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IS 12478 (1988): Ammonium sulphate, technical [CHD 1:

Inorganic Chemicals]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 IS :12478 - 1988
( Reaffirmed 1999 )
Indian Standard
,-
I
\ s*
‘I
I
SPECIFICATIONFOR
AMMONIUM SULPHATE,TECHNICAL

UDC 661*522

r-x
’ ,
\_.’

@ Copyright 1989

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC
NEW DELHI 110002

Gr 3 May I989
 IS : 12478 - 1988

Indian Standard
SPECIFICATIONFOR
AMMONIUM SULPHATE,TECHNICAL

0. FORE WORD
0.1 This Indian Standard was adopted by the in yeast production from molasses and in the
Bureau of Indian Standards on 22 August 1988, manufacture of explosives and ammunition.
after the draft finalized by the Inorganic Chemi-
0.3 This standard, however, covers the require-
cals ( Miscellaneous ) Sectional Cqmmittee .hpd
ments for ammonium sulphate used as a water
beo;nc;pproved by the Chemical Divlslon
treatment chemical, in the treatment of hides
and skins and in the manufacture of explosives
and ammunition.
0.2 Apart from its use as nitrogenous fertilizer
( see IS : 8’16-1980* ), ammonium sulphate is also 0.4 For the purpose of deciding whether a parti-
used in the treatment of hides and skin for -,ular requirement of this standard is complied
leather production. In combination with phos- with, the final value, observed or calculated,
phate and borate, it is used for fire proofing expressing the result of a test or analysis, shall
timber, plastics and insulating materials. In be rounded off in accordance with IS : 2-1960*.
combination with chlorine, ammonium sulphate The number of significant places retained in
disinfects water. It is also used as a nutrient, the rounded off value should be the same as
---- that ofthe specified value in this standard.
*Specification for ammonium sulphate, fertilizer grade
( second rroision ). *Rules for rounding off numerical values ( revised I.

1. SCOPE 4.2 Marking - Each bag shall bear legibly

and indelibly the following information:
1.1 This standard prescribes the requirements
a) Name and type of the material;
2nd methods of sampling and test for ammo-
nium sulphate, technical. b) Name of the manufacturer and his recog-
nized trade-mark, if any:
2. TYPES
c) Percentage of assay by mass;
2.1 The material shall be of the following three d) Gross and net mass in kg; and
types; e) Batch number.
a) ‘Type 1 - for leather processing,
4.2.1 The container may also be marked with
b) Type 2 - for water treatment, and the Standard Mark.
cl =ypg 3 - for explosives and ammunition. NOTE-~~- ‘l‘he use of the Standard Mark is governed by
the provisions of the Bureau of Indian Standards Act
3. REQUIREMENTS 1986 and the Rules and Regulations made thereunder.
The Standard Mark on products covered by an Indian
3.1 Description - The material shall be in Standard conve) I the assurance that they have been pro-
duced to comply with the requirements of that standard
the form of free flowing crystal or powder and under a well-defined system of inspection, testing and
shall be free from extraneous material. quality control which is devised and supervised by BIS
and operated by the producer. Standard marked products
3.2 The material shall also comply with the are also continuouslv checked bv BIS for conformitv to
requirements given in Table 1 when tested that standard as a furthersafeguard. Details of conditions
according to methods given in Appendix A. under which a licence for the use of the Standard Mark
may be granted to manufacturers or producers may be
Reference to the relevant clauses of Appendix A obtained from the Bureau of Indian Standards.
is given in co1 6 of the table.
5. SAMPLING
4. PACKING AND MARKING
5.1 Representative test samples of the material
4.1 Packing - The material shall be packed in shall be drawn as presrribctl in TS : 60~12
jute or multi-walled paper bags or jute lined ( Part 1 )-1985*.
with polyethylene film or in such other containers .-.-__ ~~
as agreed to between the purchaser and the *Methods of sampling and te5t for fertilizers: ~‘a, t I
supplier. Each bag shall be securely closed. Sampling (first rmision).
 IS:12478 - 1988

TABLE I REQUIREMENTS FOR AMMONIUM SULPHATE, TECHNICAL

( Clauses 3.2 and 5.2 )

SL CHARACTERISTICS REQUIRE~~ENTB METHOD ow ‘Iw~

No. ,-_--_-___h--------~ KEBERENC~ To ’
‘be 1 Type 2 Type 3 CLAUSE No. OB
APP~XDIX A

(1) (2) (3) (4) (5) (6)

i) Assay, percent by mass, Min 96.7 98.0 99.0 A-3

ii) Moisture, percent by mass, Max 1.0 0.25 0.25 A-4

iii) Free acidity ( as HsSOa), per- 0.70 0’15 0’025 A-5

cent by mass, Max

iv) W;rs; z;;lubles, percent by To pass - 0.05 A-G

3 the test

v) Iron ( as Fe ), percent by mass, 0.20 - A-7

Max
vi) Et~k;sso~~~e matter, percent by - 0.03 - A-8
,
vii) Arsenic, percent by mass, Max 0.01 0.005 0.05 A-9
viii) Su$$ated ash, percent by mass, - - 0’40 A-10

ix) Total chlorides ( as NH&l ), - - 0.05 A-11

percent by mass, Max

x) Nz;;esJay NO, ), percent by - - Nil A-12

9

5.2 Criteria for Conformity - For declaring site sample shall satisfy all the requirements
the conformity of the lot to the requirements of specified in Table 1.
this specification, the test results on the compo-

APPENDIX A
( Clause 3.2 3
METHODS OF TEST FOR AMMONIUM SULPHATE, TECHNICAL

A-f. QUALITY OF REAGENTS Grind as rapidly as possible to avoid loss or gain

of moisture during operation. Mix thoroughly
A-l.1 Unless specified otherwise, pure chemicals and store in tightly stoppered bottles of sizes that
and distilled water ( see IS : 1070-1977* ) shall are almost completely filled by the ground
be used in tests. sample.
NOTE - ‘ Pure chemicals ’ shall mean chemicals that NOTE - For hygroscopic samples, it is preferable to
do not contain impurities which affect the result of use electric mixer.
analysis.
A-3. ASSAY
A-2, PREPARATION OF SAMPLE FOR
ANALYSIS A-3.1 Reagents

A-2.1 Procedure - Reduce the test sample to A-3.1.1 Formaldehyde Solution - Neutralize 57
a quantity sufficient for analysis and grind not percent formaldehyde solution with 025 K
less than 0’25.5 kg of reduced sample without sodium hydroxide to phenolphthalein end point.
previous sieving. For materials that form a Filter in case some precipitates have formed.
paste on putting pressure, grind in porcelain A-3.1.2 Phcnolphthalein Indicator - 0*5 percent
pestle and mortar ( see Note ) to pass through ( m,‘v ) solution in 50 percent ethyl alcohol.
I mm IS Sieve. For dry mixtures that tend to
segregate, grind in a porcelain pestle and mortar A-3.1.3 Standard Sodium [Link] Solution - 1N
( see Note ) to p ass through 355 microns IS Sieve. ( seeIS : 2316.1968* ).
__I__~ ~~
*Specification for water for geueral laboratory use *Methods of preparation of standard solutrons foI
( second revision). calorimetric and volumetric analysis (Jir~l rsuisivn ).

2
 IS : 12478 - 1988

A-3.2 Procedure - Dissolve about 2.5 g of the red is not obtained, methyl red-methylene blue
material in water and add a mixture of formalde- mixed indicator may be used. Use preferably
hyde solution and 25 ml of water. Allow to a microburette for this titration.
stand for 30 minutes and titrate against 1 N
NOTE - The filtering medium shall be neutral and
sodium hydroxide solution to the phenolphthalein shall not contain any alkaline material which would
end point. neutralize the free acid.

A-3.3 Calculation A-5.3 Calculation

Assay [ as ( NH4 )z SO4 1, percent by mass Free acidity ( as H2SO4 ), percent by mass
66 Vx Jvx 100 = 4904 v.N
=looox M M
where where
V = volume in ml of standard sodium v= volume in ml of standard sodium
hydroxide required for the titration, hydroxide solution,
N = normality of standard sodium hydro- jY= normality of standard sodium hydroxide
xide solution, and solution, and
M = mass in g of the material taken for the mass in g of prepared sample taken
test. for the test.

A-4. MOISTURE A-6. WATER INSOLUBLES

A-4.1 Procedure - Weigh to the nearest milli- A-6.1 Apparatus
gram about 2 g of the prepared sample in a
A-6.1.1. Gooch Crucible - G. No. 4.
weighed, clean, dry squat form weighing bottle.
Heat in an air oven for about 5 hours at 129 to A-6 1.2 Oven - maintained at 100 f 2°C.
131°C to constant mass. Cool in a desiccator
and weigh. A-6.1.3 Mujle Furnace - maintained at 800 f
25°C.
A-4.2 Calculation
A-6.2 Procedure
Moisture, percent by
E lOO(n/r,- M2) A-6.2.1 Take 5 g of the material in a 500 ml
mass
Ml - Ma beaker and dissolve in about 100 ml of water
where and stir thoroughly ( heat to boiling, if neces-
Ml -= massin g of the bottle with the sary ). Cover the beaker with a watch glass
material before drying, and allow it to stand for 4 hours at room tempe-
rature. Filter the residue in a weighed Gooch
MS = mass in g of the bottle with the crucible, Apply suction and wash the residue
material after drying, and Dry the crucible in an oven main-
with water.
MS = mass in g of the bottle. tained at 100 f 2°C till constant mass is obtain-
ed. Weigh the crucible with residue and find
A-5, FRBE ACIDITY out the total matter insoluble in water.

A-5.1 Reagents A-6.3 Calculation

A-5.1.1 Statldat d Sodiunz Hydroxide Solntio~~ - a) Water insolubles, percent by mass
0.02 N. (Ma- M1) x 100
A-5.1.2 Methyl Red Indicator -
Dissolve 0.2 g of M
methyl red indicator in 100 ml neutral rectified where
spirit. Ad 0 mass in g of the sample taken fbr the
A-5.1.3 Methyl Red - Methyletze Blue Mixed test,
Indicator Solution - Prepare by mixing equal AT, -1=mass in g of empty Gooch crucible,
volumes of 0.2 percent solution of methyl red and
and 0’1 percent solution in rectified spirit of Mz = mass in g of Gooch crucible and
methylene blue. water insolubles.
A-5.2 Procedure - Dissolve about 5 g of the
prepared sample, accurately weighed, in about A-7. IRON
50 ml of cold water. Filter ( see Note ), if neces- A-7.1 Reagents
sary, and make up the volume to about 200 ml.
‘Titrate with standard sodium hydroxide solu- A-7.1.1 Nitric Acid - See IS : 2ti4-1976*.
tion, using one or two drops of methyl red as
indicator. If satisfactory end point with methyl

3
IS : 1247819 1988

A-7.1.2 Hydrochloric Acid - See IS : 265 1987’. A-9.1.1 The material shall be considered to
be free from arsenic if no stain is produced on
A-7.1.3 Ammonia
the sensitized mercuric bromide paper.
A-7.1.4 Ammonium Chloride NOTE -Atomic absorption spectrophotometric
method may be adopted as an alternative method.
A-7.2 Procedure - Weigh accurately about
10 g of the material and dissolve in 10 ml nitric
acid and 100 ml of water by heating. Precipitate [Link] ASH
iron by adding ammonia till the colour of the
A-10.1 Reagents
solution turns deep blue, heat to boil and filter.
Wash with dilute solution of ammonia till the A-10.1.1 Concentrated Nitric Acid - See IS : 264.
washings are colourless. Dissolve the residue in 1976*.
10 ml of hydrochloric acid and 50 ml of water
taken in a beaker. Add 5 g of ammonium A-10.1.2 Concentrated Sulphuric Acid - See IS :
chloride and stir to dissolve Add 20 ml of 266-19777.
ammonia, boil, cool and filter. Wash the pre- A-10.2 Procedure - Heat the crucible with a
cipitate with water, dry the residue, ignite, and small bunsen flame muffle furnace for 15 minutes
weigh to constant mass. and cool it to room temperature in a desiccator
and weigh. Place about 5 g of the sample in
A-7.3 Calculation
the weighed crucible and weigh again. Heat
Ml x 70 the crucible steadily with a small bunsen flame.
Iron content, percent by mass = Burn off the residual carbon to a dull red hot
M2
and then allow it to cool at room temperature
where in open. Treat the ash with a few drops of
Ml = mass in g of the residue, and concentrated nitric acid followed by a few drops
of concentrated sulphuric acid and again heat
Me = mass in g of the material taken for
in fuming chamber until the acids have volatiliz-
the test.
ed and the whole of the carbon has burnt off.
NOTE - Atomic absorption spectrometric method Cool the crucible in desiccator and weigh again
may be used as an alternative method.
V42).

A-8. ETHER SOLUBLE MATTER A-10.3 Calculation

Sulphated ash, (MS--M) x 100

~-8.1 Reagent percent by mass = ~____-~
(Ml--M)
A-8.1.1 Ethyl Ether - anhydrous.
where
A-8.2 Procedure - Weigh accurately about
25 g of the sample after drying for 2 h at 100 rfi M = mass in g of the empty crucible,
2°C. Mix it with about 100 ml of ethyl ether Ml = mass in g of the crucible and sample,
in a beaker, Shake for about 30 minutes and and
filter. Take the filtrate in a tared porcelain Mz = mass in g of the crucible and ash.
dish, keep in an oven maintained at 100 f 2°C
and weigh to constant mass.
~-11. TOTAL CHLORIDES
A-8.3 Calculation A-11.1 Reagents
Ether soluble matter, percent by mass A-11.1.1 Sodium Carbonate - powder.
M1
=-x 100 A-11.1.2 Dilute Nitric Acid - 1 : 4.
M2
where A-11.1.3 Potassium Cfwomate Solutio?l -
Mr = mass in g of ether soluble residue, and saturated.

llrl2 = mass in g of the sample taken for test. A-11.1.4 Standard Silver Nitrate Solution - N/20.

A-11.2 Procedure - Take about 5 g of the

A-9. ARSENIC sample in a conical flask. Add to the flask, 100 ml
of fresh water Shake the solution and filter
A-9.1 Procedure - Dissolve 10.0 g of the through No. 40 Whatman filter paper. Wash
material in about 30 ml of water and carry out the residue twice using about 5 to 10 ml of
the test as prescribed in IS : 2088-1983t. waler. Transfer the solution to a porcelain dish

*Specification for hydrochloric acid ( third r&m i. “Specification for nitric acid ( .amrd r&ion ).
tMethods for determination of arsenic ( Jecond reoiridn ). +Specification for aulphuric acid ( second rcrisio,: ,

4
 13: 12478-1998

and make neutral to phenolphthalein either with N = normality of the standard silver nitrate
sodium carbonate ( NazCOs ) or with dilute solution used, and
nitric acid as appropriate. Add two drops of M ;=I mass of the sample taken.
saturated solution of potassium chromate ( free
from chloride 1. Titrate with N/20 standard A-12. NITRATR3
so&ion of silvei nitrate until a faint but standard
A-12.1 Apparatus
permanent reddish tingle appears which indi--
cates that all the chloride has combined with A-12.1.1 White Porcelain Tile - for spot test.
silver and the slight excess has formed a pre-
cipitate of silver chromate ( AgeCrOB ). A-12.1.2 Pointed Glass Rod

A-12.2 Reagent
11.2.1 Carry out blank using all the reagents
and apply the necessary correction. A-12.2.1 Diphenylamine - 1 percent solution in
concentrated sulphuric acid.
A-11.3 Calculation
A-12.3 Procedure - Dissolve 0.5 g of the
Total chlorides ( as NHdCI ), = 5.35 v jv sample in about 100 ml of water followed by
percent by mass 50 mg of sodium chloride. M’hen the latter has
M dissolved, add 0.2 ml of diphenylamine solution.
where To this, add without agitation 12 ml concentrat-
ed sulphuric acid. After a few minutes, mix
V -= volume in ml of standard silver nitrate gently and allow it to stand for 30 minutes. No
solution required for titration, blue colour should appear.
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