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IS 13014 (1990): Sodium gluconate for electroplating [CHD


5: Electroplating Chemicals and Photographic Materials]

“!ा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”
( Reaffirmed 2003 )

Indian Standard
SODIUMGLUCONATEFOR
ELECTROPLATING- SPECIFICATION

UDC 661’733’47 : 621’357’7

@ BIS 1991

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

April 1991 Price IGroup 3


Electroplating Chemicals Sectional Committee, CHD 05i

.
FOREWORD

This Jrdian Standard was adcIted by the Eurcau of Jndifn Stsndards on 25 May 1990, after the
draft finalized by the Electroplating Chemicals Sectional Committee had been approved by the
Chemical Division Council.

Sodium gluconate is the sodium salt of gluconic acid otherwise called 1:2: 3 : 4: 5 Pentahydroxy
caproic acid. It is used in the processing of foods and pharmaceuticals, as paint stripper and
aluminium deoxider, bottle washing preparations. However, this standard covers the salt which
is largely used as a complexant ingredient of plating baths, pickling and alkaline cleaning solutions
for metal cleaners and rust removal.

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
jn 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 regard.
1s13014:l!wo

Indian Standard
SODIUM GLUCONATE FOR
l

ELECTROPLATING - SPECIFICATION
1 SCOPE Table 1 Requirements for Sodium Glucenate
for Electroplating
I.1 This standard prescribes the requirements, ( Clauses 3.2 and 5.1 )
methods of sampling and tests for sodium
gluconate for electroplating. Characteristic Require- Method of
i%. meat Test ( Ref
2 REFERENCES
AZker )
2.1 The following Indian Standards are the (1) (2) (3) (4)
necessary adjuncts to this standard: i) Sodium gluconate, percent 97.0 A
by mass, Min
IS No. Title
ii) Solubility B
264 : 1968 Nitric acid ( first revision ) T,oeP,~“,S

1070 : 1977 Water for general laboratory use iii) Specific rotation with +12 &0’5” C
sodium vapour lamp as
( second revision ) light source
3 REQUIREMENTS iv) Chloride ( as Cl ), percent 0.15 D
by mass, Max
3.1 Sodium gluconate shall be in the form of v) Sulphate (as SO, ), percent @50 E
white-to-yellowish crystalline powder, readily by mass, Max
soluble in water, sparingly soluble in alcohol, vi) Heavy metals ( as Pb ), 0.002 F
-insoluble in ether and of low toxicity. The salt percent by mass, Max
shall correspond essentially to the formula vii) Reducing agent ( as Glu- 0.05 G
NaCsH1lO,. case ), percent by mass,
MaX
3.2 Sodium gluconate shall also comply with
the requirements given in Table 1. 6 PACKING AND MARKING
4 SAMPLING 6.1 Packing
4.1 The method of drawing representative The material shall be packed in high density
samples of the material and the criteria for polyethylene wovenbagsfibre drums with poly-
determining the conformity of the material to ethylene lining not exceeding 50 kg in mass
the requirements of this specification shall be as when packed.
prescribed in Annex H.
6.2 Marking
5 TEST METHODS
The containers shall be marked with the
5.1 Tests shall be conducted as prescribed in following particulars:
co1 4 of Table 1. a) Name of the material;
5.2 Quality of Reagents b) Net mass; *

Unless specified otherwise, pure chemicals and c) Indication of the source of manufacture;
distilled water ( see IS 1070 : 1977 ) shall be d) Batch number; and
employed in tests.
e) Date of manufacture.
NOTE - ‘Pure chemicals’ shall mean chemicals
6.2.1 The containers may also be marked with
that do not contain impurities which affect the
results of analysis. the Standard Mark.
IS 13014:1990

ANNEX A
[ Table 1, SZ No. (i) ]
- DETERMINATION OF SODIUM GLUCONATE CONTENT

A-O GENERAL sulphuric acid solution. Cover the beaker with


a watch glass to prevent loss of solution from
A-0.1 A simple method of determination is to spray due to evolution of carbon dioxide. Boil
oxidize mostly to the corresponding carbonate the solution for 20-30 minutes to drive off all the
by igniting in air and to estimate the alkaline dissolved carbon dioxide. Allow the contents
residue acidimetrically. of the beaker to cool and titrate with 0’5 N
sodium hydroxide using a few drops of the
A-l REAGENTS indicator. Record the volume of alkali consum-
A-l.1Standard Sulphuric Acid Solution, 0'5N. ed corresponding to the stage when the solution
assumes a permanent pink colour.
A-l.2 Standard Sodium Hydroxide Solution,
0’5 N. A-2.2 Calculation
Sodium gluconate, percent by mass
A-l.3 Phenolphthalein Indicator
1 percent ( m/v ) solution in 1 : 1 ethanol water = ( 50 - v) x 0’5 x 218’13
10 x M
mixture, prepared by dissolving the solid into
ethanol, mixing with an equal volume of water. where
Filter, if necessary. V = the volume of alkali solution consumed
and 218’13 is the equivalent weight of
A-2 PROCEDURE sodium gluconate, and
A-2.1 Weigh accurately approximately 0’4 g of M= mass in g of the sample taken for test.
the material into a platinum crucible. Ignite at
NOTE - Porcelain will react with sodium carbo-
800 to 9CO”C, until all traces of carbon have been nate at a high temperature and hence a platinum
burnt off. Cool the crucible and carefully place crucible is to be used as the container during
it into a 250-ml beaker containing 50 ml of 0’5 iV ignition.

ANNEX B
[ Table 1, SZ No. (ii) ]

TEST FOR STABILITY

B-1 STABILITY TEST observe. The material shall be taken to have


satisfied the requirement of this test if there is
B-l.1 Weigh accurately about 1’0 g of the no turbidity at all .
material and dissolve it in 50 ml water and

ANNEX C
[ Table 1, SZ No. (iii) ]
DETERMINATION OF SPECIFIC ROTATION

C-O GENERAL thermostatically the temperature of water circn-


lating through the jacket at 20°C. Dry the
C-O.1Solutions of sodium gluconate rotate the polarimeter tube. Place the sodium vapour
plane of polarized light due to their optical 1amp about 20 cm from the instrument, switch
activity and specific rotation is a characteristic the light-source on, remove the tube from its
of the compound. rack and see that the instrument is in proper
adjustment. Prepare a solution of sodium
C-l PROCEDURE gluconate by dissolving about 5 g of an accu-
C-l.1 Set up a water-jacketed polarimeter for rately weighed quantity of the salt in water in a
measuring optical activity, according to instruc- 100 ml volumetric flask and make up to the
tions given in the instrument manual. Maintain mark. Fill the poiarimeter tube with the

2
IS 13014 : 1990

solution, taking care to eliminate any air bubble of the tube ( in dm ), and C the mass in g of
which may tend to collect therein. Insert the sodium gluconate per 100 ml of solution, and D
tube in position and at once take a reading. denotes the use of sodium vapour lamp as the
. light-source.
C-l.2 Calculation
100 x I NOTE - The solution shall be clear and the lenses
Specific rotation [ cc ] f = C , where cc and tube-windows with no liquid on the outside
and free from air bubbles. Positive angle indicates
is the observed angle or rotation, I the length dextrorotation.

ANNEX D
[ Table 1, Sl No. (iv) ]

DETERMINATION OF CHLORIDES

D-l APPARATUS water, add 2 ml of concentrated nitric acid and


D-l.1 Nessler Cylinders - 50 ml capacity. 1 ml of silver nitrate solution. Make up the
solution to 50-ml mark. Carry out a control
D-2 REAGENTS test in the other Nessler Cylinder using 1’4 ml
D-2.1 Concentrated Nitric Acid - See IS 264 : of standard chloride solution and the same
1968. quantities of other reagents in the same total
volume of the reaction mixture. Stir both the
D-2.2 Standard Chloride Solution solutions with glass rod and compare the
Dissolve 1’649 g of sodium chloride in water opalescence produced in the two cylinders after
and make up the volume to 1 000 ml. One 5 minutes.
millilitre of this solution contains 1’0 mg of D-3.2 The limit prescribed in Table 1 shall be
chloride ( as Cl ). taken as not having been exceeded if the
D-3 PROCEDURE opalescence produced in the test with the
material is not greater than that produced in the
D-3.1 Dissolve 10 g of the material in 20 ml of control test.

ANNEX E
[ Table 1, SZ No. (v) ]

DETERMINATION OF SULPHATES

E-l REAGENTS crucible or a filter paper ( Whatman No. 42 or


equivalent >. Wash the precipitate with hot
E-l.1 Dilute Hydrochloric Acid - 5 N approxi- water and ignite. Cool and weigh till constant
mately. weight is obtained.

E-l.2 Barium Chloride Solution - 10 percent E-2.2 Calculation


( w/v ). Sulphate ( as SO4 ), percent by weight
E-2 PROCEDURE W,
= 41.15-
E-2.1 Dissolve 3 g of the material in 100 ml of WZ
water and 2 ml of dilute hydrochloric acid. where
Filter, if necessary and heat the filtrate to
WI = weight in g of the precipitate, and
boiling, add slowly with constant stirring 5 ml
of barium chloride solution and allow to stand Wz = weight in g of the material taken for
overnight. Filter through a tared Gooch the test.
IS 13014 : 1990

ANNEX F
[ Table 1, Sl No. (vi) ]
.
DETERMINATION OF HEAVY METALS

F-l APPARATUS 100 ml with water. One millilitre of this solution


contains 0’1 mg of lead ( Pb ).
F-l.1 Nessler Cylinders, 50 ml capacity.
F-2.7 Sodium Snlpbate Solution, approximately
F-2 REAGENTS 10 percent ( w/v ).

F-2.1 Acetic Acid, approximately 33 percent F-3 PROCEDURE


( w/w ).
F-3.1 Weigh 5’0 g of the material into a Nessler
F-2.2 Dilute Ammonium Hydroxide, approxi- cylinder and dissolve in 30 ml of hot water.
mately 10 percent ( w/w ). Add 5 ml of acetic acid. Make it alkaline to
litmus by gradual addition of dilute ammonium
F-2.3 Hydrogen Peroxide, approximately 6 per- hydroxide and add 1 ml of potassium cyanide
cent ( w/w ). solution. Carry out a control test in the other
Nessler cylinder using 2’0 g of the material,
F-2.4 Potassium Cyanide Solution 1’0 ml of standard lead solution and the same
quantities of other reagants. Filter both the
Dissolve 10 g of potassium cyanide in 90 ml of solutions, if they are turbid, and if the colours
water, add 2 ml of hydrogen peroxide, allow to of the solutions differ, equalize by the addition
stand for 24 hours and make up to 100 ml of a few drops of a highly diluted solution of
with water. burnt sugar or other non-reactive substance.
Dilute both the solutions with water and make
F-2.5 Concentrated Nitric Acid, see IS 264 : up the volume of each to 50 ml. Add 2 drops
1968. of sodium sulphide solution, mix thoroughly
and compare the colours developed in the two
F-2.6 Standard Lead Solation cylinders after 5 minutes.
Dissolve 1’60 g of lead nitrate [ Pb ( NO* )Z ] F-3.2 The limits prescribed in Table I shah be
in water and make up the solution to 1 OOO-ml taken as not having been exceeded if the colour
mark in 3 volumetric flask. Pipette out 10 ml produced in the test with the material is not
of the solution and dilute again to exactly deeper than that produced in the control test.

ANNEX G
I:Table 1, Sl No. (vii) ]
DETERMINATION OF REDUCING AGENT

G-O GENERAL bicarbonate and introduce 5 g of potassium


iodide. Transfer the mixture to a 1 litre
The method involves treatment of an aliquot of volumetric flask, add 250 ml of 0’1 N potassium
the material with alkaline copper sulphate iodate ( obtained by, dissolving 3’567 g of
solution containing potassium iodate and potassium iodate in water in a I-litre volumetric
potassium iodide followed by titration of the flask and making up >, dilute to volume and
acidified solution against a standard sodium filter through fitted glass. Age overnight before
thiosulphate solution. use.
G-l REAGENTS G-l.2 Iodide-Oxalate Solution
Dissolve 2’5 g of potassium iodide and 2’5 g of
G-l.1 Shaffer-Somoygi Carbonate-Potassium potassium oxalate in water and dilute to 100 ml.
Iodide Reagent Prepare fresh when required.
Dissolve 25 g of anhydrous sodium carbonate rit; iodium Thiosulphate Standard Solution
and 25 g of potassium sodium tartrate ( Rochelle .
salt ) in about 500 ml water in a 2-litre breaker.
Add through a funnel with its tip under the Prepare daily from a stock solution of 0’1 N
solution surface and with stirring, 75 ml of a solution, standardized by means of a standard
solution of 100 g/l copper sulphate pentahydrate potassium dichromate solution ( approximately
( CuSOa . 5HzO ). Dissolve 20 g of sodium 0’1 N).

4
IS 13014 : 1990

64.4 Starch Indicate bath for IS minutes. Remove tubes carefully


without agitation to running water, cooling
Mix in a glass mortar 2’5 g of soluble starch, them for 4 minutes. Rinse funnels and add
about 10 mg of mercuric iodide and a little water down the side of each tube 2 ml of potassium
in order to make a paste. Dissolve in about iodide potassium oxalate solution and then 3 ml
500 ml boiling water. of 2 N sulphuric acid solution. Abstain from
shaking the solution while alkaline. Mix
G-l.5 Sulphnric Acid ( 2 N ) thoroughly so that all cuprous oxide is dissolved
Add to about 100 ml of water in a 250-ml and let stand in a cold water bath for 5 minutes
beaker, 5’5 ml of concentrated sulphuric acid mixing twice. Carry out titration with the
mix well and then make up this solution to 1-litre standard sodium thiosulphate solution using
in a volumetric flask. starch indicator. Subtract titre of the test
solution from that of the blank and calculate the
G-l.6 Glucose, Pure ( for control deter- amount of glucose as follows:
minations ). Reducing agent ( as Glucose ), percent by mass
G-2 PROCEDURE ( 0.109 9 x 0’005 N
= thiosulphate ) + 0’048
Obtain a 50 ml solution of 20 g of sodium 20
gluconate in a 50 ml volumetric flask by dis-
solving the material in water and making up. Periodically carry out control determinations
Pipette 5 ml of the solution ( containing 0’5 - with known quantities of pure glucose and apply
2’5 mg of glucose ) into a 25 x 200 mm test corrections for deviations from the equation,
tube. Introduce 5 ml of carbonate potassium mg. Glucose = ( 0’109 9 x ml 0’005 N thio-
iodide reagent and mix well by swirling. Prepare sulphate ) + 0’048
also a blank with 5 ml of water and 5 ml of
carbonate potassium iodide reagent. Keep the used for determination of the same in the test
tubes capped with funnels in a boiling water material.

ANNEX H
( Clause 4.1 )

SAMPLING OF SODIUM GLUCONATE FOR ELECTROPLATING

H-l GENERAL REQUIREMENTS FOR H-2 SCALE OF SAMPLING


SAMPLING
H-2.1 Lot
H-l.1 Samples shall be taken in a protected
place not exposed to damp air, dust or soot. In a single consignment all the containers of the
material drawn from a single batch of manu-
H-l.2 The sampling instrument shall be clean facture shall constitute a lot.
and dry.
H-2.2 For ascertaining the conformity of the
H-l.3 Precautions shall be taken to protect the material to the requirements of this specification,
samples, the material being sampled, the samples shall be tested for each lot separately.
sampling instrument and the containers for The number of containers to be selected at
samples from adventitious contamination. random from lots of different sizes shall be in
H-l.4 To draw a representative sample, the accordance with Table 2.
contents of each container selected for sampling
Table 2 Number of Containers to be Selected
shall be mixed as thoroughly as possible by from Lots of Different Sizes
suitable means.
( Clause H-2.2 )
H-l.5 The samples shall be placed in suitable,
clean, dry and air-tight bottles or other suitable Lot Size Sample Size
containers on which the material has no action. N
H-l.6 The sample container shall be of such a (1) (2;
size that they are almost completely filled by 3to 15
16 to 40 :
the sample. 41 to 110 5
6
H-l.7 Each sample containers shall be sealed i:t :: ::
air-tight after filling, and marked with full 301 to 500 i
details of sampling, the date of sampling and 501 to 800
801 and above 1:
details given under 3.2.

5
IS 13014: 1990

H-2.3 The containersshall be selected at random H-3.4 The set of referee samples consisting,
from the procedure given in IS 4905 : 1968 like the other two sets, of a composite sample
Methods of sampling may be followed. and individual samples shall bear the seal of
both, the purchaser and the manufacturer and
H-3 PREPARAXION OF TEST SAMPLES shall be kept under conditions suitable to
preserve the characteristics of the material.
H-3.1 From each of the container selected
in H-2.3 small portions of material shall be H-4 NUMBER OF TESTS
taken from different parts with the help of a
suitable sampling instrument. This portions when H-4.1 Each of the individual samples shall be
mixed together shall constitute the individual separately tested for sodium gluconate content.
sample left after preparation of the composite
sample as prescribed in H-3.2 shall be not less H-4.2 The composite sample shall be tested for
than 3 times and material required for testing all the other requirements of this specification.
prescribed in H-4.1, and shall be divided into
3 equal parts, one each for the buyer and H-5 CRITERIA FOR CONFORMITY
the manufacturer, and the third as referee
sample. H-5.1 For Individual Sample

H-3.2 From all the individual samples obtained The mean and the range of the individual tesb
in H-3.1, small but equal quantities of material results on sodium gluconate content shall be
shall be taken and mixed to constitute the computed as follows:
composite sample. The material in the com- Sum of individual test results
posite sample shall be at least three times the Mean (X)=
material required for testing prescribed in H-4.2, Number of test results
and shall be divided into three equal parts one Range ( R ) = Difference between the maxi-
each for the buyer and the manufacturer and mum and the minimum tesb
the third as referee sample. results.
H-3.3 All the samples obtained after division H-5.1.1 The lot shall be declared to have
in H-3.1 and H-3.2 shall be transferred to sepa- satisfied the requirement of sodium gluconate
rate sample container ( see H-l.5 and H-1.6) content if the value of the expression ( X - 0’6
which shall be closed air-tight, sealed and marked R ) is greater than or equal to the minimum
with identification particulars ( see H-l.7 ). value specified in Table 1.

6
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 BIS and operated by the pro-
ducer. Standard marked products are also continuously checked by BIS for conformity 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.
Buteoa ef fdimb StaRBards

BIS isastatutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality tiertification 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 ( Publication ), 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. CHD 05 ( 9265 )

Amendments Issued Since Publication


Amend No. Date of Issue Text Affected

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