012 ©KEBS

E.4 PROCEDURE

E.4.1 Standardization of the water/methanol reagent — Run into the reaction vessel enough Fischer
reagent to cover the electrodes. Switch on the stirrer and turn on a slow stream of nitrogen. When a
series of tests begins, leave the apparatus with the stirrer running for about 15 min to allow all traces
of water to be removed. (Continue the passage of nitrogen and the stirring throughout the
standardization of the water/methanol reagent and the Fischer reagent, and the determination of
water in the sample).

Close the electrical circuit through the reaction vessel run in sufficient of the water/methanol reagent
to bring the galvanometer reading just on to the scale and allow the apparatus to remain in this
condition for about 15 min during which period the galvanometer reading should remain constant,
thereby indicating that the apparatus is dry and free from air leaks. Then continue the addition of the
water/methanol reagent until a ‘null’ (see note) is obtained on the galvanometer. Disregard the
volumes of reagents used up to this point.

Now run in 10.0 mL accurately measured) of the Fiescher reagent and titrate to the ‘null’ point with
the water/methanol reagent. Repeat until successive titration do not differ by more than 0.10 mL.
Calculate the strength of the water/methanol reagent in terms of the Fischer reagent thus:-

1 mL water/methanol reagent = V1 ml Fischer reagent.

NOTE: Here the operation of the galvanometer is described as for the series circuit (Fig.8). When
the shunt circuit (Fig.9) is employed a positive reading will be obtained whenever a ‘null’
point is quoted. The ‘null’ point is taken as a constant positive reading of about 2 mm of the
scale, since at the actual zero point of the galvanometer scale an excess of water/methanol
reagent may be present.

E.4.2 Standardization of the Fischer Reagent — Prepare a standard solution of water in methanol using
the following procedure. Dry thoroughly in an oven two 100 mL one-mark volumetric flasks. While
they are still hot, close them with dry vaccine caps fitted with two hypodermic needles and allow to
cool, while passing slow stream of dry nitrogen through them. When cool, fill one of the flask (C1)
with the methanol through one of the hypodermic needles, allowing the displaced nitrogen to escape
through the other hypodermic needle fitted with a guard tube. Using a similar procedure partially fill
the other distilled water, accurately weighed (Mg), from the weighing pipette and fill up to the mark
with the methanol. Withdraw the hypodermic needles and shake the methanol/water mixture
thoroughly.

Run out from the reaction vessel most of the titrated solution remaining from the titration, leaving
sufficient to cover the drain tube, and by means of the pipette (previously dried and stored in a
desicator) transfer to the reaction vessel 10 ml of the methanol from flask C1. Start the stirrer and
run in the Fischer reagent until a decided brown colour persists. Note accurately the volume of
Fischer reagent (T2mL). Close the electrical circuit and titrate to the ‘null’ point with the
water/methanol reagent. Note the volume added (T3mL).

Perform a similar titration on 10 mL of the standard solution of water in methanol from flask C2,
noting accurately the volume of Fischer reagent added (T1mL) and the volume of water/methanol
reagent required (T4mL).

Calculate the water equivalent (F) of the Fischer reagent as follows:

100 M
F= mg water/mL.
T1 - T2 + V1 (T3 - T4 )

Where,

M = mass, in grammes, of water added in preparing the 100 mL of standard solution of water in
methanol,
22
©KEBS DKS 1180: 2012

T1 = volume in millilitres of Fischer reagent used in titration of the standard solution of water in
methanol,

T2 = Volume in millilitres of Fischer reagent used in titration of the methanol alone,

V1 = volume in millilitres of water/methanol reagent required to titrate 1 mL of water/methanol

reagent.

T3 = volume in millilitres of water/methanol reagent used in back-titration of the methanol alone,

T4 = volume in millilitres of water/methanol reagent used in back-titration of the standard

solution of water in methanol.

NOTE: The water content of the water/methanol reagent is F X M mg/mL. This value can be used
for the subsequent restandardization of the Fischer reagent, which deteriorates in storage.

E.4.3 Determination of water — Add to the reaction vessel by means of the pipette 5 mL of the methanol
and 15 mL of the pyride. Introduce the 1-ethylpiperidine into the reaction vessel. Run in the Fischer
reagent until a positive reading is obtained on the galvanometer and titrate to the ‘null’ point with the
water/methanol reagent. Disregard the volumes of Fischer and water/methanol reagents used up to
this stage.

Introduce into the reaction vessel 110 mL or 20 mL of the sample, (V2 mL) as appropriate, by means
of the pipette. Quickly run in a method excess (about 5 mL) of the Fischer reagent (A mL) as above
and as quickly as is consistent with accuracy again titrate to the ‘null’ point with water/methanol
reagent (B mL).

NOTE: The volumes of the Fischer and water/methanol reagents and calculate the water content of
the sample as follows:

(
F A - B.V1 )
Water = percent by mass
10 V2 .d

Where;

F = water equivalent of the Fischer reagent;

A = volume in milliliters of Fischer reagent added to the sample;

B = volume in milliliters of water/methanol reagent used in back-titration;

V1 = volume in milliliters of Fischer reagent required to titrate 1 mL of water/methanol reagent;

V2 = volume in milliliters of sample taken;

D = relative density of the sample at room temperature

NOTE 1: For the purpose of this calculation the figure obtained for the relative density of the sample
0 0 0
at 15.5 C, 20 C or 25 C may be used.

NOTE 2: When the sample is not soluble in methanol another suitable solvent should be used.
Examples of such solvents are pyridine, dioxan and mixtures of benzene and methanol.

APPENDIX F
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DKS 1180: 2012 ©KEBS

DETERMINATION OF ACIDITY
F.1 PRINCIPLE

A test portion is diluted with carbon dioxide-free water and titrate with standard volumetric sodium
hydroxide solution, using phenolphalein as indicator.

F.2 REAGENTS

F.2.1 General — During the analysis, use only reagents or recognized analytical grade, methylated spirits
*
complying with KS 03-591 and distilled water.

F.2.3 Sodium hydroxide — Standard volumetric solution c(NaOH) = 0.100 moL/L.

F.2.3 Phenolphthalein — 5 g/L ethanolic solution c(NaOH) = 0.100 moL/L.

Dissolve 0.5 g of phenolphthalein in 100 ml of 95 percent (V/V) ethanol or 95 percent (V/V industrial
methylated spirits and add the sodium hydroxide solution (F.2.2) until a pale pink coloration is
obtained.

F.3 APPARATUS

F.3.1 Ordinary laboratory apparatus

F.3.2 Conical flask — Of 500 mL capacity of borosilicate glass fitted with a ground glass stopper carrying
a guard tube containing sodium hydroxide on an inert support (soda lime).
*
F.3.3 Burette of 10 mL capacity — graduated in 0.02 mL divisions complying with Class A of BS 846 *.

F.4 Procedure

F.4.1 Test portion — Take 100 ± 1 mL of the sample, measured at 20 ºC.

F.4.2 Determination — Place 100 mL of water and a few clean anti-bumping granules in a conical flask
(F.3.2) and boil gently for 5 min to remove any carbon dioxide. Cool slightly and then add the test
portion (F.4.1). Boil the mixture gently for a further 5 min. At the end of the period, insert the stopper
and allow to cool to ambient temperature. Remove the stopper and add 0.5 ml of the
phenolphthalein solution (F.2.3) and titrate with the sodium hydroxide solution (F.2.2) and using the
burette (F.3.3) until a pink coloration persisting for 15 s is obtained. Stopper the flask and swirl its
contents after each addition of sodium hydroxide solution.

F.5 EXPRESSION OF RESULTS

The acidity A, expressed as a percentage by mass of acetic acid (CH3COOH), is given by the
equation:

A = 0.006 V1
p
where,

V1 is the volume of the sodium hydroxide solution used for the determination (in mL).

p is the density of the sample at 20 ºC (determined by the method described in Appendix B

(in g/mL)

*
Specification for Industrial Methylated Spirits.
*
Specification for Burettes.
24
©KEBS DKS 1180: 2012

0.006 is the mass of acetic acid corresponding to 1.00 mL of sodium hydroxide solution

c(NaOH) = 0.100 mol/L (in g).

APPENDIX G

DETERMINATION OF ALCOHOLIC IMPURITIES

G.1 PRINCIPLE

Any alcoholic impurities are acetylated by reaction with acetyl chloride. The amount of acetyl
chloride that has reacted is determined by titration with standard volumetric sodium hydroxide
solution, using 3.3 – bis (4-hydroxy-1naphyhyl_phthalide (1-naphtholphthalein) an indicator and the
alcohol equivalent is calculated.

G.2 REAGENTS

G.2.1 General — during the analysis, use only reagents of recognized analytical grade only methylated
*
spirits complying with KS 03-591

G.2.2 Pyridine — dry

G.2.3 Acetylating reagent — to 118 mL of acetyl chloride, and sufficient dry toluene to give a total volume
of 1000 mL.

G.2.4 Sodium hydroxide — standard volumetric solution, c(NaOH) = 1.00 mol/L.

G.2.5 3.3-bis (4-hydroxyl-1-naphthyl) phthalide indicator solution — 5 g/l ethanolic solution.

Dissolve o.5 g of 3,3-bis (4-hydroxyl-1-naphthyl) phthalide in 100 mL of 95 percent (V/V) ethanol or

95 percent (V/V) industrial methylated spirits.

G.3 APPARATUS

G.3.1 Ordinary laboratory apparatus

G.3.2 Two conical flasks — of 250 mL capacity fitted with ground glass stoppers.

G.3.3 Pipette — of 10 mL capacity complying with class B of BS 1583 fitted with an automatic suction
device.

G.3.4 Water bath — capable of being maintained at 60 ± 1 ºC

G.4 Procedure

G.4.1 Test portion — take 25 ± 0.1 ml of the sample, measure at 20 ºC.

G.4.2 Determination — Dry the two conical flasks (G.3.2) and place 10.0 ml of the acetylating reagent
(G.2.3) into each flask using the pipette (G.3.3). Add 2 ml of the pyridine (G.2.2) to each flask,
immediately insert the stopper tightly and mix the contents thoroughly without wetting the stoppers.

To one flask, add the test portion (F.4.1) ensuring that all of it comes into contact with acetylating
reagent. Replace the stopper and mix the contents thoroughly without wetting the stopper.

*
Specification for industrial methylated spirits.
25
DKS 1180: 2012 ©KEBS

Place both flasks in the water bath (F.3.4), maintained at 60± 1ºC, loosening the stoppers
momentarily to release any pressure and then replacing them tightly. Keep the flasks in the water
bath for 20 min, shaking them occasionally then remove the flasks and cool them to ambient
temperature.

Add 25 mL of water add 0.5 mL of the indicator solution (F.2.5) to each flask and then titrate the
contents of each flask in turn with the sodium hydroxide solution (F.2.4) until the appearance of a
faint blue colour.

G.5 EXPRESSION OF RESULTS

The alcohol content B expressed as a percentage by mass of butabol (C4H9OH), is given by the
equation:

0.296(V1 − V2 )
B=
p

Where,

V1 is the volume of the sodium hydroxide solution used for the titration of the blank
(in mL),

V2 is the volume of the sodium hydroxide solution used for the titration of the test solution (in
ml),

P is the density of the sample at 20 ºC (determined by the method described in Appendix B (in
mL).

APPENDIX H

DETERMINATION OF REFRACTIVE INDEX

H.1 APPARATUS

H.1.1 Abbe Type Universal Refractometer, used for the determination of the refractive indeces of liquid
solid bodies for light of a wavelength of 589.3nm. (D-line). The range of measurement of the
instrument extends from nb = 1.3 to 1.7. See figure 10.

H.2 PROCEDURE

Follow the instructions in the Manufacturer’s Manual for the determination of the refractive index

APPENDIX I
26
©KEBS DKS 1180: 2012

DETERMINATION OF FLASH POINT

I.1 TEST PORTION

The test portion is heated in a suitably designed closed cup in a suitable water bath. The ignition
trial is carried out after the test portion has been maintained under equilibrium conditions for at least
10 min at the selected equilibrium temperature. This procedure ensures that the air/vapour space
above the test portion has attained the saturation concentration of flammable vapour before the
ignition trial is performed. The test report records whether the test portion flashed or did not flash.

I.2 APPARATUS

I.2.1 Test Cup — A closed cup with an internal level indicator, the closed cups specified in a number of
national standards satisfy the necessary requirements. If a stirrer is fitted to the test cup used, it may
be operated during the ignition trial. If a stirrer originally fitted to the test cup is removed, the aperture
in the cover shall be securely plugged before starting the test.

FIG.1 — ABBE TYPE UNIVERSAL REFRECTOMETER

APPENDIX I
27
DKS 1180: 2012 ©KEBS

SUITABLE CLOSED CUPS SPECIFIED IN STANDARDS

The cups listed below of closed-cup apparatus described in standards are known to satisfy the
necessary requirements of method for carrying out the flash/no flash test. The method bath is not
included in the standard apparatus one must be provided (see 4.2).

Abel cup French Standard NF T 66-009

Abel cup French Standard NF M 07-011
Abel cup British Standard BS 3442(and IP 33 and IP 170)

Abel Pensky cup French Standard NF M 07-036

Abel Pensky cup German Standard DIN 51 755
Abel Pensky cup
(+ Stirrer) Swedish Standard SIS 02 18 11

Abel Pensky cup (modified

according to Bleisch) German Standard DIN 53 213. Teil 1

Pensky-Martens cup International Standard ISO 2719

Pensky-Martens cup British Standard BS 2839(and IP 34)

Pensky martens cup French Standard NF M 07-019
Pensky Martens cup German Standard DIN 51 758
Pensky Martens cup Netherlands Standard NEN-ISO 2719

Pensky Martens cup Swedish Standard SIS 02 18 12

Pensky Martens cup USA Standard Z 11.7 (and ASTM D 93)
Tag cup USA Standard Z 11.24 (and ASTM D 56)

Essentially the test cup shall be fitted with a tightly fitting cover which carries an opening slide and an
ignition device capable, when the slide is open, of inserting an ignition flame (diameter 3.5 ± 0.5
mm), when inserted, the nozzle of the ignition device shall be 1 ± 1 mm above the underside of the
cover. The equipment is such that an ignition trial can be performed by opening the slide, inserting
and removing the nozzle of the ignition device, and closing the slide again in a period of 25 ± 0.5 s.
A mechanically driven device for doing this is permitted. The source of flame in the ignition device
may be any suitable flammable gas.

I.2.2 Water — Bath-capable of being adjusted to the required temperature (I.4.1) and of adequate heat
capacity to meet the requirements of 1.4.3. A bath fitted with a stirrer and thermostat of suitable
range is convenient. (see figure 11).

I.2.3 Thermometers — The test cup shall be fitted with a thermometer of appropriate range and
dimensions, which when immersed in the test portion measures its temperature within a maximum
error of 0.5 ºC. A thermometer having a graduation at each 0.5 ºC is recommended.

The water-bath shall be fitted with a thermometer of equal precision. When required, the accuracy of
the thermometers shall be checked against a reference standard by an authorized laboratory using
the stipulated immersion.

I.2.4 Support — For holding the test cup in the water bath so that the cover and upper edge are
horizontal. The cup is immersed in direct contact with the water in such a position that the level of
the test portion in the cup is the same as that of the water in the water.

I.3 SAMPLING AND SAMPLE TREATMENT

I.3.1 Take a representative sample of the product to be tested using the appropriate sampling procedure
for the product concerned.

28
©KEBS DKS 1180: 2012

Fig. 2

The sample shall be kept in an air-tight container until it is to be tested. The ullge, i.e the air space above
the contents of the container, shall not be more than 10 per cent of the total capacity of the container.

NOTE: Samples should not be stored in plastics (polyethylene, polypropylene etc) bottles since volatile
material may diffuse through the walls of the bottle.

I.3.2 Because of the possibility of loss of volatile constituents, the sample container shall be cooled to at
least 10º below the selected equilibrium temperature before opening it to remove the test portion.
The sample shall receive only the minimum mixing treatment to ensure uniformity. After removal of
the test portion, the sample container shall immediately be tightly closed to ensure that loss of
volatile flammable components from the container is minimized. If this is not carried out, the product
sample shall be deemed unsuitable for further testing.

I.4 PROCEDURE

I.4.1 Preparation of apparatus

I.4.1.1 Adjust the temperature of the bath (I.2.2) to, and maintain it at, the selected equilibrium temperature
(subject to a tolerance of + 0.5 ºC).

I.4.1.2 The selected equilibrium temperature shall be corrected for variation from an atmosphere pressure
of 101.3 kPa (1 013 mbar or 760 mmHg), by raising the value for a higher pressure of lowering the
value for a lower pressure at the rate of 1 ºC for each 4 kPa (40 mbar or 30 mmHg) difference.

NOTE: Although this correction is only strictly valid within the atmospheric pressure range 98.0 to
104.7 kPa for pressures outside this range the error is sufficiently small to be ignored.

I.4.1.3 Carefully clean and dry the test cup (I.2.1) its cover and thermometer (I.2.3). Bring them to a
temperature at least 2 ºC below the selected equilibrium temperature.

I.4.2 TEST PORTION

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DKS 1180: 2012 ©KEBS

I.4.2.1 Obtain and prepare the test sample in accordance with clause I.3 and ensure that at all times during
this preparation its temperature is at least 10ºCbelow the selected equilibrium temperature.

I.4.2.2 Fill the test cup with the test sample until the internal level indicator just disappears under the
surface of the liquid. Take care to avoid the formation of bubbles and contact between the sample
and the cup wall above the level indicator. If either of these conditions occurs to a significant
extent, empty the cup, prepare it again according 1.4.3.1 and fill it with a fresh test portion.

I.4.3 Determination

I.4.3.1 Immediately after filling the test cup, place the cover and thermometer in position and support the
cup in the bath so that the cover is horizontal and the cup is immersed in direct contact with the
water, and with the surface of the test portion at the same level as the water in the bath.

I.4.3.2 Light the flame of the ignition device and adjust it to the size of a bead of diameter 3.5 ± 0.5 mm.

1.4.3.3 Allow the temperature of the test portion to rise within 0.5 ºC of the selected equilibrium temperature.
Maintain these conditions for 10 min or such longer time interval as is necessary, to permit the
temperature of the test portion to reach the selected equilibrium temperature. Then perform the
ignition trial by opening the slide, inserting and removing the nozzle of the ignition device, and
closing the slide again over a period of 2.3 ± 0.5 s. Watch for a flash between opening and closing
the slide.

1.4.3.4 Record whether a flash has occurred.

1.4.3.5 If flash was observed, maintain the test portion at the test temperature for 10 min and repeat the test.
If the second test results in a flash, the product shall be considered to have flashed at the selected
equilibrium temperature.

Note: 1. When the vapor mixture under test is near the flashpoint, application of the ignition
flame may give rise to a halo, however, the product is only deemed to have flashed
if a comparatively large blue flame appears and propagates itself over the surface of
the liquid. In case of doubt, the test shall be repeated with a fresh test portion and if
the doubt is unresolved by the second test, the product shall be regarded as having
flashed.

Note: 2. If a continuous luminous flame burns, in the orifice when the slide is opened and the
ignition flame is introduced, then the flashpoint lies considerably below the selected
equilibrium temperature.

APPENDIXJ

DETERMINATION OF EVAPORATION RATE – SHELL EVAPORATOR

J.1 APPARATUS

J.1.1 Evaporameter — Automatic Thin Film Evaporameter shown in figure 12.

J.1.2 Filter paper Disk — Fast, open-texture filter paper, 90 mm in diameter, with a circle approximately
60 mm in diameter (and concentric with the edge) Lightly drawn on the paper with a pencil.

J.1.3 Syringe — A1.00 mL hypodermic syringe, equiped with a 9 in (255 mm) needle of 0.050 in 1.3 mm)
outside diameter stainless steel tubing. Due to manufacturing variations, the syringe should be
calibrated before use.

J.1.4 Dehumidification Equipment — A suggested set up is given in a schematic diagram – Figure 13.

30
©KEBS DKS 1180: 2012

J.1.2 Strip Chart Recorder — Any strip chart recorder capable of recording the output signal (0 to 15 mA)
from the electronic optical weight-sensing device. The recorder should provide a range of chart
speeds including ¼ to 2 in (6.3 to 50 mm) min. It is also desirable for the recorder to accommodate
2 or more mA ranges in order to regulate the sensitivity of measurement.

J.2 Preparation of Evaporometer

J.2.1 Place the filter paper disk on the wire frame threading the hook through a small hole in the center of
the paper. Attach the wire frame to the support hook in the evaporometer.

FIG. 12 —

31
DKS 1180: 2012 ©KEBS

FIG.13 —

J.2.2 Close the evaporometer and cabinet doors and allow the temperature in both chambers and the
humidity to equilibrate at the following test conditions:

Cabinet and evaporation temperature: 77 ± ºF (25 ± 0.25 ºC)

Evaporometer humidity: 0 to 5 percent relative humidity.

Approximately 2 h are required for the humidity to drop to less than 5 percent.

J.2.3 Adjust the air flow to 21 L/min.

J.3 CONDITIONING OF SAMPLE

J.3.1 Bring the sample or a portion of it to an equilibrium temperature of 25 ± 0.5ºC in a constant

temperature bath.

J.4 PROCEDURE

J.4.1 When all components (including the filter paper in place) are at equilibrium, adjust the recording pen
to a prominent ‘zero’ position near the edge of the chart on the recorder, then turn the switch for the
chart motor to the OFF position. This constitutes the ‘zero’ load and time position for the test.

NOTE 1: The milliamphere range and chart speed should be selected if possible, so that the
dimensions of the weight and time axes of thebplotted curve are approximately the same
length.

J.4.2 Withdraw into the syringe 0.70 mL of the solvent which is at 77 ± 1.0ºF (25 ± 0.5ºC). Make certain
that all air bubbles are expelled from the syringe and the needle before application of the specimen
to the filter paper.

J.4.3 Open the small side on the right hand side of the insulating cabinet and insert the hypodermic needle
through the rubber porthole until the needle tip almost touches the disk and is just over the pencilled
line.

NOTE 2: Care must be exercised to avoid depressing the plunger of the syringe during this
operation. Otherwise the solvent will be accidentally and prematurely dispensed onto
the paper before the strip chart recorder is started.

J.4.4 When all is ready turn this strip chart motor switch to the ON position and simultaneously start
distribution of the specimen onto the filter paper. The complete specimen should be dispensed
uniformly in 10 ± 2s along the line. The recorder pen will ‘advance’ immediately to an ‘apex’ position
equivalent to the total weight of the specimen, less that portion that evaporated during the
application period. The pen will gradually return to its original position as the solvent evaporates and
the chart advances. The evaporation is complete when the recording pen has returned to its original
‘no load’ position.

NOTE 3: It is common for the final portion of the curve to exhibit a ‘tailing-off’. This is due to
artefacts of the methods such as

(i) hydrogen bonding of the last traces of solvent with the cellulose of fibres of the filter paper
and

(ii) a gradual diminution of the area of the filter paper wet by solvent (that is, in the final stage of
evaporation, drying of the paper progresses from the outer edge toward the centre of the
disk). Thus, it is common practice for the evaporation cycle to be considered ‘complete’
when the recording pen returns to 99.5 percent of the original displacement.

32
©KEBS DKS 1180: 2012

J.5 CALCULATION AND REPORTING

J.5.1 Determine the evaporation time in seconds at 10 weight percent increments to 90 percent for 95 to
100 percent from the evaporation curve as follows:

J.5.1.1 Divide the theoretical recording pen displacement for the total specimen into ten equal units along
the weight axis of the evaporation curve, then project the established 10 percent divisions to
corresponding intersecting points on the evaporation curve. The 0 percent evaporated or full load
point at zero time can be obtained either by ectrapolation of the evaporation curve back to zero
evaporation time or calculation using the weight of the sample and the calibration data for the
instruments (see annex). The routine calculation of the 0 percent evaporated, full load point is
recommended as a check for correct specimen size.

J.5.1.2 Multiply the distance along the time axis from the zero starting time by the chart speed factor in
seconds giving the total elapsed time for each defined point along the curve. For example, at a chart
speed of 1 in/min and a 20 percent evaporation point at 3.30 in the evaporation time is 198 s (60 x
3.30 = 198).
*
J.5.2 Report the relative evaporation rate by dividing 470 with the figure obtained in J.5.1.2.

Annex – Calibration of the Thin-film Evaporometer, Automatic Recording

The total deflection of the recording pen in chart units divided by the weight added corresponds to
the sensitivity of the apparatus.

For example, if the total pen deflection is 60 chart divisions for a 0.500 g weight, the sensitivity factor
is 120 chart divisions per gram. This value can then be used to establish the 100 percent specimen
load at ‘zero’ evaporation time and to calculate the percent evaporated at various time intervals. For
instance, pure n-butyl acetate (99 mol percent) has a density of 0.878 at 25 ºC, so a 070 mL
specimen at the cited calibration would deflect the pen 73.75-chart units (that is, 0.878 x 0.70 x 120
= 73.75. Each 10 per cent increment that evaporates corresponds to 73.75 chart divisions.

AMENDMENT SLIP NO. 1, PUBLISHED SEPTEMBER 2008

TO

KS 1180: 1994 Specification for ethyl methyl ketone (butanone for industrial use)

AMENDMENT
Clause 3
SL No 8

Delete the requirements of the refractive index at 20 ºC and substitute with the following:

*
470 is the evaporation rate in seconds for 90 per cent evaporation on n-Butyl.
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DKS 1180: 2012 ©KEBS

1.3788 – 1.3792

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