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-1964

Indian Standard
( Reaffirmed 2006 )
(Reaffirmed!2012)!
(Reaffirmed 2018)
METHODS OF
CHEMICAL ANALYSIS OF COPPER
( Revised.
Sixth Reprint AUGUST 1993

UDC 669’3 543

Copyright 1964
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH
NEW DELHI 110002
March 1964
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Indian Standard
METHODS OF
CHEMICAL ANALYSIS OF COPPER
Revised)
Methods of Chemical Analysis Sectional Committee, SMDC 2

Da T. National Laboratory

D B H. P. to
Dr T. )
K. L. Refractories Sectional Committee, SMDC 18,
Assay ( Ministry of
K. BOSE
G. Steel Ltd, Durgapur Steel Plant,
Durgapur
A. C. ( )
Grganisation
Ministry of Railways
Defence Research Laboratory
( Alternate)
R. K.
[ Ministry of ( D ) Ishapur
D. N. Ltd, Bombay
S. S. ( Alternate )
B. B. Indian Iron Steel Co Ltd, Burnpur
J. N. B ( Alternate )
C. R. Ferro Alloys Corporation Ltd,
ARMAN

)
SHRI A. RAO ( Alternate )
D R S. Central Glass Ceramic Research Institute
( CSIR
B. K. ( Alternate )
D. R. Director General, Ordnance Factories ( Ministrv
of Defence
R. N. (Alternate)
M. M. Non-Ferrous Metals Asso-
ciation, Calcutta
N. )
(Continued on page 2

BUREAU OF INDIAN STANDARDS

M A N A K B H A V A N , 9 B A H A D U R S HAH MARG
NEW DELHI 110002
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( Continued from page 1

Member8
V. L. N. The Iron Steel Co Ltd,
I-I. P. ( Alternate )
N. Government Test House, Calcutta
P. R. National Chemical Laboratory ( CSIR ), Poona
D R J. L. ( Alternate )
B. S. Director, IS1 Member)
Deputy Director ( S M )

S. L. B A L I
Extra Assistant Director ( S M IS1
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CONTENTS

0. ... ... ... ... ...

SCOPE ... ... ... ... ...
2. ... ... ... ... ...
3. QUALITY OF ... ... ... ...
4. DETERMINATION OF COPPER BY ELECTROLYTIC M ETHOD
5. D ETERMINATION OF A RSENIC AND A NTIMONY BY THE
PRECIPITATION ( ) METHOD ... ... 9
6. D ETERMINATION OF BY THE H YPOPHOSPHITE
METRIC ALTERNATE METHOD ( APPLICABLE IN A BSENCE
OF Se and Te) ... ... ... ... 12
7. OF BISMUTH BY THE IODIDE ( PHOTOMETRIC )
... ... ... ... ... 14
8. OF I R O N ... ... ... 16
By the (Volumetric Method . . . ... 17
By the Ammonium Thiocyanate ( Photometric ) Method 18
9. D ETERMINATION OF L EAD BY THE METHOD 19
10. OF N ICKEL BY THE
( GRAVIMETRIC METHOD ... ... ... 21
11. D ETERMINATION OF S ELENIUM BY THE
. . . ... ... ... ... 21
12. D ETERMINATION OF T ELLURIUM BY
23
13. D ETERMINATION OF BY THE C OMBUSTION 23
14. D ETERMINATION OF T IN BY THE IODIMETRIC ... 26
DETERMINATION OF PHOSPHORUS BY METHOD 28
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Indian Standard
METHODS OF
CHEMICAL ANALYSIS OF COPPER
(Revised)
0. FOREWORD
0.1 This revised Indian Standard was adopted by the Indian Standards
Institution on 28 January 1964, after the draft finalized by the Methods
of Chemical Analysis Sectional Committee had been approved by the
Structural and Metals Division Council.
This standard was originally published in 1955 and covered
chemical analysis of copper as specified in IS 191-1950 Specification
for Copper. In the revised version of IS 191-1950, which was published
in 1958, and its subsequent amendment published in 1961, a few more
grades have been included and the chemical composition modified.
Necessity was, therefore, felt to revise this standard also so that it could
cover completely all the elements within the chemical composition ranges
as specified in *IS 191-1958 Specification for Copper ( Revised
0.3 In this revised version, changes mentioned in 0.3.1 to 0.3.3 have been
introduced.
The following methods have been added:
a) Determination of Arsenic by the Hypophosphite Method, and
b) Determination of Iron by the Volumetric Method.
The methods for bismuth and iron given in
1955 have been replaced by the photometric methods.
The methods for determination of copper, tin, nickel, arsenic,
antimony and lead given in IS 440-1955 have been revised.
The methods of analysis prescribed in this standard have been prepared
with a view that they shall be useful as referee methods. Due considera-
tion been given in the preparation of this standard to the facilities
in the country for such analysis.
in
4
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0.5 Taking into consideration the views of producers, consumera and

ing authorities, the Sectional Committee responsible for the preparation of
this standard felt that it should be related to the technological methods
followed in the country in this field. Assistance has been derived from
the following publications:
1962 B OOK ASTM METHODS FOR C HEMICAL ANALYSIS OF
American Society for Testing and Materials.
B.S. 1800 1951 METHODS FOR THE OF R AW
British Standards Institution.
FURMAN , N. H. (ED.) SCOTT , W. W. Standard Methods of Chemical
5th ed. New York. D. Van Nostrand Company,
W. F., LUNDELL , G. E. F. and H. A. Applied
Inorganic Analysis, 2nd ed. New York. John Wiley and Sons, 1955.
0.6 Wherever a reference to any Indian Standard appears in this
dard, it shall be taken as a reference to the latest version of the standard.
0.7 In reporting the results of a test or analysis made in accordance
with this standard, if the final value, observed or calculated, is to be
rounded off, it shall be done in accordance with IS 2-1960 for
Rounding Off Numerical Values ( Revised

1. SCOPE
1.1 This standard prescribes the methods for determination of copper,
arsenic, antimony, bismuth, iron, lead, nickel, selenium, tellurium, oxy-
gen, tin and phosphorus in the ranges as specified in *IS: 191-1958
Specification for Copper ( Revised
2. SAMPLING
2.1 Samples shall be drawn in accordance with IS 1817-1961 Methods of
Sampling Non-Ferrous Metals for Chemical Analysis.
3. QUALITY OF REAGENTS
3.1 Unless specified otherwise, pure chemicals and distilled water [see
IS 1070-1960 Specification for Water, Distilled Quality ( Revised
shall be employed in the tests.
Pure shall that do not
which affect the of
l revision issued in
5
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DETERMINATION OF COPPER BY THE

METHOD
Outline of the Method-The sample is dissolved in sulphuric
nitric acid mixture and copper deposited electrolytically from the solution.
In case of copper, having a purity of less than percent, impurities
are removed by ferric hydroxide and then copper deposited electroly-
tically.
4.2 Apparatus -The following platinum electrodes (see Fig. 1 ) are
but strict adherence to the shape and size of the electrodes
is not essential. For agitation of electrolyte in order to decrease the
time of deposition, one of the types of rotating forms of electrodes,
generally available, may be employed.
4.2.1 Cathode-It may be formed either from plain or perforated
sheet or from wire gauze.
4.2.1.1 Gauze cathodes preferably made from gauze containing
400 mesh/cm* should be used. The wire used for making gauze should
be approximately mm in diameter. Cathode should be stiffened by
doubling the gauze for 3 mm on the top and the bottom or
by reinforcing the gauze at the top and bottom with platinum ring
or band.
4.2.1.2 The diameter of the cylinder should be approximately 30
mm and the height 50 mm. The stem should be made from platinum
alloy wire, such as platinum-iridium, platinum-rhodium or
ruthenium having diameter of approximately mm. It should be
flattened and welded along the entire length of the gauze. The overall
height of the cathode should be approximately 130 mm.
Anode-Either a spiral or a gauze anode should be used. The
spiral of seven turns with a height of approximately 50 mm and diameter
of mm should be made from mm or larger platinum wire,
the overall height being 130 mm. The gauze anode should made
of the same material and of the same general design as platinum gauze
cathode mentioned under 4.2.1. The diameter of the cylinder should be
12 mm and the height 50 mm, the overall height of the
130 mm.
4.3
Sulphuric Acid-Nitric Acid Mixture Add slowly, with
ml of concentrated sulphuric acid [ sp conforming
IS Specification for Sulphuric Acid ( Revised) to of
cool and add 210 ml of concentrated nitric acid see
4.3.2 Urea -solid.
6
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Cylindrical Platinum Spiral Platinum

Anode
All dimensions in
1 C YLINDRICAL P LATINUM C A T H O D E
PLATINUM A N O D E

4.33 Ethanol or Methanol -95 percent (v/v).

43.4 Ferric Nitrate Solution Dissolve 70 g of ferric nitrate crystals
in water and dilute to one litre.
43.5 Concentrated Ammonium Hydroxide 20 percent.
4.3.6 Ammonium Sulphate Solution 99 (
4.3.7 Dilute Acid- 1 1 and 2 (v/v).
4.3.8 -Concentrated Nitric Acid gr (conforming to 264-
1950 Specification for Nitric Acid
4.4 Procedure ( for Copper Having a Purity of percent and Over )
5 g of the accurately weighed sample into a
beaker provided with a cover glass and add 42 ml of sulphuric acid-nitric
acid mixture. After the initial reaction is over, heat to to
until completely dissolved and brown fumes are expelled.
.
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4.4.2 Wash_ down the cover and sides of the beaker and dilute
the solution sufficiently to cover the cathode cylinder. Insert the elec-
trodes, the cathode having been accurately weighed; of
split cover glass and for 16 hours at a current density
When the solution becomes reduce the current
density to add one gram of urea and wash down the cover
glasses and sides of the beaker and continue electrolysis until the deposi-
tion of copper is complete as indicated by absence of plating on the new
surface of the electrode obtained by the raised level of the solution.
4.4.3 Without interrupting the current, syphon off the
at the same time adding water to maintain the level of the solution.
Remove the cathode quickly, while washing further with water, rinse it
with water in a beaker and then dip it in two successive baths of ethanol
or methanol. Dry the cathode in an air oven at 110°C for three to five
minutes, cool and weigh for copper.
4.4.4 Calculation
Copper, percent = 100
where
A = weight in g of copper, and
B weight in g of the sample taken.
4.5 Procedure ( for Copper Having a Purity of Less Than 99’5 percent )
Dissolve the sample in the acid mixture as under 4.4.1. Eva-
porate until all the nitric acid is expelled. Dissolve the residue in 70 ml
of water, add 3 ml of ferric nitrate solution, heat just to boiling and
precipitate the iron by adding concentrated ammonium hydroxide in
slight excess keeping all the copper in solution. Filter and wash
the precipitate with ammonium sulphate solution and preserve the filtrate
and the washings.
4.5.2 Wash the precipitate back into the beaker and dissolve in dilute
sulphuric acid ( 1: 1 ). Re-precipitate with concentrated ammonium
hydroxide keeping the volume as little as possible. Filter through
the same paper and wash with ammonium sulphate solution. Again
wash the precipitate back into the beaker, dissolve, re-precipitate, filter
and wash. Combine all the filtrates and evaporate to get the proper
volume for electrolysis. Acidify with dilute sulphuric acid ( 1 2 ) and
add 15 ml in excess, and then add 2 ml of concentrated nitric acid.
the determination as described under 4.4.2 to 4.4.4.
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5. OF ARSENIC AND ANTIMONY BY THE

CO-PRECIPITATION ( IODIMETRIC ) METHOD
5.1 Outline of the Method -The sample is dissolved in nitric acid
and hydrochloric acid, Arsenic and antimony are co-precipitated with
ferric hydroxide, dissolved in sulphuric acid and determined, after
reduction and distillation as their trichlorides, volumetrically, by titra-
tion with standard iodine solution.
Apparatus An all glass distillation apparatus as shown in Fig. 2 shall
be used.
53 Reagents
53.1 Concentrated Nitric Acid -see 43.8.
5.3.2 Concentrated Hydrochloric Acid sp gr conforming to
IS 265-1962 Specification for Hydrochloric Acid ( Revised)
5.33 Ferric Nitrate Solution Dissolve 20 g of ferric nitrate crystals
Fe ( in water and dilute to 100 ml.
5.3.4 Concentrated Ammonium 20 percent.
5.3.5 Dilute Ammonium Hydroxide 1
5 3 . 6 Dilute Acid 1 3 (
5.3.7 Carbon Dioxide gas.
5.3.8 Hypophosphorus Acid SO percent (
5.3.9 Sodium Sulphite solid.
5.3.10 Sodium Hydroxide Solution 20 percent (
5.3.11 Methyl Red Indicator Solution Dissolve g of the reagent
in 60 ml of rectified spirit and make up to 100 ml with water.
5.3.12 Dilute Hydrochloric Acid 1 1 (
5.3.13 Sodium Bicarbonate solid.
5.3.14 Starch Solution Make a suspension of one gram of soluble
starch in about 10 ml of water and add it carefully to 100 ml of boiling
water. Boil for two or three minutes and cool. Prepare the solution
fresh as needed.
Potassium Iodide Solution Dissolve 100 g of potassium iodide
in water and dilute to one litre.
5.3.16 Standard Iodine Solution N approx. Dissolve 254 g of
iodine and 8 g of potassium iodide in ml of water. When solution is
9
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SEPARATING
FUNNEL
CONC HYDROCHLORIC

200-ml
FLASK

2 AND
BY

complete, dilute to one Store in a cool place in a dark-coloured

bottle. Standardize against pure arsenic trioxide
Acid Solution 25 percent (
10
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IS
5.4 Procedure
5.4.1 Transfer 20 g or less of the accurately weighed sample
ing not more than g of arsenic to a beaker and add 50 ml
of concentrated nitric acid and 20 ml of concentrated hydrochloric
acid. When the solution is complete, add 10 ml of ferric nitrate solution
and boil for one to two minutes. Dilute to 400 ml and add concentrat-
ed ammonium hydroxide until the acid is neutralized and the smell
of ammonia persists. Boil for five minutes and allow the precipitate to
settle. Filter through a rapid filter paper and wash with hot
dilute ammonium hydroxide solution, leaving some copper with the pre-
cipitate. Dissolve the precipitate through the filter paper with 25 ml of
hot dilute sulphuric acid and wash thoroughly with hot water, catching
the solution in the original beaker.
5.4.2 Transfer the clear solution to the distillation flask and fit up the
apparatus as shown in Fig. 2. Evaporate to white fumes while passing
a current of carbon dioxide through the apparatus. Allow the solution
to cool, place a beaker containing 50 ml of ice-cold water under
the condenser so that the tip of the condenser is dipped about
6 mm in water. Add 50 ml of concentrated hydrochloric acid and
one millilitre of hypophosphorus acid to the distillation flask.
5.4.3 Place about 80 ml of concentrated hydrochloric acid in the
separating funnel and pass a stream of carbon dioxide through
the apparatus. Heat the solution in the distillation flask while
concentrated hydrochloric acid from the separating funnel at a rate that
the temperature of the solution is maintained at about 110°C. Continue
distillation until all the acid from the separating funnel is added:
without disturbing the current dioxide, remove the receiver and
rinse the end of the condenser with water. Remove the beaker and
preserve for the determination arsenic ( see 5.4.5
5.4.4 Place a beaker containing 50 ml of water under the con-
denser so that the tip of the condenser dips under water. Add 80 of
concentrated hydrochloric acid in the funnel and pour it gradually
into the flask maintaining the temperature of the solution at about
until all the acid has been added. Remove the beaker containing
the distillate, add one gram of sodium sulphite, place cover on the
beaker and boil until the volume is reduced to 30 ml. Reserve the solu-
tion for the determination of antimony ( see 5.4.6
5.4.5 Cool the distillate in the beaker below neutralize with
sodium hydroxide solution using methyl red as indicator and add dilute
hydrochloric acid until the solution is just acidic. Cool and
add 8 to g of sodium bicarbonate, 5 ml of starch solution and
one millilitre of potassium, iodide solution. Titrate with Standard
iodine solution to a persistent blue tint.
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5.4.6 To the distillate reserved under for the determination

of antimony, add 80 ml of water and 10 ml of tartaric acid solution,
neutralize with sodium hydroxide to methyl red and make just acidic
with dilute hydrochloric acid. Cool, add 10 g of sodium bicarbonate,
ml of starch solution, one millilitre of potassium iodide and titrate
with standard iodine solution.
Carry out a blank determination following the same procedure
and using the same amounts of all reagents but without the sample.
5.5
Arsenic, percent C x

Antimony, percent = (A,- C x 6.09

D
where
volume in ml of the standard iodine solution required for
the sample,
volume in ml of the standard iodine solution required for
the blank,
c normality of the standard iodine solution,
D weight in g of the sample taken,
volume in ml of the standard iodine solution required for
the sample, and
= volume in ml of the standard iodine solution required for
the blank.
DETERMINATION OF ARSENIC BY THE HYPOPHOSPHITE
( ALTERNATE ) METHOD ( APPLICABLE I N
ABSENCE OF Se AND Te)
6.1 of the Method -Arsenic in the solution of the sample is
reduced by sodium hypophosphite to metallic arsenic in acid medium, and
metal by a measured excess of standard iodine solution to
pentavalent arsenic. The excess of iodine is back-titrated with standard
sodium arsenite solution.
6.2 Reagents
6.2.1 Dilute Sulphuric Acid- 1: 3
6.2.2 Concentrated Nitric Acid-see
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6.2.3 Concentrated Hydrochloric Acid see

6.2.4 Sodium Hypophosphite solid.
6.2.5 Dilute Hydrochloric Acid 1 3 (
63.6 Ammonium Chloride Solution 5 percent (
6.2.7 Standard Iodine Solution ( I ml = 0’000 15 g of As N.
Dissolve g of re-sublimed iodine and 4 g of potassium iodide in
25 ml of water. When the solution is complete, dilute to one litre with
water and store in a dark-coloured glass-stoppered bottle. Standardize
against standard arsenious oxide solution.
6.2.8 Sodium Carbonate solid.
6.2.9 Starch Solution -see 5.3.14.
6.2.10 Standard Sodium Arsenite Solution-001 N. Dissolve
g of arsenious oxide in about 4 ml of sodium hydroxide solution ( per-
cent and dilute to about 200 ml. Add dilute hydrochloric acid ( 1 20
until just acidic. Add about 2 g of sodium bicarbonate and dilute
to one litre in a volumetric flask.
6.3 Procedure
6.3.1 Transfer g of the accurately weighed sample to a beaker and
add 80 ml of dilute. sulphuric acid and 30 ml of concentrated nitric acid.
Evaporate the solution to fumes until all nitric acid is expelled. Cool,
dilute with 75 ml of hot water and boil gently to dissolve the salts.
Transfer the solution to a flask and rinse the beaker with 100 ml
of concentrated hydrochloric acid. Add 2 g of sodium hypophosphite,
warm to brisk effervescence avoiding boiling and further add 2 g of the
hypophosphite until no further effervescence occurs. Finally add 12 g of
hypophosphite and boil under reflux for 15 minutes.
63.2 Filter precipitated arsenic immediately, while hot, through
a paper-pulp pad and wash with 100 ml of dilute hydrochloric acid
containing 3 g of hypophosphite, and then about seven times with
ammonium chloride solution. Discard the filtrate and transfer the
residue immediately to a tall-type beaker, rinsing with about 50
ml of water.
Add a measured excess of the standard iodine solution, stir,
allow to stand for five minutes, then dilute if necessary. Add about 2 g of
sodium carbonate followed by a few millilitres of starch solution.
Titrate with standard sodium arsenite solution to a pronounced lighten-
ing of the Discharge the coloration by adding 3 ml more of the
standard sodium arsenite solution. Wash continuously with vigorous
shaking and back-titrate with standard iodine solution.
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6.3.4 Carry out a blank determination by following the same pro-

cedure and using the same amounts of all reagents but without the
sample.
6.4 Calculation
Arsenic, percent [ A (B + x
D
where
A volume in ml of the standard iodine solution,
B = volume in ml of the standard iodine solution equivalent to
standard sodium arsenite solution,
C = volume in ml of the standard iodine solution required for
the blank, and
D weight in g of the sample taken.
7. DETERMINATION OF BISMUTH BY THE IODIDE
METRIC ) METHOD
7.1 of the Method-Bismuth is collected and separated
from copper by precipitation with ammonia in the presence of
ferric iron and is determined photometrically using potassium iodide as
agent. The photometric measurement is made at approxi-
mately 440
7.2 Reagents
7.2.1 Concentrated Nitric Acid- see 4.3.8.
7.2.2 Ferrous Ammom’um Sulphate solid.
7.2.3 Concentrated Ammonium Hydroxide 20 percent.
7.2.4 Ammonium Carbonate Solution-Dissolve g of ammonium
carbonate in water and dilute to one litre.
7.2.5 Dilute Ammonium Hydroxide 1 9
7.2.6 Dilute Acid- 1 4 ( v/v).
7.2.7 Potassium Iodide Solution 10 percent (
7.2.8 Sodium Hypophosphite Solution 25 percent (
7.2.9 Phosphoric Acid- percent.
7.2.10 Standard Bismuth Solution ( I = I g of Bi ) Dissolve
0 g of pure bismuth metal in 10 ml of dilute nitric acid ( 1 and
2 ml of concentrated sulphuric acid and evaporate to fumes, Add few
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drops of concentrated nitric acid. Add 20 ml of water, heat to boiling

and dilute to one litre.
7.3 Procedure
73.1 Transfer 10 to 50 g ( depending upon bismuth content of
the accurately weighed sample to a beaker and add concentrated
nitric acid at the rate of 40 ml per 10 g of the sample. When the disso-
lution is complete, add g of ferrous ammonium sulphate and
boil for two minutes. Dilute to 200 ml with water and add concentrated
ammonium hydroxide until the precipitated copper hydroxide is redis-
solved, and then add a little in excess. Add 10 ml of ammonium
carbonate solution and heat to boiling. Allow the solution to stand
overnight. Filter through a rapid filter paper and wash with hot dilute
ammonium hydroxide. Dissolve the precipitate through the filter paper
with 20 ml of hot dilute sulphuric acid and wash with hot water.
Reprecipitate with concentrated ammonium hydroxide, boil for two
minutes and allow the precipitate to settle overnight. Filter and
wash with hot dilute ammonium hydroxide solution to remove the copper
completely and then twice with hot water. Dissolve the precipitate as
before.
73.2 Neutralize the solution with dilute ammonium hydroxide and
then acidify with dilute sulphuric acid avoiding excess of the acid. Add
4 ml of sodium hypophosphite solution, 10 ml of potassium iodide solu-
tion, few of phosphoric acid, and make the volume to 100 ml.
Allow the solution to stand for 10 minutes.
7.3.3 Transfer a suitable volume of the solution to an absorption cell
and take the photometric reading using a light filter at 440
7.3.4 Calibration Take a series of standard bismuth solutions
and the reagent blank. Using the same quantities of the reagents, carry
through the procedure as described under 7.3.2 and 7.3.3 and record
the photometric readings of the standard solutions along with the blank.
Correct for the blank and draw a calibration curve by plotting the pho-
tometric reading of the solutions against milligrams of bismuth per
ml of the solution.
7.4 Calculation-Convert the photometric reading of the sample solution
to milligrams of bismuth by means of a calibration curve and calculate
the percentage of bismuth as follows:
Bismuth, percent = A X1 10
where
A = weight in mg of the bismuth found in the aliquot of
the sample, and
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IS : 440 - 1964
B = weight in g of the sample represented by the aliquot
taken.

8. DETERMINA nON OF IRON

8.1 Outline of tbe Method - Iron in the solution of the sample is reduced
with stannous chloride, excess of which is destroyed by mercuric chloride.
The reduced iron is then titrated with standard potassium dichromate
solution using sodium diphenylamine sulphonate as indicator. Alterna-
tively, iron is det.ermined photometrically with thiocyanate solution and
measuring the absorbance at approximately 480 mP-.
8.2 Reagents
8.2.1 Dilute Nitric Acid - 1 : I and I : 99 (v/v).
8.2.2 Concentrated Nitric Acid - s~e 4.3.8.
8.2.3 Perchloric Acid - 70 percent.
8.2.4 Hydrobromic Acid -48 percent.
8.2.5 Concelltrated Ammonium Hydroxide - 20 percent.
8.2.6 Ammonium Chloride Solution -20 g per litre.
8.2.7 Dilute Hydrochloric Acid - I : I (v/v).
8.2.8 Stannous Chloride Solution - Dissolve, by heating, 60 g of pure
stannous chloride in a mixture of 400 ml of concentrated hydrochloric
acid and 600 ml of water until the solution is complete. Cool, add a few
pieces of granulated tin and preserve the solution in an air-tight amber-
cQioured .bottle to prevent oxidation.
8.2.9 Mercuric Chloride Solution - saturated.
8.2.10 Sulphuric Acid-Phosphoric Acid Mixture-Add slowly 150 ml
of concentrated sulphuric acid to 700 ml of water with continuous -stirr-
ing. Add to this 150 ml of syrupy phosphoric acid. Destroy any
oxidizable impurities by adding potassium permanganate solution (0'1 N)
drop by drop until the pink colour or permanganate persists, and cool the
solution.
8.2.11 Sodium Diphenylamine SuI phonate lnaicator Solution - Dissolve
0'32 g of barium diphenylamine sulphonate in 100 ml of hot water. Add
0'5 g of sodium sulphate, stir, and filter off the precipitate of barium
sulphate. Store in a dark-coloured bottle.
8~2.12 Standard Potassium Dichromate Solution - Dry pure potassium
dichromate in an oven at 105° to 110°C for one and a half hours.. Cool
in a desiccator and transfer exactly 0'490 4 g to a one-litre volumetric

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flask. Dissolve the salt in water and make up the volume to the
mark. Mix
8.2.13 Ammonium Thiocyanate Solution -Dissolve 10 g of ammonium
thiocyanate in water and dilute to one litre.
8.2.14 Standard Iron Solution ( 1 ml mg of Fe -Dissolve
1 g of ferric ammonium sulphate Fe ( NH, (SO,),. 6 in
5 ml of dilute nitric acid ( 1 1 Dilute to one litre in a volumetric
flask and mix.
8.3 Procedure By the Volumetric ) Method
8.3.1 Transfer of the accurately weighed sample, from which
extraneous iron has een removed, to a beaker. Add 50 ml of dilute
nitric acid ( 1 1 ) and heat to expel brown fumes. Dilute the solution to
100 ml with hot water and digest metastannic, if any, on a steam
bath. Filter through a close-textured paper into a beaker.
Wash with dilute nitric acid ( 1 : 99). Preserve the filtrate.
8.3.2 Transfer the paper and contents to the original beaker. Add
15 ml of concentrated nitric acid and 10 ml of perchloric acid. Heat
gently until white fumes appear. Cool and wash down the sides of the
beaker. Cover and add ml of hydrobromic acid. Remove the cover
and boil gently until white fumes appear. Repeat the hydrobromic acid
treatment to expel any traces of tin and antimony. Add
water to dissolve these soluble salts. Combine the solution with the fil-
trate preserved under 8.3.1.
8.3.3 Dilute the solution to 150 ml. Add concentrated ammonium
hydroxide solution until slightly but distinctly alkaline. Boil gently for
a few minutes. Allow the precipitate to settle for two minutes, filter
while hot. Wash the precipitate a few times alternately with ammonium
chloride solution and hot water to remove traces of the soluble salts.
8.3.4 Dissolve the precipitate on the filter paper with 20 ml of dilute
hydrochloric acid and wash thoroughly with hot water to remove
the last traces of iron. Collect the solution and the washings in
beaker in which precipitation was done. Reprecipitate iron and dissolve
it as before.
8.3.5 Concentrate the final solution to about 20 ml and heat to
boiling. To the boiling solution, add stannous chloride solution
wise with continuous stirring until the solution becomes Add
one drop of stannous chloride in excess. Dilute the solution to 50 ml and
cool to room temperature. Add IO ml of mercuric chloride solution in
one instalment. At this stage, silky white precipitate appears; if it fails to
appear or if a black precipitate appears, reject the test. If the precipi-
tate is too much, add further 5 ml of mercuric chloride solution.
for about 2 to 5 minutes and add 15 ml of sulphuric acid-phosphoric acid
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mixture and dilute to 100 ml. Add 3 to 4 drops of sodium diphenylamine

sulphonate indicator solution and titrate with standard dichromate
solution while stirring continuously until the green begins to
darken. Continue titration until a drop of dichromate solution produces
a suitable violet blue coloration.
8.3.6 Carry out a blank determination following the same procedure
and using the same amounts of all the reagents, but without the
sample.
Calculation
Iron, percent (A B)Cx
D
where
A volume in ml of the standard dichromate solution requir-
ed to titrate solution,
B volume in ml of the standard dichromate solution required
to titrate the blank,
normality of the standard dichromate solution, and
D = weight in g of the sample taken.
8.4 Procedure By the Ammonium ( Photometric ) Method
Weigh accurately about 10 g of the sample into a
tall-type beaker covered with a well-fitting cover glass and dissolve
by adding 100 ml of dilute nitric acid ( 1 1 Allow to stand on a hot
plate until all nitrous fumes are expelled. Dilute to approximately 300
ml with warm water and add concentrated ammonium hydroxide until
all basic salts have been dissolved. Bring to the boil carefully, place on
a hot plate and allow to stand for about one hour to affect coagulation
of iron hydroxide. Filter and wash several times with warm dilute
ammopium hydroxide.
Dissolve the precipitate back into the original beaker with 10 ml
of hot dilute hydrochloric acid, wash thoroughly with hot water, dilute to
approximately 300 ml with warm water. Add concentrated ammonium
hydroxide in slight excess to precipitate iron hydroxide, bring to the boil
carefully and place the beaker on a hot plate to allow the precipitate to
settle. Filter and wash well with hot water. Add 15 ml of hot dilute
hydrochloric acid to the same beaker in which the precipitate was made
to dissolve the adhering iron hydroxide. Pour the hot acid from beaker
through the filter paper into a beaker and wash the beaker and
filter paper carefully with hot distilled water. Cool the solution, transfer
to a graduated flask and make up to the mark with water.
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8.4.3 Transfer a suitable aliquot containing less than mg of iron

to a volumetric flask. Add sufficient dilute nitric acid ( 1 1 ) so
that its total content in the solution is 10 ml. Add one millilitre of
hydrogen peroxide and mix. Add ml of ammonium thiocyanate solu-
tion, dilute to the mark and mix *thoroughly.
8.4.4 Transfer a suitable portion of the solution to an absorption cell
and measure the absorbance at approximately 486
8.4.5 Calibration Curve Take a series of standard iron solutions and
the reagent blank. Using the same quantities of the reagents, follow the
procedure as under 8.4.3 and 8.4.4 and record the photometric readings
of the standard solutions along with the blank. Correct for the blank and
draw a calibration curve by plotting photometric readings of the solutions
against milligrams of iron per 100 ml of the solution.
8.4.6 Calculation -Convert the photometric reading of the sample
solution to milligrams of iron by means of calibration curve and calculate
the percentage of iron as follows:
Iron, percent = A X
where
A = weight in mg of iron found in the aliquot solution used,
and
B weight in g of the sample represented by the aliquot taken.
9. DETERMINATION OF LEAD THE COLORIMETRIC
METHOD
9.1 Outline of the Method Lead is deposited electrolytically from nitric
acid solution of the sample and estimated as sulphide.
9.2 Apparatus same as under 4.2.
9.3 Reagents
9.3.1 Dilute Nitric Acid : (
9.3.2 Hydrogen Peroxide Solution 3 percent.
9.3.3 Acidified Hydrogen Sulphide Solution Saturate dilute sulphuric
acid ( 1: 99 ) with hydrogen sulphide gas.
9.3.4 Ammonium Acetate Solution Dissolve 23 g of ammonium ace-
tate water and 3 ml of glacial acetic acid and dilute to ml
approximately 3 N
*The is for minutes, but be protected from direct sunlight.

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9.35 Sucrose Solution 50 percent ( w/v

93.6 Standard Lead Acetate Solution 1 ml I g of Pb )
Dissolve 1 g of lead acetate 3 in water
containing a little acetic acid, and dilute to one
9.4 Procedure
9.4.1 Transfer g of the accurately weighed sample into a
beaker, cover and dissolve in 60 ml of dilute nitric acid. When dis-
solution is complete boil gently to expel brown fumes. Wash down the
cover glass and the sides of the beaker and dilute to 250 ml.
9.4.2 Insert the electrodes into the solution, cover with a pair of split
glass and for two hours at a current density of to
with agitation of the electrolyte or run the electrolysis overnight at a
current density of Wash down the cover glass and sides of
the beaker. When the electrolysis is complete as indicated by absence of
darkening of the fresh anode surface, syphon off the electrolyte, at the
same time filling the beaker with water. Remove the anode quickly
and rinse thoroughly with water.
9.43 Dissolve the deposit of lead peroxide in 5 ml of dilute nitric acid
and few drops of hydrogen peroxide solution. Evaporate to dryness and
take up with water. Transfer to a volumetric flask and dilute
to the mark and mix well.
9.4.4 Pipette a suitable aliquot into a Nessler tube. Add
6 ml of ammonium acetate solution, 3 drops of dilute nitric acid, one
millilitte of sucrose solution and 6 ml of hydrogen sulphide
Make up the volume to 100 ml with water. Mix well and compare the
colour against series of solutions each containing measured volume
of the standard lead solution to which all the reagents have been added
in the same quantities as in the test solution. It is important to add
hydrogen sulphide solution simultaneously to the standard and the test
solutions.
9.5
Lead, percent = x
where
volume in ml of the standard lead solution required for
matching the colour of the test solution, and
B weight in g of the sample represented by the aliquot taken.
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10. DETERMINATION OF NICKEL BY THE

DIMETHYLGLYOXIME ( GRAVIMETRIC) METHOD
10.1 of the Method After the removal of copper, nickel is preci-
pitated with dimethlyglyoxime in alkaline medium, dried and weighed.
10.2 Reagents
10.2.1 Mixed Acids Pour 240 ml of concentrated sulphuric acid
(sp gr into 600 ml of water, cool and add 160 ml of concentrated
nitric acid ( sp gr 1.42
10.2.2 Tartatic Acid Solution-Dissolve 250 g of tartaric acid in
water and dilute to one litre.
10.23 Concentrated Ammonium Hydroxide 20 percent.
Dimethylglyoxime Solution Dissolve 10 g of dimethylglyoxime
in one litre of,rectified spirit, 95 percent j [conforming to IS 323-
1959 Specification for Rectified Spirit ( Revised) Filter before use.
10.3 Procedure-Weigh 5 g of the sample accurately and dissolve in 50 ml
of mixed acids, cool if necessary. When action has almost ceased, warm
to complete solution and to remove all nitrous fumes. Cool and dilute to
approximately 300 ml and remove the copper by electrolysis as under
Add 10 ml of tartaric acid solution. Neutralize with concentrated ammo-
nium hydroxide and add one millilitre excess. The solution should
remain clear after this treatment. Heat nearly to boiling and add with
stirring ml of dimethylglyoxime solution for each one milligram of
nickel present, then add 5 to 10 ml of the dimethylglyoxime solution in
excess, pouring directly into the solution and not down the beaker wall.
Stir the mixture vigorously and allow to cool to room temperature while
stirring occasionally. Filter through a sintered glass crucible and wash
well with hot water. Dry the precipitate at 110” to 120°C to constant
weight and weigh as nickel dimethylglyoxime.
10.4
Nickel, percent = x 2032
where
A weight in g of nickel dimethylglyoxime, and
B weight in g of the sample taken.
11. DETERMINATION OF SELENIUM BY THE GRAVJMETRIC
METHOD
11.1 of the Method Selenium and tellurium are separated from
copper by precipitation with ammonium hydroxide in presence of ferric
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iron. The precipitate is dissolved in hydrochloric acid and selenium

separated by sulphur dioxide, leaving tellurium in the filtrate.
11.2 Reagents
11.2.1 Concentrated Nitric Acid see 4.3.8.
11.23 Ferric Nitrate Solution see 4.3.4.
11.23 Concentrated Hydrochloric Acid see 5.3.2.
113.4 Concentrated Ammonium Hydroxide percent.
11.2.5 Dilute Ammonium Hydroxide 1 9 (
11.2.6 Dilute Hydrochloric Acid 1 1 (
11.2.7 Sulphur Dioxide Solution Pass sulphur dioxide gas in water
until saturated.
11.2.8 Rectified Spirit 95 percent ( v/v conforming to IS :
Specification for Rectified Spirit ( Revised)
11.3 Procedure
Take about 50 g of the accurately weighed sample in a large
beaker and dissolve in concentrated nitric acid avoiding excess as far as
possible. Add 5 to 10 ml of the ferric nitrate solution and evaporate to
expel most of the free acid. Dilute to 500 ml and treat the solution with
excess of concentrated ammonium hydroxide. Roil the solution for a
minute or two and allow to settle overnight. Filter off the hydroxide
precipitate and wash with dilute ammonium hydroxide.
Dissolve the precipitate on the filter paper in hot dilute hydro-
chloric acid and wash thoroughly with hot water. Add 200 ml of con-
centrated hydrochloric acid and cool to 20°C. Add 20 ml of sulphur
dioxide solution and allow to stand for 30 minutes. Filter through a
weighed sintered glass crucible ( porosity 4 ), wash with dilute hydrochloric
acid and then with cold water and rectified spirit. Preserve the filtrate
for tellurium determination (see 12). Dry the precipitate at 105 to
to constant weight and weigh as selenium metal.
11.4 Calculation
Selenium, = X 100
where
A weight in g of selenium, and
B weight in g of the sample taken.
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DETERMINATION OF TELLURIUM BY THE GRAVIMETRIC

METHOD
12.1 of the Method Tellurium is determined from the filtrate
from selenium determination, after dilution and adjustment of the acidity
of the solution and precipitation with sulphur dioxide.
12.2 Reagents
12.2.1 Tattaric Acid solid.
123.2 Concentrated Ammonium Hydroxide 20 percent.
Dioxide Solution saturated solution in water.
12.2.4 Hydrarine Hydrochloride Solution Dissolve 15 of hydrazine
hydrochloride in water and dilute to 100 ml.
123.5 Rectified Spirit see 11.2.8.
123.6 Carbon Dioxide gas.
12.3 Procedure -To the filtrate preserved under 113.2, add 2 g of tartaric
acid; dilute to with water and add 50 ml of concentrated ammo-
nium hydroxide.’ Add 20 ml of sulphur dioxide solution and then 10 ml of
hydrazine hydrochloride solution. Heat boiling and boil for two minutes.
Add 10 ml more of sulphur dioxide solution and allow to settle overnight.
Filter through a weighed glass crucible ( porosity 4 ); wash with
water and finally with rectified spirit. Dry to constant weight at
105 to 110°C to constant weight in an atmosphere of carbon dioxide and
weigh as tellurium metal.
12.4 Calculation
Tellurium, percent = x 100
where
A weight in g of tellurium, and
B weight in g of the sample taken for the test under 11.3.1.
13. DETERMINATION OF OXYGEN BY THE COMBUSTION
METHOD
13.1 Outline of the Method Oxygen is determined from the weight of
water formed on combustion in a current of hydrogen.
13.2 -The type of apparatus to be used is shown in Fig. 3.
13.2.1 Furnace-The furnace consists of a horizontal combustion tube
heated by electricity or gas. A combustion tube, 600 mm long and
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PLATINUM GAUZE

GLASS

or BY
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20 mm bore, made either of silica, quartz, or porcelain, glazed on

one or both sides, shall be used.
Hydrogen -Hydrogen may be obtained from hydrogen cylinder
or generated by the action of hydrochloric acid on zinc in Kipp’s
apparatus.
13.2.3 Hydrogen Purifier Hydrogen shall be free from oxygen and
moisture. ‘The gas is, therefore, first passed through wash bottles contain-
ing potassium hydroxide and sulphuric acid, and then through a silica
tube of mm bore containing platinum gauze, and maintained at a red
heat whereby water is formed if any oxygen is present. The water
formed is absorbed by passing through a U-tube containing phosphorus
pentoxide.
13.2.4 Absorption Tubes -The product of combustion, water, is
absorbed in a tared absorption tube containing phosphorus pentoxide to
which is connected a guard tube containing phosphorus pentoxide. The
phosphorus pentoxide tubes should be charged with alternate layers of
phosphorus pentoxide and glass wool, beginning and ending with the
latter. Phosphorus pentoxide, on absorbing water, tends to clog up
the absorption tube. To avoid this, and also to increase the efficiency
of the absorbent, use of small pumice stones (approximately 3 mm in
diameter ) shaken in phosphorus pentoxide are recommended.
13.3 Procedure Assemble apparatus as shown in Fig. 3 and test for
leaks. Pass hydrogen for 30 minutes. Weigh the tared absorption tube
( after bringing the hydrogen under atmospheric pressure by momen-
tarily opening the stopcock towards the guard tube ( Us) before
disconnecting the latter. Heat to the sample which has been
drilled with considerable care to avoid overheating and cool in a
desiccator. Place 50 g of the material in a large combustion boat and
insert it into the combustion tube. Pass hydrogen for 30 minutes, the
tube being cold. Connect the tared phosphorus pentoxide absorption
tube and the guard tube. Sweep out the air by passing hydrogen. for
30 minutes. Start the heating and bring the temperature to Pass
the current of hydrogen at the rate of about 100 ml per minute for
2 to 3 hours or until there is no further increase in the weight of the
tared absorption tube. Cool and weigh the absorption tube as before.
Calculation
Oxygen, percent (by weight ) = x
where
A weight in g of the absorption tube after test,
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IS: 1964
B = weight in g of the tared absorption tube in blank run,
and
C = weight in g of the sample taken.
14. DETERMINATION OF TIN BY THE IODIMETRIC METHOD
14.1 Outline of the Method Tin is collected and separated from copper
by precipitation with ammonium hydroxide in presence of iron. After
reduction of the solution, tin is determined iodimetrically.
14.2 Reagents
14.21 Concentrated Hydrochloric Acid see 53.2.
14.23 Dilute Nitric Acid 1 1 (
Ferric Nitrate Solution see 43.4.
143.4 Concentrated Ammonium Hydroxide 20 percent.
142.5 Ammonium Chloride Solution one percent (
Dilute Hydrochloric Acid 1 1 (
Chloride Dissolve 20 g of antimony
chloride in water and dilute to one
Test Lead
Nickel a roll of nickel sheet.
Carbon Dioxide gas.
14.2.11 Potassium Iodide Solution Dissolve 100 g of potassium
iodide in water and dilute to one litre.
Starch Solution see 5.3.14.
Standard Potassium Zodate Solution N. Twice recrys-
tallize potassium iodate from water and dry at 180°C to constant weight.
Dissolve 5 g of potassium iodate in 200 ml of water containing one
gram of sodium hydroxide and add 10 g of potassium iodide. When the
solution is complete, dilute to one litre in a volumetric flask. Standardize
the solution against pure tin following the procedure described under
143 Procedure
143.1 Take, in large akers, 100 g of the accurately weighed sample
in two g lots in the of copper with copper content more than
percent, and in one lot of 50 g of the sample in the case of copper
with copper content lower than percent. For each 50 g of the
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material, add 75 ml of water, ml of concentrated hydrochloric acid

and 150 ml of dilute nitric acid.
143.2 When the solution is complete, add 10 ml of ferric nitrate solu-
tion and boil for two minutes. Dilute to 400 ml with water and add
concentrated ammonium hydroxide until the precipitated copper hydroxide
is redissolved and the smell of ammonia persists. Heat to boiling and
allow to settle for one hour, Filter through a rapid filter paper and wash
with hot ammonium chloride solution. Dissolve the precipitate in
concentrated hydrochloric acid. Combine the solutions if the sample is
taken in more than one lot.
143.3 Reprecipitate with concentrated ammonium hydroxide, boil,
filter and wash thoroughly with hot ammonium chloride solution. Remove
the filter paper and the precipitate from the funnel and place it in a
Erlenmeyer flask. Add 200 ml of water to the flask containing
the filter paper and the precipitate. Add 75 of concentrated hydro-
chloric acid, two drops of antimony chloride solution and 5 of test lead
or the roll of sheet nickel and swirl the flask to break up the filter paper
and to aid in the solution of the precipitate. Stopper the flask with a
three-holed rubber stopper containing an inlet tube for carbon dioxide,
an air condenser, and a hole for the burette (glass plugged) (see Fig. 4).
During reduction a very slow stream of carbon dioxide shall he passed
through the flask. Heat the solution to boiling and boil with continuous
evolution of gas for at least 45 minutes.
143.4 After reduction is complete, cool the contents of the flask to
about maintaining an atmosphere of carbon dioxide by passing
carbon dioxide gas into the flask. Add 5 ml of potassium iodide solution
and 5 ml of starch solution and titrate with the standard potassium iodate
solution to a persistent blue
14.3.5 Carry out a blank determination, following the same procedure
and using the same quantities of all reagents but without the sample.
14.4
Tin, percent D
where
A = volume in ml of the standard iodate solution required for
the sample,
B = volume in ml of the standard iodate solution required for
the blank,
C tin equivalent of the standard potassium iodate solution
in g per ml, and
weight in of the sample taken.
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AP P A R A T U S FOB R EDUCTION
15. DETERMINATION OF PHOSPHORUS BY ALKALIMETRIC
METHOD
15.1 Outline 01 the Method The sample is dissolved in nitric acid and
phosphorus precipitated as ammonium phosphomolybdate, filtered
washed and dissolved in excess of standard alkali solution. The un
reacted alkali is back-titrated against standard acid.
15.2 Reagents
15.2.1 Concentrated Nitric Acid see 4.3.8.
15.2.2 Potassium Permanganate Solution 10 g per litre
15.2.3 Ammoniufn Nitrite Solution percent (
15.2.4 Ammonium Nitrate solid.
15.2.5 Ammonium Molybdate Solution Add solution
( 15.2.5.1) slowly and with constant stirring to solution
(see ) kept cool in a cold water-bath. Add 10 ml of ammonium
phosphate (one gram per litre ) and keep the solution at least for
24 hours. Filter the solution through filter paper No. before use.
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IS
15.2.5.1 Solution ( A Dissolve 100 of molybdic acid (
85 percent) or g of ammonium molybdate in a mixture of ml of
concentrated ammonium hydroxide and 270 ml Cool the
solution.
15.2.5.2 Solution ( B 490 ml of concentrated nitric acid to
ml of water and cool.
15.2.6 Potassium Nitrate Wash 10 per litre (
Indicator Solution-Dissolve g of
phenolphthalein in 100 ml of 60 percent alcohol.
15.2.8 Sodium Hydroxide Solution N approximately.
15.2.9 Standard Hydrochloric Solution N. Dilute 16
concentrated hydrochloric acid to one litre and standardize against
sodium carbonate.
15.3 Procedure
15.3.1 Transfer one to five grams of the accurately weighed sample,
preferably containing 5 mg of phosphorus, to a Erlynmeyer flask
and dissolve in concentrated nitric acid using 5 ml for each gram of the
sampla. Heat gently to expel brown fumes and add 100 ml of water.
Heat the solution and add potassium permanganate solution
until a deep purple colour persists. Boil for 5 minutes, destroy the excess
of potassium permanganate and manganese dioxide by adding ammonium
nitrite solution until the solution is blue in colour. Boil for
5 minutes.
156.2 the solution to 45°C and add 5 g of ammonium nitrate.
Add 60 ml of ammonium molybdate solution in small portions while
shaking the flask. Close the flask and shake vigorously for 5 minutes
and keep it at 50 to 60°C for one hour. Filter the precipitate through a
thick filter paper pulp prepared on a disc in a funnel. Wash the preci-
pitate two to three times with dilute nitric acid, then with potassium
nitrate wash solution until 10 ml of the filtrate in a test tube
does not consume more than one drop of sodium hydroxide solution
(begin testing from the third wash
Transfer the filter paper and the precipitate to the flask, add
ml of water, stopper it and shake vigorously until the filter paper is
disintegrated. Wash down the add 3 to 4 drops of
indicator solution and while shaking the flask’ from the
standard sodium hydroxide solution until pink persists.
Add 2 ml in excess. Dilute with about ml of and titrate with
hydrochloric to the of the
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Carry out a blank determination following the same procedure

and using the same quantity of standard sodium hydroxide solution
which was added in the test, and titrate with standard hydrochloric acid
using 3 to 4 drops of phenolphthalein indicator solution.
19.4 Calculation
Phosphorus, percent = ( A D
c x

where
volume in ml of the standard hydrochloric acid required
for the blank test,
volume in ml of the standard hydrochloric acid required
for the sample,
normality of the standard hydrochloric acid, and
weight in g of the sample taken.

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