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भारतीय मानक IS 14355 : 2022

Indian Standard

रंग रोगन के लिए

जि़क डस्ट पिगमेंट — विशिष्टि
(  पहला पनु रीक्षण )

Zinc Dust
Pigment for Paints — Specification
( First Revision )

ICS 87.060.10

© BIS 2022

भारतीय मानक ब्रयू ो

B U R E A U O F I N D I A N S TA N D A R D S
मानक भवन, 9 बहादरु शाह ज़फर मार्ग, नई िदल्ली – 110002
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI-110002
         www.bis.gov.in  
www.standardsbis.in

January 2022  Price Group 6

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Raw Materials for Paints, Varnishes and Related Products Sectional Committee, CHD 21

FOREWORD
This Indian Standard (First Revision) was adopted by the Bureau of Indian Standards, after the draft finalized by
the Raw Materials for Paints, Varnishes and Related Products Sectional Committee had been approved by the
Chemical Division Council.
This standard was first published in 1996. Zinc dust is widely used by the paint industry to make zinc based
antirust pigments. In fact, the performance of this pigment depends largely on the quality of zinc dust used as raw
material. The need was, therefore, felt that Indian Standard on this subject should be formulated to reduce the
variation of quality of the raw material.
In this standard, some important criteria like the shape of dust particles which has an effect on the performance
properties of paint have been included.
Raw material for paint products may contain lead and other heavy and toxic metals either because of use as
catalyst or their compounds being essential adjunct of formulation in manufacturing of paints. Taking cognizance
of the fact that lead and toxic heavy metal exposure of human being, particularly children in residential premises
is injurious to health and having adverse impact on human health and safety, the Committee responsible for
formulation of this standard has felt the need to introduce restriction of lead and toxic heavy metal restriction in
all paint raw material product standards. Revision of this standard has been taken up with a view to incorporate the
maximum permissible limit of lead and heavy metal restriction clause in this standard. Therefore, in this revision,
lead restriction up to a maximum permissible limit of 90 ppm and toxic heavy metals restriction (cumulative
other than lead) as 0.1 percent maximum has been prescribed to avoid hazardous impact of lead and heavy metal
exposure and consequent adverse impact on environment and human health.
Further, majority of consumers are not aware of the consequences of lead and other heavy metal toxicity and its
long-term implications to human health. Therefore, in this revision, along with lead and heavy metal restriction, a
suitable cautionary notice has been included in the marking clause.
The composition of the technical committee responsible for formulation of this standard is given in Annex G.
For the purpose of deciding whether a particular requirement of this standard is complied with the final value,
observed or calculated, expressing the result of a test or analysis shall be rounded off in accordance with
IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )’. The number of significant places retained in the
rounded off value should be the same as that of the specified value in this standard.
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IS 14355 : 2022

Indian Standard
ZINC DUST PIGMENT
FOR PAINTS — SPECIFICATION
( First Revision )

1 SCOPE 4 REQUIREMENTS
This standard prescribes requirements and method of 4.1 Residue on Sieve
sampling and test for zinc dust pigment for paints.
The residue on sieve, when tested as per the method
2 REFERENCES prescribed in Annex A shall be maximum 0.5 percent
on 45-micron sieve.
The Indian Standards listed below contain provisions
which through reference in this text, constitute 4.2 Particle Shape
provision of this standard. At the time of publication, It shall be spherical and uniform when examined by
the editions indicated were valid. All standards are a microscope (× 400 magnification). Irregular and non
subject to revision, and parties to agreements based on spherical particles shall not be acceptable.
this standard are encouraged to investigate by dated
or undated the possibility of applying the most recent 4.3 The material shall comply with the requirements
editions of the standards. given in Table 1.
IS No. Title 4.4 Keeping Properties
The material shall also conform to all the requirements
33 : 1992 Methods of sampling and as mentioned in 4.4, 4.2 and Table 1 when tested after
test for inorganic pigments a period of 18 months from the date of manufacture.
and extenders for paints
4.5 Lead Restriction
(third revision)
The material shall be tested for restriction from lead in
266 : 1993 Sulphuric acid (third revision)
accordance with IS 101 (Part 8/Sec 5), or by Atomic
1303 : 1983 Glossary of terms relating to Absorption Spectrometer (AAS) or by ICP. When thus
paints (second revision) tested the material shall not contain lead or compounds
1070 : 1992 Reagent grade water of lead or mixtures of both, calculated as metallic lead
(third revision) exceeding 90 ppm (see Note).
4611 : 1991 Metallic zinc powder (zinc dust) NOTE — When no lead is used during production (lead free).
(second revision) 4.6 Toxic heavy Metal Restriction
101 (Part 8/Sec 5) Methods of sampling and Product shall not be manufactured using mercury
: 1993 test for paints, varnishes, and and mercury compounds, cadmium, chromium VI,
related products: Part 8 Tests arsenic, antimony and their oxides. The material shall
for pigments and other solids, not contain more than 0.1 percent by weight in total
Section 5 Lead restriction test of above toxic heavy metals in the form of natural
460 (Part 2) : Test sieves — Specification: Part impurities or impurities entailed by the production
2020 2 Perforated plate test sieves process which are contained in the raw material, when
(fourth revision) tested by the relevant Atomic Absorption Spectroscopic
methods or by ICP method.
3 TERMINOLOGY
For the purpose of this standard, definitions given under
IS 33 and IS 1303 shall apply.

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IS 14355 : 2022

Table 1 Requirements for Zinc Dust Pigments for Paints

( Clauses 4.3, 4.4 and 7.1 )
Sl No. Characteristic Requirement Method of Test, Ref to
Annex Cl No. in IS 4611
(1) (2) (3) (4) (5)
i) Total zinc (as Zn), Min, percent by mass 98.0 B –
ii) Metallic zinc, percent by mass, Min 96.0 – A-2
iii) Zinc oxide, percent by mass, Max 4.0 C –
iv) Lead, percent by mass, Max 0.2 – A-4
v) Cadmium, percent by mass, Max 0.1 – A-6
vi) Calcium as CaO, percent by mass, Max 0.7 D –
vii) Moisture and other volatile matter, percent by mass, Max 0.1 – A-9
viii) Iron, percent by mass, Max 0.04 – A-5
ix) Particle size distribution: E –
a) Median particle size, microns 6-10*
b) Specific surface area, m2/g 0.17
x) Specific gravity, at 30°C, Min 7.0 F –
* Value may be 2-5 microns if intended for shop primers

5 PACKING AND MARKING 5.2.2 BIS Certification Marking

The product(s) conforming to the requirements of
5.1 Packing
this standard may be certified as per the conformity
The material shall be packed in 25 kg mild steel drums assessment schemes under the provisions of the
with polyethylene bag inside. The material shall be Bureau of Indian Standards Act, 2016 and the Rules
protected against air and moisture by placing desiccant and Regulations framed thereunder, and the products
bags of silica gel at the opening end of the containing may be marked with the Standard Mark.
drum.
6 SAMPLING
5.2 Marking
5.2.1 The containers shall be marked with the following 6.1 Representative sample of the material shall be
information; drawn as prescribed under IS 33.
a) Name of the material; 6.2 Criteria for Conformity
b) Indication of the source of manufacture; A lot shall be declared as conforming if the
c) Mass of the material; characteristics tested on the composite sample satisfy
d) Batch No. or lot No. in code or otherwise; the requirements given in this specification.
e) Month and year of manufacture; 7 TEST METHODS
f) Lead content (Maximum);
g) Toxic heavy metals content; and 7.1 Tests shall be conducted as prescribed in Annexes A
to F and IS 4611 in accordance with the requirements of
h) Cautionary note as below:
4.1 and col 4 and 5 of Table 1.
1) Keep out of reach of children, or
2) This product may be harmful is swallowed or 7.2 Quality of Reagents
inhaled. Unless otherwise specified, pure chemicals and distilled
water (see IS 1070) shall be employed in tests.
NOTE — ‘Pure chemicals’ shall mean chemicals that do not
contain impurities which affect the results of analysis.

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IS 14355 : 2022

ANNEX A
( Clause 4.1 )
DETERMINATION OF RESIDUE ON SIEVE

A-1 APPARATUS camel-hair brush at the rate of two strokes per second
during two periods of 10 s each. Raise the sieve from
A-1.1 Sieve — 45 micron IS Sieve (see IS 460 Part 2). the dish after each 10 s period to let the liquid on the
sieve run through. Change the liquid in the dish after
A-2 PROCEDURE every two brushing periods. Continue this operation
until the water passing over the residue and through
A-2.1 Dry the sieve in an oven at 105 ± 2 °C, cool, and the sieve is clear and free from solid particles. When
then weigh. the washing appears to be complete, collect about
A-2.2 Weigh 10 g of the pigment to be tested to an 200 ml of the wash liquid, after passing over the residue
accuracy of 1 mg. Wet the sieve on both sides with and through the sieve, in a clean 400 ml beaker. Stir
alcohol and transfer the specimen of pigment of the the liquid vigorously, and set the beaker on a black
sieve and again wet with alcohol. surface. The washing is not considered complete until
such a test fails to show any particles collected about
A-2.3 Hold the sieve under a tap delivering about 300 the middle of the bottom of the beaker.
to 500 ml of water per minute. By slightly shaking the
sieve, the pigment will be rapidly carried through. A soft A-2.4 When the washing is complete wash the pigment
camel-hair brush may be used in aiding the operation. particles adhering to the brush back into the sieve and
After most of the finely divided portion of the pigment wipe off the water below the sieve. Add a few drops of
has passed through the sieve, place the sieve, in alcohol and then of ether to expedite drying. Dry the
200 mm porcelain dish containing 250 ml of water so sieves for 1 h at 105 °C, cool, and weigh. Calculate the
that the sieve is covered to a depth of about 12 mm. percent of coarse particles.
Brush the pigment remaining on the sieve with a soft

ANNEX B
[ Table 1, Item (i) ]
DETERMINATION OF TOTAL ZINC

B-0 GENERAL B-1.1.4 Diphenylamine Indicator — Dissolve 1 g of

diphenylamine in 100 ml of concentrated sulphuric
Two methods are prescribed. In Method 1 total zinc
acid. It shall be freshly prepared.
content in the sample is determined volumetrically
using potassium ferrocyanide solution. Method 2 is the B-1.1.5 Standard Potassium Ferrocyanide
alternate method and uses EDTA method. Solution — Dissolve 21.12 g of potassium ferrocyanide
and 0.3 g of potassium ferricyanide in one litre of water
B-1 METHOD 1 and standardize as described in B-1.1.5.1.
B-1.0 Outline of the Method B-1.1.5.1 Standardization of Potassium Ferrocyanide
Total zinc content in the sample is determined Solution — Weigh accurately 4 to 5 g of pure zinc in
volumetrically using potassium ferrocyanide solution. a beaker, add 60 ml of dilute hydrochloric acid and
heat carefully till it dissolves completely. To facilitate
B-1.1 Reagents dissolution about 0.02 g of iron fillings free from zinc
may also be added. After all the zinc has dissolved, cool,
B-1.1.1 Concentrated Sulphuric Acid — Conforming dilute and make up to one litre. Pipette out 20 ml of
to IS 266. made up zinc solution into a 500 ml conical flask, dilute
B-1.1.2 Ammonium Hydroxide — 20 percent (m/v). to 100 ml with water and neutralize with ammonium
hydroxide, added carefully till a white precipitate
B-1.1.3 Dilute Hydrochloric Acid — Approximately appears. Add dilute hydrochloric acid drop by drop till
6 N. the precipitate just dissolves and add 5 ml dilute acid in
excess. Warm to 60 °C, add 3 drops of diphenylamine

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IS 14355 : 2022

indicator and titrate against potassium ferrocyanide approximately 300 ml of water. Dissolve 28 g of sodium
solution. A precipitate is formed with deepening in hydroxide in approximately 300 ml of water. Combine
colour as the end point approaches, the end point being the two solutions, cool and dilute to 1 litre with water.
the sudden colour change with the addition of one drop
from blue violet to a pale green colour persisting even B-2.1.7 Ethylene diamine tetracetic acid (EDTA),
after thorough shaking. Repeat the titration to obtain disodium salt, dehydrate, solution, zinc factor T, in g
constant values. Calculate the mass of zinc equivalent Zn/ml (that is 1 ml of disodium EDTA solution) will
to 1 ml of potassium ferrocyanide solution. form a complex with T g of zinc.
Dissolve about 20 g of disodium EDTA, dehydrate,
B-1.2 Procedure in water and make up to 1 litre with water. Store in a
Weigh about 2.5 g of the material accurately into a polyethylene bottle.
beaker, moisten with alcohol and dissolve in 40 ml Standardize against a 0.05 M zinc sulphate solution.
of dilute hydrochloric acid by heating. Cool, filter, if
necessary, and make up to 500 ml. B-2.1.8 Xylenol Orange
B-1.2.1 Pipette 20 ml of the made up solution into a 0.1 g indicator (sodium salt) in 100 ml of water.
250 ml beaker, dilute to 50 ml and pass hydrogen B-2.1.9 Bromothymol Blue
sulphide for about 5 min. Keep for 10 min. Heat to
80 °C. Filter and collect the filtrate in a 500 ml conical 0.1 g in 100 ml of 96 percent ethanol (v/v).
flask. Boil the filtrate till free from hydrogen sulphide. B-2.2 Procedure
Just neutralize with ammonium hydroxide, make acidic
with dilute hydrochloric acid, warm to 60 °C and titrate Weigh to the nearest 0.001 g, about 1.5 g of the sample
against the standard potassium ferrocyanide solution into a 250-ml beaker. Dissolve the sample in 20 ml of
exactly as was done for the standardization of the the hydrochloric acid (B-2.1.1) and add 1 or 2 ml of the
ferrocyanide solution. nitric acid (B-2.1.4) to ensure that any lead present is
dissolved. Add 5 ml of the sulphuric acid (B-2.1.3) and
B-1.3 Calculation evaporate until strongly, fuming. Cool, then add 100 ml
2 500VF of water, boil for a short time and allow to stand until
Total zinc (as Zn), percent by mass = the following day.
M
Filter the solution through a sintered glass or silica
where crucible; wash the crucible, collecting the filtration in
V = volume in ml, of standard potassium a 500 ml one-mark volumetric flask. Make the solution
ferrocyanide solution used in the titration; up to the mark and mix thoroughly.
F= mass in g, of the zinc equivalent to one ml of By means of a pipette, transfer 50 ml of the solution to
standard potassium ferrocyanide solution; and a 500 ml conical flask; add 200 ml of water and 3 drops
M = mass in g, of the material taken for the test. of the bromothymol blue indicator (B-2.1.9), then
add ammonia solution (B-2.1.5) drop by drop, until
B-2 METHOD 2 the colour turns blue. Then add the hydrochloric acid
(B-2.1.2) until the red colour changes to pale yellow.
B-2.1 Reagents After that add 20 ml of the buffer solution (B-2.1.6) and
3 drops xylenol orange indicator (B-2.1.8) and titrate
B-2.1.1 Concentrated Hydrochloric Acid — Density with the disodium EDTA solution (B-2.1.7) until the
1.18 g/ml. red colour changes to pale yellow.
B-2.1.2 Dilute Hydrochloric Acid — Dilute 200 ml of B-2.3 Calculations
the hydrochloric acid (B 2.1.1) to 1 litre, with water.
1 000VT
B-2.1.3 Sulphuric Acid — Density 1.84 g/ml. Total zinc (as Zn), percent by mass =
m
Slowly add 1 part by volume of sulphuric acid (density where
1.84 g/ml) to 1 part by volume of water.
m = mass in grams, of the test portion;
B-2.1.4 Nitric Acid — Density 1.42 g/ml. T = zinc factor in grams, per millilitre, of the
disodium EDTA solution; and
B-2.1.5 Ammonia Solution — Density 0.880 g/ml.
V = volume in millilitres, of the disodium EDTA
B-2.1.6 Buffer Solution — Dissolve 200 g of solution used.
hydroxylammonium chloride (NH2OH.HCl) in

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IS 14355 : 2022

ANNEX C
[ Table 1, Sl. No. (iii) ]
DETERMINATION OE ZINC OXIDE

C-1 REAGENTS C-5 PROCEDURE

C-1.1 Ferric Chloride Solution Weigh 0.2 g of the sample, transfer immediately to a
dry, 600-ml heavy-wall Erlenmeyer flask, and add
Prepare a solution containing 20 g of ferric chloride 50 ml of the FeCl3 solution. Tightly stopper the flask
(FcCl3.6H2O) and 20 ml of 20 percent sodium acetate and agitate constantly for approximately 15 min. As
(NaC2H3O2) solution per 100 ml. It is advisable to soon as the zinc dust is all dissolved, add 50 ml of the
make up only one day’s supply at a time (50 ml are Zimmerman-Reinhardt solution and 250 ml of water.
required for each determination).
Titrate with 0.1 N KMnO4 solution.
C-2 POTASSIUM PERMANGANATE (KMNO4) NOTE — If preferred, the reduced iron may be titrated
STANDARD SOLUTION (0.1N, 1ml = 0.008 with 0.1 N potassium di-chromate (K2Cr2O7) solution, using
gTiO2) solution diphenylamine sulphonate in the presence of H3PO4
as an internal indicator.
Dissolve 3.16 g of KMnO4 in water and dilute to
1 litre. Let it stand for 8 to 14 days, siphon off the clear C-6 BLANK
solution (or filter through a medium porosity fritted Make a blank determination, following the same
disk), and standardize against standard sodium oxalate procedure and using the same amounts of all reagents
(Na2C2O4) as follows: prior to the titration. (The blank is usually 0.1 to 0.2 ml
In a 400-ml beaker dissolve 0.250 0 to 0.300 0 g of of 0.1 N KMnO4 solution.)
the Standard sodium oxalate in 250 ml of hot water
(80 to 90 °C) and add 15 ml of H2SO4 (1 : 1). Titrate C-7 CALCULATION
at once with the KMnO4 solution, stirring the liquid Calculate the percent of metallic zinc as follows:
vigorously and continuously. The KMnO4 must not be
added more rapidly than 10 to 15 ml/min, and the last Metallic Zinc,percent
0.5 to 1 ml must be added drop wise with particular = [(V3 – B3) (N × 0.0327)/S2] ×100
care to allow each drop to be fully decolorized before where
the next is introduced. The solution shall not be below V3 = as millilitres of KMnO4 solution required for
60°C by the time the end point has been reached. (More titration of the specimen,;
rapid cooling may be prevented by allowing the beaker
to stand on a small hot plate during the titration. The use B3 = millilitres of KMnO4 solution required for
of a small non-mercury type thermometer as a stirring titration of the blank;
rod is most convenient.) Keep the KMnO4 solution in N = normality of the KMnO4 solution;
a glass-stoppered bottle painted black to keep out light, S2 = grams of sample used; and
or in a brown glass bottle stored in a dark place. 0.0327 = milli equivalent weight of Zn.
C-3 SODIUM ACETATE SOLUTION (200 g/l) C-8 CALCULATION
Dissolve 200 g of sodium acetate (NaC2H3O2) or 332 g Calculate the percent of ZnO as follows:
of NaC2H3O2.H2O, in water and dilute to 1 litre.
ZnO, percent = (A-C) × 1.244 7
C-4 ZIMMERMAN-REINHARDT SOLUTION where
Prepare a solution containing 67 g of manganese A = percent of total zinc, and
sulphate (MnSO4.4H2O), 130 ml of sulphuric acid C = percent of metallic zinc.
(H2SO4) (sp gr 1.84), and 138 ml of phosphoric acid
(H3PO4) (85 percent) per litre.

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IS 14355 : 2022

ANNEX D
[ Table 1, Sl No. (vi) ]
DETERMINATION OF CALCIUM

D-1 REAGENTS Catch in a clean 400 ml beaker, dilute (if necessary) to

a volume of about 250 ml, and add 25 ml of saturated
D-1.1 Ammonium Oxalate, Saturated Solution ammonium oxalate solution. Bring to a boil, and add
Mix 50 g of ammonium oxalate and 1 litre of water. NH4OH in slight excess. Boil until the precipitate
becomes crystalline and dense. Let it stand for 1 h on a
D-1.2 Ammonium Oxalate Solution (10 g/l) steam bath. Allow to cool. Filter and wash with small
Dissolve 10 g of ammonium oxalate in water and dilute amounts of hot water until all ammonium oxalate is
to 1 litre. removed.

D-1.3 Potassium Permanganate, Standard Solution D-2.3 Remove the paper from the funnel and spread it
(0.1 N) — See C-2 out on the inside of a 600 ml beaker above 300 ml of
warm water to which has been added 20 ml of H2SO4
D-2 PROCEDURE (1 : 1). Rinse the precipitate off the paper with water
from a wash bottle and warm the solution to 80 °C.
D-2.1 Transfer 10 g of the sample, weighed accurately Titrate at this temperature with KMnO4 solution. As
to 0.1 g, to a 400 ml beaker. Dissolve in 30 ml of soon as a persistent pink end point is obtained, drop the
HC1 (1 : 1), keeping the beaker covered. Dilute to paper into the liquid, rinse the side of the beaker, and
200 ml. The solution at this point should be clear and quickly complete the titration.
transparent. Neutralize with NH4OH. (Some zinc,
because of its high concentration, will precipitate out as D-2.4 Calculation
hydroxide at this point.) Add NH4OH (sp gr 0.90) drop Calculate the percent of calcium as CaO, as follows:
wise, stirring until the solution becomes clear. Heat (CaO,percent = [(V4 N 0.02804)/(S3] × 100)
nearly to boiling and add 75 ml of saturated ammonium
oxalate solution. Boil until the precipitate assumes a where
dense crystalline appearance. Allow to settle on a steam V4 = millilitres of KMnO4 solution required for
bath for 20 min and then cool. Filter on close-grained titration of the sample;
paper and wash five times with a cold ammonium N = normality of the KMnO4 solution required for
oxalate solution (10 g/l). titration of the sample; and
D-2.2 Carefully dissolve the precipitate from the filter S3 = grams of specimen used.
paper, using alternately hot HC1 (1:3) and hot water.

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IS 14355 : 2022

ANNEX E
[ Table 1, Sl No. (ix) ]
DETERMINATION OF PARTICLE SIZE DISTRIBUTION

E-0 PRINCIPLE cut sections being turned upwards at an angle of 30° to the
horizontal.
The rate of fall of spherical particles through a medium
in which they are dispersed is proportional to the square
of the particle diameter (Stokes’ law). The Andreasen
method for determination of particle size distribution
makes use of this relationship and expresses the
particle size distribution in terms of distribution of
spherical particles of the same settlement rate. In the
determination, a dilute suspension is prepared and the
concentration of solids at a fixed point below the surface
is determined at a series of time intervals calculated to
correspond to certain equivalent spherical diameters.

E-1 APPARATUS

E-1.1 Sedimentation Vessel, Glass

About 56 mm internal diameter and having a graduated
scale from 0 to 200 mm marked on its side. The zero
graduation line shall be not less than 25 mm from the
inside base of the vessel, and the capacity of the vessel
up to the 200 mm line shall be about 550 to 620 ml
(Fig. 1).
E-1.2 Pipette
Fitted with a two-way tap and side discharge tube.
The capacity of the pipette to the graduation line is
conveniently 10 ml. A bell-shaped dome with a ground
glass joint to fit the neck of the sedimentation vessel
is fused to the pipette. A small vent hole is made in
this dome. The inlet to the pipette stem must be level
with the zero line on the sedimentation vessel. The
stem from the pipette bulb to the sampling inlet shall
be constructed of capillary glass tubing with a bore not
less than 1 mm and not more than 1.3 mm. The tube
above the bulb shall be 4-4.5 mm bore.
E-1.3 Transparent-Sided Constant-Temperature
Bath
It shall be of at least 15 litre capacity, maintained at a
temperature of 23 ± 0.5 °C into which the sedimentation
vessel can be immersed up to the 200 mm graduation
line. The bath shall be positioned away from sources Fig. 1 Sedimentation Vessel
of vibration and the circulating system shall not cause For Particle Size Distribution
vibration.
E-1.5 Dispersion Vessel
E-1.4 Mechanical Stirrer
Shall be of appropriate dimensions, such as a 1 000 ml
Capable of rotating at a suitable speed for complete gas jar.
dispersion (1 000 ± 100 rpm is generally suitable). The
stirrer shall be designed to lift the dispersion and to E-1.6 Balance
avoid the creation of a vortex. Having sensitivity of not less than 0.1 mg.
NOTE — A suitable stirrer may be made from an approximately
40 mm diameter brass disk with four equally spaced cuts, the E-1.7 Water Bath

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E-1.8 Wide-Mouth Weighing Bottles 20 microns (see E-3.3) and thereafter in progression so
Suitable for evaporation, of capacity not less than that the limiting diameters stand in a 2 : 1 progression.
20 ml, or a small laboratory centrifuge and centrifuge Alternatively, the samples may be taken at convenient
tubes preferably of 20 ml capacity but of not less than times approximately in a 2:1 progression and the exact
10 ml capacity. spherical particle diameters corresponding to each
sample calculated. The time to fill the pipette shall be
E-1.9 Stop-Watch or Stop-clock about 20 s. Discharge the suspension from the pipette
into a tared weighing bottle. When the bulb has drained,
E-2 CALIBRATION OF APPARATUS remove the rubber suction tube and run 5 to 7 ml of
ethanol from an ordinary 10 ml pipette into the bulb
E-2.1 Pipette of the sedimentation pipette to wash into the weighing
Thoroughly clean the pipette. Partly fill the bottle any particles adhering to the surface. The stem
sedimentation vessel with distilled water. Set the tap in of the sedimentation pipette shall remain filled with
the sampling position and, by means of a rubber tube, suspension. Dry the contents of the weighing bottle on
suck water into the bulb to the level of the graduation water bath until the difference between the successive
line. Reverse the tap to the discharge position and weighings is not greater than 0.1 mg. Calculate the mass
allow the water to drain into a tared weighing bottle. of the fraction, mn, allowing for the mass of dispersing
Apply pressure through the rubber tube to blow any agent, which shall be determined by carrying out a
water remaining in the bulb and the discharge tube into blank test. The determination of the different fractions
the weighing bottle. Weigh the bottle to the nearest may be carried out by means of chemical methods if
0.001 g and calculate from this mass the internal this procedure is more suitable.
volume Vp of the pipette. The depth of immersion of the pipette decreases as each
fraction is withdrawn. Determine the exact decrease in
E-2.2 Sedimentation Vessel
depth by experiment and allow for it in the subsequent
Thoroughly clean the sedimentation vessel, and weigh calculations. Suppose that the decrease is 4 mm for
it, with the pipette in place, to the nearest 0.1 g. Then each fraction withdrawn, and that depth after the first
fill it to the 200 mm line with water at 23 ± 0.5 °C and fraction has been withdrawn will be 196 mm, and
reweigh. Calculate from the mass of water the internal the mean depth h1 used for calculation of the initial
volume Vs of the vessel. diameter corresponding to the first fraction will be
198 mm. The mean depth h2 for the second fraction
E-3 PROCEDURE will be 194 mm, and accordingly up to n th number of
withdrawals.
E-3.1 Test Sample
Using 5 g of zinc dust sample prepare a dispersion by E-3.3 Calculation of Withdrawal Time
placing the test portion in the dispersion vessel adding The withdrawal time, tn, in seconds for the nth sample
ethanol at 23 ± 0.5 °C to give a total volume of about is given by the equation:
500 ml and stirring with the mechanical stirrer for
15 min. Immediately pour all the suspension into the 18hn .
tn   106
sedimentation vessel and make up to the 200 mm line  S1  S2  .ɡ.(d n )2
with ethanol. Transfer the sedimentation vessel to the
constant temperature bath. where
η = the absolute viscosity, in newton seconds per
E-3.2 Allow the sedimentation vessel to stand immersed square metre of the medium;
to the 200 mm line until it has reached the temperature
of the bath. Record this temperature, which shall not hn = the mean depth in millimetres, at which the nth
differ greatly from that of the room. When temperature sample extraction is made;
equilibrium has been attained, mix the contents S1 = the density, in megagrams per cubic metre (or
thoroughly by placing a finger over the vent hole and grams per cubic centimetre), of the medium;
inverting the vessel several times. Immediately after S2 = the density, in megagrams per cubic metre (or
mixing, replace the vessel and start the stop-clock or grams per cubic centimetre), of the particle;
stop-watch. ɡ = the acceleration due to gravity, in metres per
Withdraw from the suspension by means of the second squared; and
pipette a series of samples of volume Vp at depths dn = the limiting stokes diameter, in micrometres,
ho at increasing time intervals after mixing, starting corresponding to the nth sample extraction.
at time t1 corresponding to a particle size of about

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E-3.4 Calculation of Cumulative Percentage where

Undersize mn = the mass, in grams, of the fraction corrected
The cumulative percentage by mass, Pn of particles for the mass of the dispersing agent;
smaller than each of the limiting stokes diameters dn m2 = the mass, in grams, of the test portion;
for each time interval t n is given by the formula:
Vp = the volume, in ml, of the pipette; and
mn × V3 V3 = the volume, in ml, of the sedimentation vessel.
× 100
m2 × V p

ANNEX F
[ Table 1, Sl No.(x) ]
DETERMINATION OF RELATIVE DENSITY

F-0 PRINCIPLE bottle. Shake thoroughly with the stopper and place till
all the sample is thoroughly wetted. Wait for 15 min or
The method described here applies to solids only and
until such time when all the air bubbles are eliminated.
consists in finding out the mass of water occupying
Add more of water containing 0.5 percent of wetting
the same volume as a known mass of the sample. Then
agent to make up to the mark and weigh (W3). Pour
the relative density of the sample under test is the ratio
out the contents of the bottle and wash thoroughly with
of mass of the sample to mass of water occupying the
water. Finally fill up the bottle to the mark with distilled
same volume as the sample.
water and weigh (W4). Make a note of the temperature
F-1 PROCEDURE at which the determination is carried out.
NOTE — The density of water remains practically unchanged
Weigh accurately a clean and dry Regnault’s on addition of 0.5 percent of it own mass of wetting agent
specific gravity bottle/volumetric flask of 50 ml Hence this value does not significantly differ from the actual.
capacity (W1). Take about 5 g of the sample into the
bottle/flask and weigh again (W2). Add about 30-35 ml F-2 CALCULATION
water containing 0.5 percent of a suitable wetting W2  W1
agent (for example, calsolene oil HS), washing down Relative Density 
any portion of sample sticking to the inside wall of the W4  W3

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ANNEX G
( Foreword )
COMMITTEE COMPOSITION
Raw materials for Paints, Varnishes and Related Products Sectional Committee, CHD 21
,

Organization Representative(s)

In personal capacity (Retired from IIT Bombay) Prof A. S. Khanna (Chairman)

Office of Micro, Small and Medium Enterprises, Shri Sunil Kumar Newar
New Delhi Shri Santosh Kumar (Alternate)
Harcourt Butler Technical University, Kanpur Dr P. K. Kamani
Dr Arun Maithani (Alternate)
ICT, Mumbai Prof Sabnis
Prof Mahanwar (Alternate)
Indian Institute of Chem Technology, Hyderabad Dr Ramanuj Narayen
Dr Pratyay Basak (Alternate)
Institute of Minerals and Materials Technology Nominationa Awaited
University Institute of Chemical Technogy, Jalgaon Prof Ravindra Puri
Shriram Institute of Industrial Research Shri A. K. Majumdar
Central Electro Chemical Research Institute, C. Arunchandran
Karaikudi D. Sherwood (Alternate)
National Test House, Ghaziabad Nomination Awaited
Naval Materials Research Laboratory Nomination Awaited
Birla White Dr R. K. Singh
Shri Om Prakash Gautam (Alternate)
Asian Paints Ltd, Mumbai Mr Rajeev Kumar Goel
Dr Subrahmanya Shreepathi (Alternate)
Atul Limited Dr Mahesh Soni
Dr Jayesh Joshi Updated Nominees (Alternate)
Berger Paints India Limited, Kolkata Shri T. K. Dhar
Shri Swagata Chakraborty (Alternate)
Clariant Chemicals (India) Ltd, New Delhi Shri Nitin Vaidya
Shri Umesh Kapoor (Alternate)
Heubach India, Mumbai Shri J. I. Sevak
Hindustan Zinc Limited, Delhi Shrimati Payal Chauhan
Indian Chemical Council Nomination Awaited
Indian lead zinc development association, New Delhi Shri K. Sridhar
Indian Small Scale Paint Association Shri Mukund Hulyalkar
Shri Mukesh Goyal (Alternate)
J J Chemicals Nomination Awaited
Kansai Nerolac Paints Ltd, Mumbai Shri Laxman Nikam
Shri Manoj Kumar Somani (Alternate)
Shalimar Paints Limited Shri Gokul C. Sutradhar
Shri Chinmaya Nayak (Alternate)

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Organization Representative(s)

SSPC India Chapter Dr Buddhadeb Duari

Subhajit Bhattacharya Kaushik Duari
Young Professionals
20 Microns Limited, Mumbai Dr Anil Bansal
Rubamin Limited Nomination Awaited
Vapi Oxide Colours Pvt Ltd (VOXCO), Vapi Shri Ishan Raveshia
Shrimati Minal Mayekar (Alternate)
Consumer Voice Shri M. A. U. Khan
Shri B. K. Mukhopadhaya (Alternate)
BIS Director General Ajay K. Lal, Scientist ‘E’ and Head (CHD)
[ Representing Director General ( Ex-officio ) ]

Member Secretary
Pushpendra Kumar
Scientist ‘B’ (CHD), BIS

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Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 2016 to promote harmonious
development of the activities of standardization, marking and quality certification of goods and attending to
connected matters in the country.

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Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed
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should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of
‘BIS Catalogue’ and ‘Standards: Monthly Additions’.
This Indian Standard has been developed from Doc No.: CHD 21 (17010).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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