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IS 13475 (1992): Sodium Formate [PCD 9: Organic Chemicals


Alcohols and Allied Products and Dye Intermediates]

“!ा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”

Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
IS 13475 : 1992

( Reaffirmed 2004 )

lndian Standard
SODIUM FORMATE-SPECIFICATION

UDC 661*733*12

Q BIS 1992

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

September 1992 Price Group 4


.

Organic Chemicals ( Miscellaneous ) Sectional Committee, PCD 9

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the
Organic Chemicals ( Miscellaneous ) Sectional Committee had been approved by the Petroleum, Coal
and Related Products Division Council.
Sodium formate ( sodium salt of formic acid ) is used as a tanning agent in leather industry, in the
manufacture of various chemicals like formic acid, sodium hydrosulphite, various metal formates, in dyeing
and printing fabrics and also in analytical chemistry as a precipitant for the noble metals.
It is manufactured on industrial scale, generally by two routes :
a) by direct synthesis through reaction between sodium hydroxide and carbon monoxide; and
b) as a by product in the manufacture of pentaerythritol.
This standard contains clauses 4.3 and 5.1 which call for an agreement between the purchaser and the
supplier.
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 ;Lccordance
with IS 2 : 1960 <Rules for rounding bfl’ uumcrical values ( reui.red )‘. The number of significant places
retained in the rounded off value should be the same as that of the specified value in this standard.
IS 13475: 1992

Indian Standard
SODIUM FORMATE - SPECIFICATION
1 SCOPE Table 1 Requirements for Sodium Formate
( Clause 4.4 )
This standard prescribes the requirements,
methods of sampling and test for sodium Method of
Sl Characteristics Requirements
formate. No. rA_-h-- -7 Test ( Ref
Grade 1 Grade 2 to Annex )

/r REFERENCES (1) (2) (3) (4) (5)


i) Assay, percent by 95’0 85’0 A
The following Indian Standards are necessary mass, Min
adjuncts to this standard: ii) Organic impurities 4’0 - 1%
percent by mass,
IS Jvo. Title Max
iii) Volatile matter 43 4.0 C
1070 : 1992 Reagent grade water - Speci- percent by mass,
fication ( third revision ) Mox
iv) Heavy metals, 5’0 - D
4161 : 1967 Nessler cylinders ppm, Mah
v) Iron, ppm, A4uw 10.0 - E ’
4905 : 1968 Methods for random sampling vi) Matter insoluble Nil 0’50 F
in water, percent
by mass, Max
3 GRADES
vii) Sulphate content To pass - G
the test
The material shall be of following two grades:
viii) Chloride content To pass - H
the test
,Grade 1 - suitable for the manufacture of
chemicals, and
5.2 Marking
Grade 2 - for leather tanning and other The containers shall be legibly and indelibly
treatments. marked with the following:
a} Indication of the source of manufacture;
4 REQUIREMENTS
b) Name, grade and net mass of the material
4.1 The material shall be in the form of white in the container; and
granules or crystalline powder or aqueous solution c) Lot or batch number, in code or other-
with slight odour of formic acid. wise.
5.2.1 The containers may also be marked with
4.2 The material shall be soluble in water,
the Standard Mark.
glycerol and slightly soluble in alcohol.
6 SAMPLING
4.3 The granule/particle size shall be as agreed
The method of drawing representative samples
to between the purchaser and the supplier.
of the material and the criteria for conformity
4.4 The material shall also comply with the shall be as prescribed in Annex J.
requirements given in Table 1 when tested accord- 7 TEST METHODS
ine to the methods referred in co1 5 of the
T:ble 1. 7.1 Tests shall be conducted according to the
method of test referred in co1 5 of Table 1.

5 PACKING AND MARKING 7.2 Quality of Reagents


Unless specified, otherwise, pure chemicals and
5.1 Packing distilled water ( .wc IS 1070 : 1992 ) shall be used
in tests.
The material shall be packed in well-closed suit-
able containers as agreed to between the purchaser NOTE - ‘Pure chemicals shall mean chemicals that
do not contain impurities which affect thr result of
and the supplier. analysis.

1
IS 13475 : 1992

ANNEX A
[ Table 1, St Jvo. (i) J

ASSAY

A-l GENERAL A-3 METHOD B

Three methods, namely, Method A, Method B A-3.1 Reagents


and Method C have been prescribed. Method C
A-3.1.1 Potassium Bromate Solution - 0.1 N.
is given as a referee instrumental method, to be
employed in the case of dispute. Dissolve 2.8 g of potassium bromatc in distilled
water and make it up t0 1 OOO ml.
A-2 METHOD A
A.3.1.2 Sodium Acetate - :! K.
A-2.1 General
Dissolve 272 g oi sodium acetate trihydrate irr
This method is applicable to the material produ- distilled water and make it to 100 ml.
ced as a by product in pentaerythritol manufac-
ture. A-3.1.3 So&urn Thiosulphate
Dissolve 26 g of sodium thiosulphate in distilled
A-2.2 Reagents water and make it to 1 000 ml in a volumetric
flask.
A-2.2.1 Glacial Acetic Acid
A-3.1.4 Potassium Iodide Solution
A-2.2.2 Crystal Violet Indicator
Dissolve 20 g of potassium iodide in distilled
Dissolve 0.2 g of crystal violet powder in 1000 ml water and make it up to 100 ml.
of glacial acetic acid. A-3.1.5 Potassium Bromide Crytslalline

A-2.2.3 Perchloric Acid - 0.1 N. A-3.2 Preparation of Sample Solution ftom


Solid Sodium Formate
Mix 10.2 ml of 60 percent perchloric acid with
500 ml of glacial acetic acid contained in a 1 !OOO-ml Weigh accurately 1’7 g of the sample and transfer
volumetric flask, add to it 30 ml of pure acetic it to a 500-ml volunletric flask and dissolve it with
anhydride and shake the contents of the flask to some distilled water and make it up to 580-ml
ensure thorough mixing. Dilute to one litre with with distilled water. Shake it well and use this fc>r
glacial acetic acid and .shake it well, the determination.

A-3.3 Procedure
A-2.3 Procedure
Pipette out 15 ml of the sample from thr .“OO-nil
Weigh accurately about 0.1 to 0.15 g 0f‘ the mate- volumetric flask ( A-3.2 ) into a YJO-ml iodide
rial in a 25%ml flask which has been previously flask with glass stopper. Then pipette 30 ml ot
dried at 105°C for one hour and cooled in a desic- 0.1 N potassium bromate solution ( A-3.1.1 ) into
cator and immediately add 80 ml of glacial acetic the flask. Add 4 g of potassium bromide and
acid ( A-2.2.1 ) and swirl the contents 0f Bask 35 ml of distilled water. Make th:: tOta vcilume to
gently until the solids dissolve. Warm gently, if 8O ml and completely dissnlve potassium bromide.
necessary, but solution must be cooled off before Add 12 ml of 2 N sodium acetate and immedi;i-
titration. Add one drop of crystal violet indicator telv connect the tiask to a cooling tube wida ;I
( A-2.2.2 ) and titrate against O-1 N perchloride universal joint I’ the cooling tube should br
acid ( A-2.2.3 ) until colour changes from blue to of 1 meter ‘length kd 9 mrr: I. T> ). Add 5 ml 3-1t
bluish green. 20 percent HC1 from t!lr tq> of the cooling
tube and swir! the solution and place :he iodinlc
A-2.4 Calculation flask with tile c<4ng tube iu a constaxit tempera-
ture bath \vhic:h is kept at 60°C prior to placing
Assay, v x Jv x 6.8 the flask :~~ri allow it t0 : t-act at the same tea;-I-
percent by mass = perature ( ILI’C: ) fr)r onra hour ( during the
M
reaction, s\\--lcl
’ the fiask f0r two, three times Ito
where ensure thorough mixing for reaction ). After one
hour, remove the flask along with cooling tube
L’ = volume of perchloric acid consumed, from water bath and cool it to 15°C in an it:?
water bath. Introduce .< ml of putassiunr ,orlicl~
N = normality of perchloric acid, and
snlution ( A-3.1.4 ) through rhe cooiing t&c,
Jf = mass of the sample taken. f0llowed by 5 ml of 20 percent HU. \2’nslr tlte
IS 13475 : 1992

inside of the tube with approximately 10 ml of and the solution is titrated conductimetrically
water. After 15 minutes take out flask from ice with standard hydrochloric acid solution while
water and remove the cooling tube. Rinse the stirring and gradual change in conductance is
joint of the cooling tube with water and stopper measured using standardized conductivity cell.
the flask, place the flasks in dark for approxima- A graph is plotted against concentration versus
tely 15 minutes. Then titrate the content of the conductance and end point is measured where an
flask with 0.1 N sodium thiosulphate solution abrupt change in conductivity is noted.
( A-3.1.3 ) using starch as an indicator and
determine the end point and note this volume A-4.2 Reagents
( VI ). Carry out the blank test in a similar Standard hydrochloric acid - 0.1 N.
manner using all the reagents in the same order
and note the end point ( r-, ). A-4.3 Apparatus
A-3.4 Calculations A-4.3.1 Conductivity Meter

*s:;;; percent ‘lY= ( v, _ Jfl ) x fl x 0.003 4 A-4.3.2 Standard Couductivity Cell - with given
--
hf X 3 cell constant.
where A-4.4 Procedure
V, = volume in ml of btarldard sodium thio- W&ah accurately about 5 g of the material and
sulphate ( A-3.1.3 i used for titration transt’er it IO 100 ml flask and dissolve it by
of sample; adding distilled water and make up to the mark.
l’:! = volume in ml of standard sodium thio- Take 10 ml of sample from the flask and transfer
suiphate used for titration of blank; it to a X10-ml beaker. Add 90ml of distilled water
and ritrate the contents against 1 N HCX using
N = normality of standa:-d sodium thiosul-
magnetic stirrer and conductivity meter with
phate solution; and
standardized conductivity cell. Note down the
>II = mass of the sample taken, g. readings of titration and conductane, with gradual
A-4 METHOD C addition ( in 1 ml fraction ) OF hydrochloric acid
and tind out the end point as shown in Fig. 1
A-4.1 Outline of the Method which is the volume of hydrochloric acid uspd for
A known quantity of material is dissolved in water titrating sodium formate.

END POINT

G! 2 3 L S 6 7 8-9
UOLUME OF 5rAblGARO HYDROCHLORIC ACID ADDED
Fro. 1 CONDVCTIMETRIC TITRATION CURVES
3
.

IS 13475 I 1992

A-4.5 Calculations where


GIL = grams per litre of sodium formate;
GIL E= v x Jf x 68 V- volume in ml of standard hydrochloric
10 acid solution;
Jv= normality of standard hydrochloric
Assay, percent by
GIL x 100 acid solution; and
mass =
M M = mass of sample taken, g.

ANNEX B
[ Table 1, SZJvo. (ii) ]

ORGANIC IMPURITIES ( BY DIFFERENCE )

B-l CALCULATION substracting from one hundred the some of


nerctnt of assay, volatile matter and water
organic impurities shall be determined by &olubles,

ANNEX C
[ Table 1, SZJvo. (iii) 3
DETERMINATION OF VOLATILE MATTER

c-1 PROCEDURE where


Weigh accurately approximately 10 g of sample
A4 ~1 mass of sample taken for test, g;
in a weighing bottle and keep it for 2 hours in an
air oven at 15°C. Cool in a desiccator and weigh. Ml = mass of sample with weighing bottle, g;
Dry again and repeat until constant mass is ob-
and
tained.
c-2 CALCULATION M z = mass of sample after drying with weigh-
ing bottle, g.
Volatile matter,
MI---fifa x ,,,0
percent by mass = M

ANNEX D
[ Table 1, Sl flo. (iv) ]

TEST FOR HEAVY METALS ( OTHER THAN IRON )

D-l REAGENTS volumetric flask and dissolve it in water and mahe


up to the mark. One millilitre of this solution
D-l. 1 Hydrochloric Acid containing 0.1 mg of lead ( as Pb ) .

Approximately 1 N. D-2 PROCEDURE

D-1.2 Hydrogen sulphido Solution D-2.1 Take 20 & 0.2 g of the material in a Nes+
ler cylind:.r and add 2.5 ml of hydro&lori~ acitl
Saturate a small quantity of water with hydrogen solution. IMute the contents to lU0 ml with water
sulphide gas. This solution shall be prepared and saturate with hydrogen sulphide solution. ‘I’o
fresh. another Nessler cylinder containing 80 ml 01
D-l.3 Standard Lead Solution water, add an agreed volume of standard Iraci
solution followed by 2.5 ml of hydroch!ori: :~cid
Weigh accurately ( up to I)*1 mg accuracy ) 0.16 g solution and saturate with llytirogen sulpni~ic~
of lead nitrate. Place in a 1 000 ml one.mark solution and dilute to 100 ml.

4
IS 13475 : 1992

D-2.2 The material shall be taken to have passed not darker than that produced with the standard
the test if the colour produced with the material is lead solution.

ANNEX E
[ Tuble 1, $1 Jvo. (v) ]

DETERMINATION OF IRON CONTENT

E-l OUTLINE OF THE METHOD E-3 PROCEDURE

The colour produced and extracted in mixed sol- Weigh accurately about 5 g of sample (~$1) and
vent’s layer, when the material is treated with dissolve it in 50 ml of wa.ter. Add 10 ml of hydro-
hydrochloric acid and potassium thiocyanate chloric acid and boil it until the total volume is
followed by mixture of amyl alcohol and any1 reduced to about 10 ml. Cool and transfer into
acetate, is compared to that produced by the IOO-ml volumetric flask and make up to the mark
standard iron solution under identical conditions. with distilled water. Take 10 ml of made up
solution in a Nessler tube. Add few drops of 0.2 N
E-2 REAGENTS potassium permanganate solution till permanga-
nate colour persists and add 5 ml of 20 percent
E-2.1 Concentrated Hydrochloric Acid potassium thiocyanate solution, shake well, add
10 ml of amy 1 alcohol, amyl acetate mixture and
E-2.2 Potassium Thiocyanate
extract the roloured iron complex in this mixtures
20 percent ( m/m ). layer. Carry out a blank test by taking 1 ml of
hydrochloric acid in another Nessler cylinder and
E-2.3 Potassium Permanganate add these reagents in the same order. Then add
standard iron solution drop by drop to the blank
O-2 N.
Nessler tube until both the tubes have same
E-2.4 Organic Mixture intensity of colour observed in an organic layer.
Note the volume of standard iron solution con-
Mizh;clual volumes of amyl acetate and amyl sumed (V) for producing the colour ( cqu~l to
that of sample ) in the blank tube.

E-2.5 Standard Iron Solution E-4 CALCULATION


vx 10
Iron, ppm = M
Dissolve 7.022 g of ferrous ammonium sulphate in
a mixture of 600 ml of water and 350 ml of dilute where
sulphuric acid and dilute to 1 000 ml with water.
M = mass of material taken for test, g; and
Further dilute 1 ml of the solution so obtained
to 1 000 ml with water. One millilitre of the dilut- Y = volume of standard iron solution u?ed,
ed solution contains 0.001 mg of iron ( as Fe ). ml.

ANNEX F
[ Tdh 1, 3 m. (vi) I

DETERMINATION OF WATER INSOLUBLE MATTER

F-l PROCEDURE F-2 CALCULATION

Weigh accurately 20 g of thr sample and dissolve Matter insoluble,


.,lY1 - M,
it in 100 ml of distilled water. The dissolved percent : __ ___ x 100
A4
sample solution is liltered through a weighed
where
sinterrd glass crucible of G3 porosity. After
filtration, heat the crucible for one hour in an M = mass of sample taken for test, g:
air oven at 120°C. Cool in a desiccator and ,VZl = mass of crucible with residue, g:( and
weigh. .\I s = mass of crucible, ,g.

5
1s 13475 : 1992

ANNEX G
[Tab/e 1, SZjlro. (vii) ]

DETERMINATION OF SULPHATES

G-l APPARATUS make up to 100 ml.


Nessler Cylinder - 50 ml capacity ( see IS 4161 : G-3 PROCEDURE
196; ).
G-3.1 Dissolve 2.0 g of the material in 50 ml of
G-2 REAGENTS
water contained in the Nessler cylinder. Add 1 ml
G-2.1 Dilute Hydrochloric Acid of dilute hydrochloric acid and 1 ml of barium
Approximately, 5 N. chloride solution. Allow to stand for one hour.
G-2.2 Barium Chloride Solution G-3.2 The material shall be taken to have passed
Dissolve 12 g of barium chloride in water and the test if no tL1rbidit.yor precipitate is produced.

ANNEX H
[ Table 1, SZJVO.(viii) ]

DETERMINATION OF CHLORIDE

H-l APPARATUS H-3 PROCEDURE


Nessler Cylinder - 50 ml ( see IS 4161 : 1967 ).
H-3.1 Dissolve 2-O g 01 the material m 50 ml of
H-2 REAGENTS water contained in Nessler cylinder, Add 1 ml of
H-2.1 Dilute Nitric Acid dilute lritric acid and 1 ml of silver nitrate solu-
tion.
Approximately, 5 N.
H-2.2 Silver Nitric Solution H-3.2 The material shall be taken to have passed
Dissolve 4-2 g of silver nitrate in 100 ml of water. in the test if no opalescence is produced.

ANNEX J
( Clause 6 )

SAMPLING OF SODIUM FORMATE

J-I GENERAL J-1.5 The samples shall be placed in suitable,


clean, dry and air-tight containers on which tht:
J-1.1 Samples shall not be taken in the exposed material has 110 action.
place.
J-l.6 The sample containers shall be of such a
J-1.2 l’lle sampling instrument shall be clean and size that they almost but not completely filled h,
dry. the sample.

J-l.3 precautions shall be taken to protect the J-l.7 Each sample container shall bc sealed air-
silmples, the material being sampled, the sampl- tight after filling and marked with full idcntifica-
ing instrument and the containers for samples tion particulars such as sample number, the date:
11om adventitious contamination. of sampling, batch of manufacture of the material
and other important particulars of the consign-
mcht.
J-l.4 To draw a representative sample, the con-
tents of each container selected for sampling shall J-l.8 Sample shall be stored in suclr a mannci
be mixed as thoroughly as possible by suitable that the temprrature of the material does not var)
means. unduly from the normal trmperaturc.

6
iS 13475: 1992

J-2 Scale of Sampling J-3 PREPARATION OF SAMPLES


J-2.1 Lot J-3.1 From each of the packages selected, draw
with an appropriate sampling instrument small
In a single consignment, all packages of the same
quantity of material from different portions of the
sizes, containing material from the same batch of
packages and mix thoroughly. This shall consti-
manufacture, shall constitute a lot. If a consign-
tute the representative sample for the package.
ment is known to consist cf packages belonging to
different batches of manufacture, packages belong-
J-3.2 From the sample representing different
ing to the same batch of manufacture shall be
packages selected in J-2.3 small but approximately
grouped together and each such group shall
equal quantity of material shall be taken and
constitute a lot.
mixed thoroughly to form a composite sample
J-2.2 For ascertaining the conformity of the which shall be sufficient for carrying out triplicate
material in a lot to the requirements of this speci- tests for the characteristics given in Table 1. The
fication, samples shall be tested on each lot composite sample shall be divided into three equal
separately. parts, one for the purchaser, another for the
supplier and third for the reference.
J-2.3 ‘Ihe rnmber of Fackages to be sampled for
this Furpose shall depend on the size of the~lot J-3.3 The referee sample shall bear the seals of
and shzll be in actor_dance with Table 2. both the purchaser and the supplier and shall be
kept at a place agreed to between the two. It
Table 2 Scale of Sampling shall be used in case of any dispute between the
two.
Lot Size Number of Containers
to be Selected
J-3.4 The composite sample shall be transferred
(1) (2) to separate containers. The sample containers
up to 50 3 shall then be sealed with stoppers and labeled
51 ), IO0 4 with full identification particulars given
101 ,> 150 5 in J-1.7.
151 ,, 300 6
301 ,, 500 J-4 NUMBER OF TESTS
501 ,, 800 8
Tests for all characteristics given in Table 1 shall
801 ), 1 300 9
be conducted on the composite sample.
1 301 and above 10
J-5 CRITERIA FOR CONFORMlTY
J-2.3.1 These packages shall be selected at ran-
dom. In order to ensure the randomness of The lot shall be declared as conforming to this
selection, random number tables shall be used, specification, if the test results on ,the composite
For guidance to the use of random number table, sample for each of the characteristics meet
reference may be made to IS 4905 : 1968. relevant requirements given in Table 1.
.

Standard Mark
The use of the Standard Mark is governed by the provisions of the Bureau of Indian
Standards Act, 1986 and the Rules and Regulations made thereunder. The Standard Mark on
products covered by an Indian Standard conveys the assurance that they have been
produced to comply with the requirements of that standard under a well defined system of
inspection, testing and quality control which is devised and supervised by B1S and operated
by the producer. Standard marked products are ah.0 continuously checked by BIS for con-
formity to that standard as a further safeguard. Details of conditions under which a licence
for the use of the Standard Mark may be granted to manufacturers or producers may be
obtained from the Bureau of Indian Standards.
Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian StandardP Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality certification of goods
and attending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced in any
form without the prior permission in writing of BIS. This does not preclude the free use, in the course of
implementing the standard, of necessary details, such as symbols and sizes, type or grade designations.
Enquiries relating to copyright be addressed to the Director ( Publications ), BIS.

Revision of Indian Standards

Indian Standards are reviewed periodically and revised, when necessary and amendments, if any, are
issued from time to time. Users of Indian Standards should ascertain that they are in possession of the
latest amendments or edition. Comments on this Indian Standard may be sent to BIS giving the
following reference:

Dot : No. PCD 9 ( 789 )

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS

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Telephones : 331 01 31, 331 13 75 ( Common to all offices)

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---__
)‘rint.cfRINew lndin I’rinrina I’mss. Khxn 111lnkl,,

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