Chemical Analysis of Aluminium and Its Alloys: Indian Standard

Free Standard provided by BIS via BSB Edge Private Limited to Swaptul Enterprises -
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(Reaffirmed 2013)

IS 504 (Parts 1 to 12): 2002
(Reaffirmed 2012)
(Reaffirmed 2018)

(Reaffirmed 2011)
(Reaffirmed 2010)
(Reaffirmed 2009)
Indian Standard
CHEMICAL ANALYSIS OF (Reaffirmed 2008)
ALUMINIUM AND ITS ALLOYS

PARTS 1 TO 12
(Reaffirmed 2007)
(Second Revision )

(Reaffirmed 2006)
ICS 77.120.10
(Reaffirmed 2005)
0 BIS 2002
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
June 2002 Price Group 11
-,
Methods of Chemical/ Instrumental Analysis of Non-Ferrous Metals Sectional Committee, MTD 28
FOREWORD
This Indian Standard (Parts 1 to 12) (Second Revision) was adopted by the Bureau of Indian Standards, after
the draft finalized by the Methods of Chemical/Instrumental Anaylsis of Non-Ferrous Metals Sectional Committee
had been approved by the Metallurgical Engineering Division Council.
This standard was first published in 1954 and subsequently revised in 1963. This revision of the standard
covers following parts:
Part 1 Determination of Silicon and Lead
Part 2 Determination of Iron
Part 3 Determination of Copper
Part 4 Determination of Zinc
Part 5 Determination of Manganese
Part 6 Determination of Magnesium
Part 7 Determination of Nickel
Part 8 Determination of Chromium
Part 9 Determination of Tin
Part 10 Determination of Antimony
Part 11 Determination of Titanium
Part 12 Determination of Vanadium
‘ihe main changes in this revision from its earlier version are as below:
Part 1 The spectrophotometric method for determination of silicon up to 0.1 percent has been incorporated
and determination of lead by the sulphide method has been updated.
Part 4 Determination of zinc by dithizone photometric method and by ‘Mercuric thiocyanate method’
have been updated.
Part 5 Determination of manganese in the range of 0.01 to 0.10 percent by periodate (photometric)
method and up to 0,5 percent by persulphate method have been deleted.
Part 6 EDTA method for determination of magnesium in the range 0.5 to 11 percent has been deleted.
Part 8 Determination of chromium by perstdphate oxidation method has been incorporated.
Part 11 Spectrophotometric method for determination of titanium in the range 0.001 to 1.0 percent using
diantipyrylmethane has been incorporated as an alternate method.
Part 12 Determination of vanadium in the range 0.005 to 0.02 percent using N- cinnamoyl- N- phenyl-
hydroxamic acid (spectrophotometric) method has been incorporated as new part which was not
covered in the standard earlier.
The standard although revised in parts is being printed in as a single publication for the convenience of users.
Parts 13 to 16 covering Determination of Sodium, Berillium, Zirconium and Lithium are under preparation and
shall be printed as soon as finalized
The composition of the Committee responsible for the formulation of this standard is given in Annex A.
In reporting the result 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 ‘Rules for rounding off numerical
values (revised)’.
IS 504 (part 1) :2002
Indian Standard
CHEMICAL ANALYSIS OF
PART 1 DETERMINATION OF SILICON AND LEAD
(Second llevision)
1 SCOPE 5 DETERMINATION OF SILICON IN
ALUMINIUM METAL BY SPECTRO-
1.1 This standard (Part 1) describes the following PHOTOMETRIC METHOD
methods for determination of different ranges of silicon
in aluminium and its alloys. 5.1 Outline of the Method
Range Method The silicon in the sample solution is converted to
(Percent by mass) silicomolybdate complex, and subsequently reduced
by ascorbic acid. The spectrophotometric measurement
Uptoo.lo Spectrophotometric method is made at 815 nm.
0.02-0.03 Molybdenum yellow
5.2 Reagents
(photometric method)
0.3 and above Gravimetric method 5.2.1 Sodium Hydroxide Solution (15 percent)
1.2 It also describes the method for determination of Dissolve 15 g of sodium hydroxide pellets in 100 ml
distilled water. Store in a plastic container.
lead by the sulphide calorimetric method.
5.2.2 Dilute Nitric Acid (BN)
2 REFERENCES
To 493 ml of distilled water slowly add 507 ml of
The Indian Standards listed below contain provisions nitric acid and stir to mix completely.
which through reference in this text, constitute
5.2.3 Ammonium Molybdate Solution (14.5 percent)
provisions of this standard. At the time of publication,
the editions indicated were valid. All standards are Dissolve 14.5 g of ammonium molybdate in 100 ml
subject to revision, and parties to agreements based water and store in a plastic container.
on this standard are encouraged to investigate the
5.2.4 Tartaric Acid Solution (10 percent)
possibility of applying the most recent editions of the
standards indicated below: Dissolve 10 g of tartaric acid in 100 ml distilled water
and store in a plastic container.
IS No. Title
5.2.5 Dilute Sulphuric Acid (16 N)
264:1976 Nitric acid (second revision)
265:1993 Hydrochloric acid ~ourth revision) To 566 ml of distilled water, slowly and 434 ml of
sulphuric acid with constant stirring and cooling under
266:1993 Sulphuric acid (third revision)
tap water.
1070:1992 Reagent grade water (third revision)
1817:1961 Methods of sampling of non~ferrous 5.2.6 Ascorbic Acid Solution (2 percent)
metals for chemical analysis
Take 2 g of ascorbic acid and dissolve it in 100 ml
3 SAMPLING distilled water. Store in a plastic container. Always
use a freshly prepared solution.
The sample shall be drawn and prepared in accordance
with the method prescribed in IS 1817. 5.2.7 A[uminium Solution for Matrix Correction
4 QUALITY OF REAGENTS Take 1000 g aluminium wire of purity 99.9 percent

minimum, and dissolve in 20 ml of sodium hydroxide
Unless specified otherwise, analytical grade reagents and extract the content in 50 ml of nitric acid (8 N).
and reagent grade water (see IS 1070) shall be Make up the volume to 250 ml. Store in a plastic
employed for the test. container.
1
.,
Free Standard provided by BIS via BSB Edge Private Limited to Swaptul Enterprises - —A
-a
1S 504 (Part 1) :2002
5,2.8 Standard Silicon Solution A (100 mg/1) 5.3.5.2 Draw the calibration curve by plotting the
concentration of the 5 standard solutions of silicon vs
Fuse 0.214 g of anhydrous silica with 2 g of sodium absorbance.
carbonate in platinum crucible. Cool the melt, dissolve
completely in water and dilute to 1 000 ml in a volu- 5.4 Calculation
metric flask . Store the solution in a polyethylene
bottle. M X 250
Silicon, percent by mass =
m
5.2.9 Standard Silicon Solution B (1O mgll)
where
Transfer 10 ml of solution A (5.2.8) to a 100 ml volu-
J,f. mass, in mg/ml of the sample found in
metric flask and make up the volume with distilled
water. aliquot taken from the calibration curve,
and
5.3 Procedure m= mass, in g of the sample taken.
5.3.1 Weigh accurately 1000 g of sample and transfer 6 DETERMINATION OF SILICON BY THE
to a cleaned nickel crucible or teflon/stainless steel MOLYBDENUM YELLOW SPECTRO-PHOTO-
beaker of 100 ml capacity. Add 20 ml of sodium METRIC METHOD (FOR SILICON CONTENT
hydroxide (15 percent) and cover the crucible by a lid BETWEEN 0.02 TO 0.3 PERCENT)
with a slight opening. Wait for 5 to 10 min and open
the lid. If some of the portion remain undissolved then 6.1 Outline of the Method
heat slowly to dissolve all.
The sample is dissolved in sodium hydroxide and the
5.3.2 Carefully pour the contents to a beaker solution acidified with nitric acid. The orthosilicic acid
containing 50 ml of nitric acid (8 N) and transfer the formed is converted to yellow silicomolybdic acid by
washings of the crucible with hot water in to the same the addition of ammonium molybdate to the solution.
beaker. Heat slowly over a hot plate until all the salts Spectrophotometric measurement of the yellow com-
get dissolved. Cool, transfer the solution to a 250 ml plex is then made at about 400 nm.
Polyethylene volumetric flask with the washings of
the beaker with distilled water, and make up to the 6.2 Reagents
mark with distilled water.
6.2.1 Sodium Hydroxide Solution — 40 percent (m/v) ---
5.3.3 Take 10 ml of sample solution in 100 ml beaker.
Weigh 40 g of sodium hydroxide pellets in a plastic,
5.3.4 Add 10 ml of ammonium molybdate solution polyethylene or stainless steel beaker and add 100 ml
(5.2.3). Wait for 10 min to complete the reaction. Check of water. Stir with a plastic rod until entire mass dis-
the pH of the solution and bring it to 0.85-0,90 by solves. Cool and store in a plastic or polythene bottle.
dropwise addition of dilute nitric acid. Transfer the
solution to a 100 ml volumetric flask with the washings 6.2.2 Dilute Nitric Acid —1: 1 (v/v).
of the beaker with distilled water. To it add 5 ml of

6.2.3 Ammonium Molybdate Solution — 10 percent (m/v)
tartaric acid and shake gently for mixing. Add 11 ml of
sulphuric acid(16N). Cool the solution under tap water Dissolve 100 g of ammonium molybdate in water and
to 25-30”C. Add 2 ml of freshly prepared ascorbic acid dilute to one Iitre. Filter before use.
solution and make up the volume with distilled water.
Note the time. Measure the absorbance/concentration 6.2.4 Standard Silicon Solution (1 ml – 0.05 mg of Si)
at 815 nm after 10 min but not beyond 30 min.
Fuse 0.107 g of anhydrous silica with 1.0 g of sodium
5.3.5 Find the concentration of the sample solution carbonate in a platinum crucible. Cool the melt, dissolve
from the calibration curve and calculate the percentage completely in water, and dilute to one Iitre in a volumet-
of silicon as given in 5.4. ric flask. Store the solution in a polyethylene bottle.
5.3.5.1 Calibration curve NOTE — In case anhydrous silica k not available, adjust the
weight of sil ica used according to the actual silicon content of the
Take six No. 100-ml beaker and use one of them as sample.
blank. To each of it add 10 ml of aluminium solution

6.3 Procedure
for matrix correction. Serially add 1,2,3,4 and 5 ml
of standard silicon solution B (5.2.9) and follow rest 6.3.1 Transfer 0.5 g of the accurately weighed sample
of the procedure as specified in 5.3.4. to a 250 ml stainless steel or nickel beaker. Add 10 ml
2
Ja
1S 504 (Part 1) :2002

J,l
“i
of sodium hydroxide solution by means of a pipette. A = mass in mg of silicon found in the aliquot
Cover the beaker and warm it to start the reaction. solution, and
When the reaction subsides, wash the walls of the B = mass in g of the sample represented by
beaker and cover. Heat to complete the dissolution and the aliquot taken.
boil for a few minutes. In case of alloys containing
NOTE — In case of high manganese alloys, the solution after
magnesium, concentrate the solution by boiling to addition of nitric acid maybe coloured brownish yellow. If so,
ensure complete conversion of magnesium silicide to bleach the colour by dropwise addition of saturated solution of
sodium silicate. Dilute the solution by washing the sodium sulphk to the hot solution. Then add sufficient potassium
perrnanganate solution (O. 1 N) until a pink colour is obtained.
walls of the beaker and the cover with water. Cool
Add finally just enough oxalic acid solution (one percent, ndv) to
and transfer the contents of the beaker to a Pyrex destroy the pink colour.
beaker containing 25 to 30 ml of dilute nitric acid
(measured accurately). Transfer the contents of the 7 DETERMINATION OF SILICON BY THE
metallic beaker completely to the glass beaker with a GRAVIMETRIC METHOD (FOR SILICON
jet of water. Wash the metallic beaker three or four CONTENT OVER 0.3 PERCENT)
times with hot water, using a small quantity at a time,
and transfer the washings to the glass beaker. Shake 7.1 Outline of the Method
the contents of the beaker well and boil until the Silicon is converted to sodium silicate by alkaline
solution becomes clear (avoid excess boiling). Cool attack. After acidification and removal of interfering
the solution. elements, silica is determined by hydrofluorization of
the residue.
6.3.2 Filter the solution through medium textured
filter paper into a 250 ml volumetric flask. Wash the 7.2 Reagents
beaker 5 or 6 times with hot water. Dilute the solution
to about 220 ml. Cool to room temperature, add 10 to 7.2.1 Sodium Hydroxide Solution — 50 percent (m/v).
25 ml of ammonium molybdate solution and make up 7.2.2 Hydrogen Peroxide,— 20 volumes.
the volume to the mark. Shake the flask well. Allow
the solution to stand for 15 min to develop the yellow 7.2.3 Sulphuric Acid — rd. = 1.84.
colour fully.
7.2.4 Sulphuric Acid — Perchloric Acid Mixture
6.3.3 Transfer a suitable portion of the solution to an
Add 624 ml of sulphuric acid (rd. = 1.84) and 85 ml
absorption cell (4 cm) and adjust the spectro-
of perchloric acid (70 percent) to 315 ml of water. ..-
photometer to the initial setting. Take the spectro-
Mix and make up to 1 Iitre.
photometric readings within ten minutes of the
development of colour, using a light filter at 7.2.5 Perchloric Acid Solution
approximately 400 nm.
Add 600 ml of perchloric acid (70 percent) to 400 ml
6.3.4 Calibration Curve of water and mix.
Take a series of standard silicon solutions and a 7.2.6 Nitric Acid — rd. = 1.42.
reagent blank. Using same quantities of reagents,
7.2.7 Sulphurous Acid — Saturate water with sulphur
carry through all the stages as described under
dioxide gas. Prepare fresh as needed.
6.3.2 and 6.3.3 and record the spectrophotometric
readings of all the standard solutions along with 7.2.8 Sulphurous Acid — 1:1, 1:3, and :99 (v/v).
the blank. Draw a calibration curve by plotting the
spectrophotometric readings of the standard 7.2.9 Hydrochloric Acid — rd. 1.16,
solution against milligrams of silicon per 100 ml 7.2.10 Ammonium Acetate Solution
of the solution.
Dissolve 25 g of ammonium acetate in d stilled water
6.3.5 Convert the spectrophotometric readings of the containing 1 ml of glacial acetic acid and make up to
sample to milligrams of silicon by means of calibration 100 ml with water.
curve, and calculate the percentage of silicon as given
in 6.4. 7.2.11 Dilute Hydrochloric Ac;d — 1:99 (vIv).
7.2.12 HydrojZuoric Acid (40 percent)

6.4 Calculation
NOTE — Hydrofluoric acid is extremely irritating and corrosive
to skin and mucous membrane and produces severe skin bums
Silicon, percent by mass = ~ x + which are slow to heal. in case of contact with skin, wash well
with water and seek medical help immediately.
3
IS 504 (Part 1) :2002
7.3 Procedure lead retained in the residue may be removed as

under 7.3.5.1.
7.3.1 Depending upon the silicon content of the
sample, adjust the weight of the sample to be taken 7.3.5.1 Afier fuming (see 7.3.3) take up the sample
for analysis as given below. Accurately weigh the with 5 ml of hydrochloric acid and 100 ml of hot water.
sample and transfer it to a stainless steel beaker or a Filter and wash with hot dilute hydrochloric acid. The
nickel beaker: analyst may select the method for lead separation that
best suits his plan for using the filtrate in subsequent
Silicon Content Mass in g of the Sample
analysis.
Percent to be Taken “.
7.3.6 Moisten the residue with a few drops of water,
Over 0.3 up to 1 2
then add 5 to 10 drops of dilute sulphuric acid (1:1)
Over 1 up to 3 1 and a few millilitres of hydrofluoric acid. Evaporate
Over 3 up to 7 0.5 to dryness, ignite at 900”C, cool and weigh. Repeat
Over 7 0.25 the treatment with hydrofluoric acid and ignite to
7.3.2 Add 12 ml of sodium hydroxide solution per constant weight. The loss in weight represents silica.
gram of the sample taken. When the reaction is 7.3.7 Make a blank determination, following the same
complete, wash down the cover and sides of the vessel procedure and using the same amounts of all reagents,
with small jet of hot water. Keep the volume of the but without the sample.
solution as low as possible. Place on the hot plate and
evaporate cautiously to syrupy consistency. Add 7.4 Calculation
hydrogen peroxide dropwise (about 30 drops) and
A-B
repeat the evaporation. Add more hydrogen peroxide Total silicon, percent = — X 46.72
dropwise until the solution is completely oxidized. c
where /
Remove the vessel from hot plate, cool, wash the sides
with 10 ml of sulphuric acid — perchloric acid A = mass in g, of silica as obtained in 7.3.6
mixture. Rinse the nickel vessel, first with hot water from the difference in weight before and
and then with a few mil Iilitres of perch loric acid after HF treatment;
solution to which an equal volume of water has been B = massing, of silica obtained in the blank;
added. Clean the vessel thoroughly by means of a and
rubber-tipped glass rod and finally rinse with hot C = mass in g, of the sample taken.
water. -----
8 DETERMINATION OF LEAD BY THE
7.3.3 Add 5 ml of nitric acid and few ml of sulphurous SULPHIDE (CALORIMETRIC) METHOD
acid to the solution, evaporate to dense white fumes,
cover, fume for 15 min and cool. Add 100 ml of water 8.1 Outline of the Method
and 10 ml of dilute sulphuric acid ( 1:3). Stir well and
Lead is determined calorimetrically from the
heat until the soluble salts are dissolved. If manganese,
ammonium acetate extract obtained after silicon
dioxide is present, bring it into solution with a few
determination.
drops of hydrogen peroxide or sulphurous acid.
7.3.4 Add paper pulp, and filter on a low ash medium 8.2 Reagents
textures paper. Remove all silica from the beaker by 8.2.1 Dilute Nitric Acid — 1:1 (vIv).
means of rubber tipped glass rod and wash the paper
and contents thoroughly with dilute sulphuric acid 8.2.2 Sucrose Solution — 100 percent (m/v).
(1: 99). Recover silica from the filtrate by evaporating
the filtrate, fuming and proceeding as under 7.3.3. 8.2.3 Hydrogen Sulphide Solution
Add the recovered silica to the main silica residue. Saturate dilute sulphuric acid (1:99) with hydrogen
Place the papers and precipitate in a platinum crucible, sulphide gas.
dry and ignite slowly at 500”C until free of carbon,
then heat at 900 to 950”C for 25 min. Cool in a 8.2.4 Standard Lead Solution (1ml=0.0001 g of Pb)
desiccator, weigh and again ignite at the same
Dissolve 0.183 1.g of lead acetate crystals
temperature as a check for constant mass.
[pb (CHJC02)2.3HzO] in water containing a little
7.3.5 If lead is present, wash the main silica residue acetic acid and dilute to one litre.
(see 7.3.4) with hot ammonium acetate solution and
preserve the ammonium acetate extract separately 8.3 Procedure
for determination of lead (see 8). Alternatively and Transfer the ammonium acetate extract preserved
4
IS 504 (Part 1) :2002
under 7.3.5 to a 100 ml Nessler tube. Add water to 8.4 Calculation !4

make the solution to 90 ml. Add 3 drops of dilute
M X 0.1
,.
nitric acid, one millilitre of sucrose solution and 5 ml Lead, percent by mass= —
of hydrogen sulphide solution. Make up the volume m
to 100 ml with water, and mix well. Compare the where
intensity of colour with those of series of standard
solutions each containing same quantities of all the M = mass in mg of lead found in the sample,
reagents as were added in the test solution. It is and
important to add hydrogen, sulphide solution, m = mass in g of the sample taken.
simultaneously to the standard and test solutions.
IS 504 (Part 2) :2002
Indian Standard
PART 2 DETERMINATION OF IRON
(Second Revision)
1 SCOPE 5.2 Reagents
This standard (Part 2) describes the O-phenanthroline 5.2.1 Hydroxylawnonium Chloride Solution (1 O percent)
(Spectrophotometric) method of determination of iron
up to 0.1 percent and (titrimetric) method above Dissolve 10 g hydroxylammonium chloride in 100 ml
0.1 percent in aluminium and its alloys. of distilled water. Store in a plastic container.
2 REFERENCES 5.2.21-10 Phenanthroline Solution (0.25 percent)
The Indian Standards listed below contain provisions Dissolve 0.25 g of 1-10 phenanthroline in minimum
which through reference in this text, constitute amount of ethyl alcohol and make the total volume to
provisions of this standard. At the time of publication, 100 ml with distilled water. Store in a plastic container.
the editions indicated were valid. All standards are
subject to revision, and parties to agreements based 5.2.3 Buffer Solution
on this standard are encouraged to investigate the 5.2.3.1 Dissolve 272 g of sodium acetate in 500 ml of
possibility of applying the most recent editions of the water. Add 240 ml of acetic acid. Make up the total
standards indicated below : volume to 1 000 ml by distilled water. Store in a plastic
IS No. Title container.
10.70:1992 Reagent grade water (third revision) 5.2.3.2 Sodium hydroxide solution (15 percent)
1817:1961 Methods of sampling of non-ferrous
metals for chemical analysis Dissolve 15g of sodium hydroxide pellets in distilled .- --
water. Cool and make up to 100 ml. Store in
3 SAMPLING
polyethylene container.
with the method prescribed in IS 1817. 5.2.4 Aluminium Solution for Matrix Correction
Dissolve 1 000 g of aluminium metal (purity

4 QUALITY OF REAGENTS
9,9.99 percent) in 20 ml of sodium hydroxide (15
Unless specified otherwise, analytical grade reagents percent) and extract the content in 50 ml of 8N nitric
and reagent grade water (see 1S 1070) shall be acid. Make up the volume to 250 ml. Store in a plastic
employed for the test. container.
5 DETERMINATION OF IRON BY 5.2.5 Stock Iron Solution (1 000 mg/1)

THE O-PHENANTHROLINE (SPECTRO-
PHOTOMETRIC) METHOD (FOR IRON Dissolve lg of pure iron (99.99 percent) in 1:1
CONTENT BETWEEN 0.03 TO 0.10 hydrochloric acid and make up to one litre.
PERCENT) 5.2.5.1 Standard iron solution A (100 mg/1)
5.1 Outline of the Method
Using a pipette transfer 10 ml of the stock iron solution
All the trivalent iron in the sample solution is reduced (1 000 ppm) to a 100 ml volumetric flask and make
by hydroxylammoniurn chloride to give bivalent iron, up the volume with distilled water.
which is complexed with 1-10 phenanthroline. The
complex gives an orange red coloration in acetate 5.2.5.2 Standard iron solution B (10 mgtl)
buffer at pH 3.5 to 4.2.
Pipette out 10 ml of standard iron solution (5.2.5.1)
The intensity of the colour is measured at 510 nm to a 100 ml volumetric flask and makeup the volume
spectrophotometrical ly. to 100 ml with water.
6
1S 504 (Part 2) :2002
5.3 Procedure complete mixing. It is desirable to add a small volume

of H2SOdwhile preparing the solution.
5.3.1 Follow the procedure specified in 5.2.1 to 5.3.3
of Part 1 for preparation of sample solution. 6.2.3 Stannous Chloride Solution ( 10 percent)
5.3.2 Add 5 ml of hydroxylammonium chloride solu- Dissolve 10 g of stannous chloride in 10 ml of hydro-
tion and 5 ml of 1:10 phenanthroline solution and chloric acid by heating over a hot plate. Cool it and
homogenize. Add 15 ml of the acetate buffer and make make up the volume to 100 ml with water. Store it in
up the volume to 100 ml and homogenize. Measure a plastic dropping bottle.
the absorbance at510 nm by a spectrophotometer using
6.2.4 Mercuric Chloride Solution (Saturated
suitably prepared reagent blank.
Prepare a saturated solution of mercuric chloride with
5.3.3 Find the concentration of the sample solution
distilled water and store in a plastic container.
from the calibration curve and calculate the percentage
of iron as given in 5.3.5. NOTE — Mercury and its compounds are highly poisonous, Take
proper precautions while handling and disposing off them.
5.3.4 Calibration Curve
6.2.5 Sodium Diphenylamine Sulphonate Solution
In a series of six volumetric flasks, add 1,2,3,4 and (0.20 percent)
5 ml of standard iron solution B to obtain 0.1, 0.2,
0.3, 0.4 and 0.5 mg/1 of iron respectively. Use flask Dissolve 0.2 g of sodium diphenylamine sulphonate
numbered ‘O‘ for reagent blank. Follow rest of the in 100 ml of distilled water and store it in a dropping
procedure as specified in 5.3.2. bottle.
5.3.5 Calculation 6.2.6 Phosphoric-Sulphuric Acid Mixture
In a cleaned 1-Iitre beaker take 500 ml of distilled

M X 250
Iron, percent by mass = water. Add 250 ml of sulphuric acid slowly with
m constant stirring and cooling under tap water. To the
where cooled solution add 250 ml of phosphoric acid and
homogenize.
M= mass in mg/ml of sample found (in aliquot
taken) from the calibration curve, and 6.3 Procedure
m= mass in g, of the sample taken.
6.3.1 Take 1000 g of sample drillings in a cleaned
6 DETERMINATION OF IRON BY POTASSIUM 500 ml conical flask. Add 50 ml of acid mixture and
BICHROMATE (TITRIMETRIC) METHOD wait until the reaction is complete and the solution is
(FOR IRON CONTENT >0.10 PERCENT) clear. If some metal drillings remain unreacted, then
heat gently over a hot plate until al}the sample goes
6.1 Outline of the Method into the solution.
All the iron present in the sample is brought to solution NOTE — If the colour of the solution is yellow then heat it over
by dissolving it in acid mixture. The trivalent iron if a hot plate and decolourize it with dropwise addition ofstannous
chloride solution. Adjust sufficient and do not add in excess,
present, is reduced to bivalent by stannous chloride.
The entire iron is oxidized by potassium bichromate. 6.3.2 Cool it immediately under tap water to room
temperature. Add 10 ml of saturated solution of
6.2 Reagents
mercuric chloride at a time to it and shake gently.
6.2.1 Acid Mixture Silky white precipitate would appear. If it is black in
colour, discard the solution and repeat the procedure
In a cleaned 2-litre glass beaker, take 1000 ml from the beginning.
distilled water. To it add 450 ml of sulphuric acid
slowly with constant stirring and cooling under tap 6.3.3 Add 10 ml of phosphoric–sulphuric acid mixture
water. To the solution add 550 ml of hydrochloric acid and 5-6 drops of sodium diphenylamine sulphonate
slowly and stir to mix it completely. indicator. Titrate against potassium bichromate
solution to a suitable violet coloration.
6.2.2 Potassium Bichromate Solution (N155.85)
7 STANDARDIZATION OF POTASSIUM
Take 1.7558 g of dried (at 110”C for 1 h) potassium
BICHROMATE SOLUTION
bichromate and transfer it carefully to a 2-litre
volumetric flask. Add 300 ml of water to it and shake Take 10 ml of standard iron solution 1000 mg/1 add
until all the crystals dissolve. Then make up the 50 ml of acid mixture and heat it. If the colour is
volume with water and shake the entire solution for yellow, then decolourize as described above. Add
7
1S 504( Part 2):2002
10 ml phosphoric–sulphuric acid mixture and 5-8 where

drops of sodium diphenylamine sulphonate indicator.
v = the volume of bichromate consumed in ml.
Titrate against potassium bichromate solution to
1000 ml of N/55.85 K, CrJ 07 = lg of iron
a stable violet coloration.
If the factor is 1.0 then
If the potassium dichrornate solution is exactly N/55.85
then 10 ml of the 1 000 mg/1 iron solution will con- Percent, iron mlof bichromate consumed
sume 10 ml of the potassium bichromate solution. in sample = Xloo
1 OOOxmassof sample
If the potassium bichromate solution is not exactly
N/55.85 then tind out the factor (F) as follows: otherwise
10ml ml~f bichromate consumed x FX 100”

F. — pCXCeIlt, kOIl
v in sample = 1 OOOxmassofsample
IS 504(Part 3):2002
,{
Indian Standard i
PART 3 DETERMINATION OF COPPER
(Second Revision )
1 SCOPE to 600 ml of water, cool and add 300 ml ofhydrochlo-
ric acid (rd. = 1.16) and 300 ml of nitric acid.
This standard (Part 3) describes the methods for
determination of copper up to 0.1 percent by the 5.2.2 Dilute Sulphuric Acid — I: 1, 1:99 (v/v).
Diethyl-dithiocarbarnate (spectrophotometric) method
5.2.3 Hvdroj7uoric Acid (40 percent)
and above 0.1 percent by the iodimetric method in
aluminium and its alloys. 5.2.4 Hydrogen Sr.dphide — Gas.
2 REFERENCES 5.2.5 Hydrogen Sulphide Wash Solution
The following Indian Standards are necessary adjuncts Pass hydrogen sulphide gas through dilute sulphuric
to this standard: acid (1 :99) to obtain a saturated solution for the
existing.
1SNo. Title
5.2.6 Dilute Nitric Acid — 1:2 (v/v).
264:1976 Nitric acid (second revision)
265:1993 Hydrochloric acid ~ourth revision) 5.2.7 Ammonium Hydroxide (20 percent)
266:1993 Sulphuric acid (third revision) 5.2.8 Dilute Ammonium Hydroxide Wash Solution —
1070:1992 Reagent grade water (third revision) 1:20 (v/v).
metals for chemical analysis 5.2.9 Citric Acid Solution — 20 percent (m/v).
3 SAMPLING 5.2.10 Sodium Diethyl-Dithiocarbamate Solution —
0.1 percent (m/v).
The sample shall be drawn and prepared in accordance ----
with the method prescribed in 1S 1817. 5.2.11 Carbon Tetrachloride
4 QUALITY OF REAGENTS 5.2.12 Sodium Sulphate — Solid.
Unless specified otherwise, analytical grade reagents 5.2.13 Standard Copper Solution ( 1 ml = 0.01 mg
and reagent grade water (see IS 1070) shall be of Cu).
employed for the test. Dissolve one gram of electrolytic copper in 10 ml of
dilute nitric acid (1: 1) evaporate nearly to dryness and
5 DETERMINATION OF COPPER BY THE
dilute to 1000 ml in a volumetric flask. Pipette 10 ml
DIETHYL-DITHIOCARBAMATE (SPECTRO-
from this solution and dilute to one Iitre.
PHOTOMETRIC) METHOD (FOR COPPER
CONTENT UP TO 0.1 PERCENT) 5.3 Procedure
5.3.1 Weigh accurately 2 g of sample and transfer to a
The sample is treated with mixed acids and the sili- 400 ml beaker, Add 10 ml of the mixed acids and
con removed. Copper is precipitated as sulphide from after the reaction has subsided, add 60 ml more. Add
the acid solution of the sample and any copper left in 20 ml of dilute sulphuric acid (1:1) and evaporate the
the residue is also recovered. The copper is dissolved solution to fumes. Continue fuming for ten minutes.
in nitric acid, complexed with diethyl-dithiocarbamate Cool, dilute to 200 ml and boil until soluble salts are
and determined spectrophotometrically at approxi- dissolved, filter the insoluble matter on a paper pulp
mately 435 nm. pad and wash with hot dilute sulphuric acid (1 :99).
Preserve the filtrate.
5.2 Reagents
5.3.2 Ignite the residue in a silica basin at a temperature
5.2.1 Mixed Acid.~ not exceeding 600”C. Transfer the residue to a platinum
Add 170 ml of sulphuric acid (rd. = 1.84) cautiously, crucible. Moisten it with a little water. Add 2 to 3 drops
9
1S 504 (Part 3) :2002
of dilute sulphuric acid (1:1) and 8 to 10 ml of solution, and

hydrofluoric acid. Evaporate the dryness and ignite for rn = mass in g of the sample represented by
about 5 min. dissolve inafewmillilitres ofwater and the aliquot taken.
mix with the filtrate preserved under 5.3.1. NOTE— Since the carbon tetrachloride
extract of copper complex
is readily bleached by exposure to strong light, extraction should
5.3.3 Adjust the volume to 300 ml. Heat the solution be carried out in artificial Iightorweak daylight.
to 60”C, add a small quantity ofashless paper pulp
and pass hydrogen sulphide for about half an hour 6 DETERMINATION OF COPPER BY THE
and keep for another half an hour at about 50 to 60°C. IODIMETRIC METHOD (FOR COPPER CON-
Filter through medium textured filter paper and wash TENT OVER 0.1 PERCENT)
8 to 10 times with hydrogen sulphide wash sohstion.
Transfer the filter paper along with the precipitate to 6.1 Outline of the Method
the same beaker in which copper was precipitated. The sample is treated with mixed acids, the silicon
Add 30 to 40 ml of dilute nitric acid (1 :2) and digest removed by fuming and subsequent filtration and
on a hot plate for 15 to 20 min. Dilute to 70-80 ml copper in the filtrate is precipitated as sulphide. The
with hot water and make distinctly ammoniacal. Keep copper sulphide is ignited and dissolved in acid and
just boiling for 3 to 4 min. and filter through fine the copper determined iodimetrically. Antimony, if
textured filter paper into a 200 ml volumetric flask. present, is separated from the copper sulphide in
Wash with hot dilute ammonium hydroxide wash alkaline sulphide solution.
solution and discard the residue.
6.2 Reagents
5.3.4 Pipette a suitable aliquot (depending on the
copper content of the solution) into a 250 ml separating 6.2.1 Sulphuric Acid — rd. = 1.84.
funnel. Add 10 ml of citric acid. Make distinctly
6.2.2 Nitric Acid — rd. = 1.42.
ammoniacal. Add 10 ml of sodium diethyl-dithio-
carbamate solution, mix well and allow to stand for 6.2.3 Hydrochloric Acid — rd. = 1.16.
15 min. Extract successively with 25 ml, 15 ml and
10 mI of carbon tetrachloride. Combine carbon tetra- 6.2.4 Mixed Acids
chloride extracts and make up to 50 ml in a graduated To 700 ml of water add gradually 150 ml of sulphuric
flask. Add a little anhydrous sodium sulphate to clear acid. Cool, then add 75 ml of nitric acid and 75 ml of
the solution. hydrochloric acid.
--- ---
5.3.5 Transfer a suitable aliquot to an absorption cell 6.2.5 Hydro$uoric Acid (40 percent.)
and adjust the spectrophotometer to the initial setting.
Take the spectrophotometric reading at 435 nm or 6.2.6 Dilute Sulphuric Acid — 1 ; 1(v/v). /
using a photometer with a light filter at 435 nm. 6.2.7 Ammonium Fluoride — Solid.
5.3.6 Calibration Curve 6.2.8 Ammonium Hydroxide (20 percent)
Take a series of standard copper solutions and a 6.2.9 Acetic Acid — Glacial.
reagent blank. Using same quantities of all reagents,
carry through all the stages as described under 5.3.4 6.2.10 Urea Solution — 20 percent (m/v).
and 5.3.5 and record the spectrophotometric readings Dissolve 20 g of urea in 100 ml of distilled water.
of the standard solutions along with the blank. Draw
a calibration curve by plotting the spectrophotometric 6.2.11 Potassium Iodide Solution — 50 percent (m/v).
readings of standard solutions against milligrams of 6.2.12 StandardSodium Thiosulphate Solution (0,05 N
copper per 50 mI of organic extract of solution. and 0.02 N),
5.4 Calculation Dissolve 12.41 g of sodium thiosulphate in distilled
water and make up to 1 000 ml. Stabilize by the
Convert the spectrophotornetric reading of the sample
addition of 2 to 3 grams of borax per litre, For pre-
to milligrams of copper by means of calibration curve
paring standard thiosulphate solution (0.02 N). Dilute
and calculate the percentage of copper as follows :
200 ml of standard thiosulphate solution (0.05) to 500
ml with water. This solution shall be used when the
Copper, percent by mass = X x ~

copper content is between 0.3 to 2.5 percent.
m Standardize the solution as described under 6.2.12.1.
where 6.2.12.1 Weigh out exactly one gram of electrolytic
copper, dissolve in 10 ml of dilute nitric acid (1:1).
M = mass in mg of copper found in the aliquot
10
-4
IS 504(Part 3):2002 I!
,,
of hydrogen sulphide gas through the solution for ~ ‘$
Boil nearly to dryness and dilute with water. Cool and
make up the solution to 250 ml in a graduated flask. 20 min. Add some ashless paper pulp and let stand !!!
for a few minutes to allow the precipitate to coagulate. ,4
Pipette out exactly 25 ml (for standardizing 0.05 N
solution). Add ammonium fluoride, ammonia, acetic Filter and wash the paper and precipitate 6 to 8 times
acid, urea and potassium iodide as described under 6.3 with warm hydrogen sulphide wash solution.
and titrate with thiosulphate solution to be .’1,,
6.3.2 Dry and ignite the copper sulphide residue at “‘!
standardized, using starch as indicator. ( ~i
not more than 700”C in a porcelain or silica crucible.
6.2.13 Starch Solution Moisten the residue in the crucible with a few drops
of water and warm with 2 to 3 ml of nitric acid to
Make a suspension of one gram of soluble starch in re-dissolve. Transfer to 300 ml of conical flask or
about 10 ml of water and add it carefully to 100 ml of beaker, boil nearly to dryness to remove most of the
boiling water. Boil for 2 or 3 min and cool. Prepare excess nitric acid and re-dissolve in approximately
the solution fresh as needed. 10 ml of water.
6.2.14 Ammonium Thiocyanate — Solid. 6.3.3 Add 0.1 to 0.2 g of ammonium fluoride, neu-
6.2.15 Hydrochloric Acid–Nitric Acid Mixture tralize carefully by adding ammonium hydroxide drop
by drop until blue complex is formed, and then add
Mix 500 ml of hydrochloric acid (6.2.3) with 500 ml one drop in excess. Acidify with glacial acetic acid
of nitric acid (6.2.2). added dropwise, and add ten drops in excess, followed
6.2.16 Sodium Hydroxide Solution — 20 percent (m/v). by a drop of urea solution. Wash the sides of the flask
or beaker using not more than 5 ml of water. Add 5
6.2.17 Sodium Sulphide Solution — 15 percent (m/v). ml of potassium iodide solution and titrate with stand-
6.2.18 Sodium Hydroxide — Sodium Sulphide Wash ard sodium thiosulphate solution adding one milli-
Solution litre starch solution as indicator towards the end of
the titration. Add about one to two grams of
Mi%equal volumes of sodium hydroxide solution( one ammonium thiocyanate (to liberate the absorbed
percent) and sodium sulphide solution (one percent). iodine) and continue the titration until the blue colour
6.2.19 Dilute Nitric Acid — 1 : 1 (v/v). is completely discharged.
6.2.20 Sulphurous Acid 6.3.4 Calculation
Saturate water with sulphur dioxide. Prepare fresh as AxB

needed. Copper, percent by mass= —x 100
c
6.2.21 Hydrogen Sulphide — Gas.
where
6.2.22 Hydrogen Sulphide Wash Solution
A= volume in ml, of the standard sodium thio-
Satura~e dilute sulphuric acid (1:99) with hydrogen sulphate solution required to titrate the
sulphide gas. sample;
6.3 Procedure (In the Absence of Antimony) B= copper equivalent of the standard sodium
thiosulphate solution in g/ml; and
6.3.1 Take 2 g of the accurately weighed samples c= mass in g, of the sample taken.
(see Note) in a 400 ml beaker and treat with 50 ml of
mixed acids. After the reaction has subsided, add 6.4 Procedure (In the Presence of Antimony
20 ml more of the mixed acids, adding a little nitric and Tin)
acid if necessary. If silicon content is small (less than 6.4.1 Treat 2 g of the accurately weighed sample in a
2 percent), the recovery of copper from the residue is 600 ml beaker with 40 ml of hydrochloric acid-nitric
unnecessary provided that sufficient hydrofluoric acid acid mixture. When the reaction is complete, dilute
is added at this stage to give a clear solution. Add slightly and evaporate by boiling until just pasty
20 ml of dilute sulphuric acid, evaporate the solution Dissolve in a small amount of water and pour into
to fuming and continue fuming for 10 rein, cool, 100 ml of sodium hydroxide solution with constant
dilute to 200 ml and boil until the solution is clear. stirring. Dilute to 300 ml, bring to the boil, and 25 ml
Filter off the insoluble matter on a paper pulp pad and of sodium sulphide wash solution, re-boil and allow
wash with hot water. Precipitate copper by following the precipitate to settle for 30 min. Filter on a paper
the procedure given below: pulp pad and wash with sodium hydroxide-sodium
Heat the filtrate to 60 to 70° and pass a steady stream sulphide wash solution.
11
IS 504 (Part 3) :2002
6.4.2 Extract the residue with hot dilute nitric acid with 250 ml of hot water, heat to 60”C and saturate
adding a little sulphurous acid, if necessary, and wash with hydrogen sulphide gas. Filter off the copper
with hot water. Add 5 ml of sulphuric acid and sulphide and wash with hydrogen suIphide wash
evaporate by boiling to a low bulk. Dry the paper pulp solution, dry and ignite the paper and the residue as
pad, from which the bulk of the copper sulphide has before. Moisten the residue in the crucible with a few
been extracted and ignite for 20 to 30 min in a platinum drops of water and warm with 2 to 3 ml of nitric acid
crucible at approximately 700°C. Dissolve the residue to dissolve. Transfer to a conical flask or beaker, boil
in a few drops of nitric acid, add a few drops of nearly to dryness and dissolve in a small amount of
hydrofluoric acid, if necessary, to remove the silicon, water. Proceed further as described under 6.3.3
combine with the sulphuric acid solution obtained and 6.3.4.
above and evaporate the solution to fuming, cool, dilute
..-
/
I
12
IS 504(Part 4):2002
Indian Standard
PART 4 DETERMINATION OF ZINC
(Second Revision)
1 SCOPE 5.2 Reagents
This standard (Part 4) describes the method for deter- 5.2.1 Dilute Hydrochloric Acid — 1:1 (v/v).
mination of zinc up to 0,1 percent by the Dithizone
5.2.2 Potassium Chlorate — Solid.
(Spectrophotometric) method and by Mercuric
Thiocyanate (Volumetric) method and above 5.2.3 Carbon Tetrachloride
0.1 percent by Mercuric Thiocyanate (Gravimetric)
5.2.4 Complex – Forming Solution
method in aluminium and its alloys.
Add successively, with shaking, to a 500 ml separator
2 REFERENCES funnel, 15 drops of ammonium hydroxide, 1.5 ml of
The Indian Standards listed below contain provisions ammonium oxalate solution (5 percent), 15 ml of
which through reference in this text, constitute sodium acetate (5 percent), 35 ml of hydrochloric acid
provisions of this standard. At the time of publication, (l N), and a mixture of 120 ml of sodium thiosulphate
the editions indicated were valid. All standards are solution (50 percent) and 150 ml of sodium sulphide
subject to revision, and parties to agreements based solution (one percent). Shake the solution with small
on this standard are encouraged to investigate the portions of dithizone until the latter remains green.
possibility of applying the most recent editions of the Since the extraction of zinc proceeds slowly, it is better
standards indicated below: to use a shaking machine and allow 10 min for the
reaction. Remove droplets of dithizone by finally
IS No. Title washing with carbon tetrachloride. Slight separation
264:1976 Nitric acid (second revision) of sulphur in aqueous solution does no harm.
----
265:1993 Hydrochloric acid ~ourth revision) 5.2.5 Dithizone Solution
1817:1961 Methods of sampling of non-ferrous Dissolve 0.01 g of reagent in 100 ml of carbon
metals for chemical analysis tetrachloride.
3 SAMPLING 5.2.6 Sodium Sulphide Wash Solution
The sample shall be drawn and prepared in accordance Dissolve 5 g of sodium sulphide in 500 ml of water.
with the method prescribed in 1S 1817. Dilute 25 ml of the solution to 500 ml.
4 QUALITY OF REAGENTS 5.2.7 Standard Zinc Solution ( 1 ml= 0.01 mg of Zn)
Unless specified otherwise, analytical grade reagents Dissolve 0.1 g of pure zinc (purity 99.95 percent) in
and reagent grade water (see IS 1070) shall be 5 to 10 ml of dilute hydrochloric acid (1: 1). Cool and
employed for the test. dilute to one litre in a volumetric flask. Transfer
10 ml of this solution to a 100 ml volumetric flask
5 DETERMINATION OF ZINC BY THE and make up the volume to the mark.
DITHIZONE (PHOTOMETRIC) METHOD (FOR
5.2.8 Ammonium Hydroxide (20 percent)
ZINC CONTENT BELOW 0.1 PERCENT)
5.1 Outline of the Method 5.2.9 Ammonium Oxalate Solution (5 percent)
The sample is dissolved in hydrochloric acid and 5.2.10 Sodium Acetate Solution (5 percent)
potassium chlorate. Red colour complex obtained by 5.2.11 Sodium Thiosulphate Solution (50 percent)
the addition of dithizone to an aliquot of the solution
is extracted with carbon tetrachloride and determined 5.3 Procedure
spectrophotometricall y at about 530 nm.
5.3.1 Dissolve 0.25 g of the accurately weighed sample
in 12.5 ml of dilute hydrochloric acid, ~dd 0.2 g-of
13
IS 504 (Part 4) :2002
potassium chlorate and boil for 5 min. Dilute the 6 DETERMINATION OF ZINC BY MERCURIC
solution to 250 ml in the volumetric flask and filter THIOCYANATE METHOD
through coarse paper, rejecting the first portion of the
filtrate. 6.1 Outline of the Method
5.3.2 Pipette a suitable aliquot (depending upon the The sample is dissolved in mixed acids, silicon and
zinc content of the sample) into a 100 ml separator copper precipitated by fuming and by means of
funnel, add 30 ml of complex forming solution and hydrogen sulphide respectively. From the filtrate zinc
10 ml of dithizone solution and shake vigorously. If is precipitated as sulphide in the presence of formic
the carbon tetrachloride becomes red or red-violet in acid. Zinc sulphide is extracted with acid and zinc
a short time, draw off the extract into a graduated glass mercuric thiocyanate precipitated from the extract,
stoppered, 25 ml cylinder and shake the aqueous phase dried and weighed or titrated with standard potassium
with a fresh 5 ml portion of dithizone solution. If after iodate solution depending upon the zinc content.
5 min the carbon tetrachloride is only a dark violet,
6.2 Reagents
separate it, add 1 ml of dithizone solution and shake
for a minute. The last extract shall remain green. Wash 6.2.1 Mixed Acid
the last extract with carbon tetrachloride.
Add 150 ml of sulphuric acid (rd. = 1.84) cautiously
5.3.3 Add 5 ml of the sodium sulphide wash solution to 700 ml of water and cool. Then add 75 ml of
to the combined extract and dilute the latter to 25 ml hydrochloric acid (rd.= 1.16) and 75 ml of nitric acid
with carbon tetrachloride. Shake a few times with the (rd. = 1.42).
wash solution and draw off the carbon tetrachloride
6.2.2 Dilute Szdphuric Acid — 1:1 (v/v),
phase. Repeat the washings three to four times with
5 ml portions of the wash solution. The last portion of 6.2.3 Hydrogen Stdphide — Gas.
the wash solution shall remain colorless. Filter the
carbon tetrachloride extract through an acid-free, filter
paper of coarse texture to remove water droplets. Saturate sulphuric acid (one percent) with hydrogen
Transfer a suitable portion of the solution to an sulphide gas.
absorption cell and take the photometric readings using
6.2.5 Tartaric Acid Solution —30 percent (v/v).
a light filter at 530 nm or use a spectrophotometer to
measure the absorbance at 530 nm. 6.2.6 Ammonium Hydroxide (20 percent)
5.3.4 Calibration Curve 6.2.7 Met@lRedIndicator Solution — 0.1 percent (v.#v) ----
Take a series of standard zinc solutions and the reagent Dissolve 0.1 g of methyl red in 3.72 ml of sodium
blank. Using the same quantities of reagents, carry hydroxide solution (O.1 N) and dilute to 250 ml with
through all stages as described under 5.3.2 and 5.3.3 water. Filter, if necessary.
and record the spectrophotometric readings of all the
6.2.8 Formic Acid Mixture
standard solutions along with the blank. Draw a
calibration curve by plotting the spectrophotometric To 20 ml of formic acid (rd. = 1.20), add 25 g of
readings of standard solutions against milligrams of ammonium sulphate and 3 ml of ammonium hydroxide
zinc per hundred millilitres of the solution. and dilute to 100 ml.
5.4 Calculation 6.2.9 Formic Acid Wash Solution

Convert the spectrophotometric reading of the sample Dilute 25 ml of formic acid mixture to one litre and
to milligrams of zinc by means of calibration curve, saturate with hydrogen sulphide gas.
and cal~ulate the percentage of zinc as follows:
6.2.10 Dilute Hydrochloric Acid — 1:1 (v/v).
6.2.11 Nitric Acid — rd. = 1.42.

Zinc, percent = # x +
6.2.12 Ammonium Nitrate — Solid.
where 6.2.13 Methylated Spirit
A = mass in mg, of zinc found in the aliquot 6.2.14 Sulphuric Acid — A4ethylated Spirit Mixture
of the sample solution used; and
Add one millilitre of sulphuric acid (rd.= 1.84) to
B = mass in g of the sample represented by
200 ml of water and then add 200 ml of industrial
the aliquot taken. methylated spirit.
14
Free Standard provided by BIS via BSB Edge Private Limited to Swaptul Enterprises - —.?*
-.
IS 504( Part4) :2002
6.2.15 A4ercuric Potassium Thiocyanate Solution of formic acid mixture, heat to 70 to 80”C. Add a
little paper pulp and pass hydrogen sulphide gas
Dissolve 54 gof mercuric chloride in water, add to
rapidly through the solution for 30 min. Allow the
76 g of potassium thiocyanate dissolved in water and
precipitate of zinc sulphide to coagulate, filter on a
dilute to two Iitres. Filter before use.
pulp pad and wash with warm formic acid wash
6.2.16 Concentrated Hydrochloric Acid solution. Extract the precipitate with dilute hydro-
chloric acid and wash with hot water. Add 5 ml of
6.2.17 Chloroform
nitric acid and 10 ml of dilute sulphuric acid.
6.2.18 Standard Zinc Solution ( 1ml = 0.0001 g of Zn) Evaporate to fuming, decolourize with a few crystals
of ammonium nitrate and fume for 10 min. Wash down
Dissolve 0.1 g pure electrolytic zinc in sufficient dilute
and re-fume for 10 rein, cool, dilute to 50 ml with
sulphuric acid (1:1) and dilute to 1 000 ml with water.
water, add 50 ml of methylated spirit, mix well and
6.2.19 Standard Potassium Iodate Solution allow to stand overnight-. Filter-the lead sulphate
through a sintered glass filter funnel containing paper
Dissolve 9.820 g of potassium iodate in water and dilute
pulp pad using gentle suction, and wash with cold
to 1 000 ml. Pipette three portions each of 20 ml of
sulphuric acid-methylated spirit mixture.
standard zinc solution into separate 200 ml beakers.
To each add 5 ml of dilute sulphuric acid (1:1), dilute 6.3.4 Evaporate the filtrate to dryness, add 35 ml of
to 75 ml with water and precipitate with 25 ml of water and 10 ml of dilute sulphuric acid, boil until
mercuric potassium thiocyanate solution. Filter, wash clear. Cool and precipitate the zinc with 25 ml of
the precipitates. Extract and titrate each extract mercuric potassium thiocyanate solution with vigorous
separately with standard potassium iodate solution as stirring. Allow to stand for at least 8 h and filter by
described in 6.3. From the mean titre adjust the strength suction on a weighed sintered-glass crucible. Wash
of the potassium iodate solution so that 1 ml = 0.0001 6 times (25 ml each time) with mercuric potassium
g, 0.0002 g or 0.0005 g of zinc depending on the thiocyanate solution, diluted 50 times. Dry at 11O“C
amount of zinc expected in the sample. to constant weight.
6.3 Procedure (Gravimetric Method) (for Zinc Con- 6.3.5 Carry out a blank determination, following the
tent Above 0.1 Percent) same procedure and using the same amounts of all
reagents, but without the sample.
6.3.1 Depending upon the zinc content of the sample,
adjust the mass of the sample and volume of the mixed 6.3.6 Calculation
--
acid as given below to a conical weighed beaker:
(A- B) X1312
Zinc Content, Mass in g of Volume in ml of Zinc, percent by mass = —
percent the Sample Mixed Acid c“
to be Taken Required where
Over 2 up to 4 0.5 25
A = mass in g, of zinc mercuric thiocyanate,
Over I up to 2 1 35
B = correction for the blank in g, and
Over 0.1 up to 1 2 70
C = mass in g, of the sample taken.
Over 0.05 up to 0.1 3 90
6.4 Procedure [By Mercuric Thiocyanate
up to 0.05 5 100 (Volumetric) Method (for Zinc Content up to 0.1
6.3.2 Cool, if necessary. Add 20 ml of dilute sulphuric Percent)!
acid carefully, evaporate to fumes and continue fuming 6.4.1 Take the filtered and washed zinc mercuric
for 10 min. cool, dilute to 200 ml with water and boil thiocyanate precipitate as obtained under 6.3.4 in a 60
until solution is complete. Allow it to cool. Cool to ml of hydrochloric acid added round the edge of the
60 to 70°C and pass hydrogen sulphide rapidly through sintered-glass filter funnel. Allow to stand for 1 min
the solution for approximately 20 min. Allow the and then apply suction. Add further 2 ml of hydrochloric
precipitate to coagulate. Immediately filter the silica acid dropwise as before, wash alternately with 1 ml of
and copper sulphides on a paper pulp pad, wash with water and hydrochloric acid. Finally pour 0.5 ml of
warm hydrogen sulphide wash solution. water. Add 0.5 to 1 ml of chloroform to the solution in
6.3.3 Boil the filtrate to remove all hydrogen sulphide the bottle and titrate with standard potassium iodate
gas and adjust the volume to about 250 ml. Add 25 ml solution until the chloroform layer isjust colorless. In
of tartaric acid solution and neutralize with ammonium most cases the titration is started by adding 4 drops of
hydroxide using methyl red as indicator. Add 25 ml iodate solution and then shaking. Further additions are
then made drop by drop with thorough shaking.
15
Free Standard provided by BIS via BSB Edge Private Limited to Swaptul Enterprises - .. e%
IS 504 (Part 4) :2002
6.4.2 Calculation B = volume in ml, of the standard potassium

iodate solution required for the blank;
(A- B) CXIOO
Zinc, percent by mass = C = zinc equivalent of the standard potassium
D
iodate solution in g/ml; and
where
D = mass in g, of the sample taken.
A = volume in ml, of the standard potassium
iodate solution used in the test;
..- --
16
IS 504 (Part 5) :2002
Indian Standard 4
CHEMICAL ANALYSIS OF 1
PART 5 DETERMINATION OF MANGANESE
(Second Revision)
1 SCOPE 5.2.3 Sulphurous Acid
This standard (Part 5) describes method for determi- Make approximately 5 percent solution of sulphur
nation of manganese content in the range 0.1 to 1.5 dioxide in water.
percent by the Bismuthate method.
5.2.4 Dilute Nitric Acid — 3:97 (vIv).
2 REFERENCES 5.2.5 Phosphoric Acid — 85 percent (mIv).
The Indian Standards listed below contain provisions 5.2.6 Standard Ferrous Ammonium Sulphate Solution
which through reference in this text, constitute (0.03 N)
the editions indicated were valid. All standards are Dissolve 6 g of ferrous ammonium sulphate [Fe (NH,)2
subject to revision, and parties to agreements based (S0,),. 6H20] in cold dilute sulphuric acid (5:95) and
on this standard are encouraged to investigate the make the volume to 500 ml with this acid. Mix well
possibility of applying the most recent editions of the and keep in an amber-coloured glass-stoppered bottle.
standards indicated below: 5.2.7 Standard Sodium Oxalate Solution
IS No. Title Dissolve 2.01 g of sodium oxalate in water and make
264:1976 Nitric Acid (second revision) up to one litre in a graduated flask.
1070:1992 Reagent grade water (third revision) 5.2.8 Standard Potassium Permanganate Solution
1817:1961 Methods of sampling of non-ferrous (0.030 N)
Dissolve 0.958 g of potassium permanganate in water -- -
3 SAMPLING
and dilute to 1 000 ml. Set the solution aside for two
The sample shall be drawn and prepared in accordance weeks in a dark place, filter without washing through
with IS 1817. a fritted glass crucible and store in a dark-coloured
stoppered bottle. Standardize the permanganate
4 QUALITY OF REAGENTS solution against standard sodium oxalate solution
Unless specified otherwise, analytical grade reagents (see 7.2.7).
and reagent grade water (see 1S 1070) shall be
5.3 Procedure
employed for the test.
5.3.1 Depending upon the manganese content of the
5 DETERMINATION OF MANGANESE BY THE sample, transfer an accurately weighed sample and
BISMUTHATE METHOD (FOR MANGANESE the volume of sodium hydroxide, in solution as given
CONTENT BETWEEN 0.01 TO 1.5 PERCENT) below to a 500 ml beaker :
5.1 Outline of the Method Manganese Content, Mass in g of Volume in ml of
Percent by Mass the Sample to Sodium
Manganese in the solution of the sample is oxidized
be Taken Hydroxide
to permanganic acid by means of sodium bismuthate
Solution Required
in nitric acid medium and the permanganate thus
formed is titrated with standard ferrous ammonium Over 1.0 up to 1.5 1 25
sulphate solution. Over 0.25 up to 1.0 3 50
5.2 Reagent Over 0.1 up to 0.25 5 100
5.2.1 Nitric acid — rd. = 1.42. Treat the sample with 25 ml of sodium hydroxide
solution (50 ml for 2 g of sample) and bring to boil-
5.2.2 Sodium Bismuthate — Solid. ing point on a hot plate until all visible action ceases.
17
—.
1S 504(Part 5):2002
(For silicon content greater than 4 percent, concent- solution. Titrate immediately the excess of ferrous
rate the solution at this stage to about half volume). iron with the standard permanganate solution to the
Cool slightly, then add 60 ml of the acid mixture faint pink colour.
(100 ml for a 2 g sample) wash down the sides of the
5.3.4 Carry out a blank determination following the
beaker and boil gently until solution is
same procedure and using the same amount of the
complete and nitrous fumes are expelled.
standard ferrous ammonium sulphate solution and
5.3.2 Dissolve the sample as described under 5.3.1. other reagent as were used in the titration, but without
Neutralize the solution with nitric acid and add 40 ml the sample.
in excess. Boil the solution and add 0.5 g of sodium
bismuthate. Boil for 2 to 3 min and dissolve the 5.4 Calculation
precipitated oxides of manganese in sufficient amount
of sulphurous acid, added dropwise till solution is (A- B) CX1.I
Manganese, percent =
clear. Boil to expel oxides of sulphur and nitrogen. D
Dilute to about 100 ml with water and cool the solution
where
to 10 to 15”C.
A= volume, in ml of the standard
5.3.3 Add about 0.5 g of sodium bismuthate (or 26
permanganate solution required to titrate
times more than manganese content of the sample
the blank;
but not less than 0.5 g). Agitate for 2 or 3 min and
filter immediately through asbestos Gooch crucible. B= volume, in ml of the standard permanganate
Wash with cold dilute nitric acid until the washings solution required to titrate the excess of
are colorless. Reject the insoluble residue and ferrous ammonium sulphate solution;
maintain the temperature of the filtrate at 10 to 15°C. c= normality of the standard permanganate
Add 2 ml of syrupy phosphoric acid to the measured solution; and
excess of standard ferrous ammonium sulphate D= mass, in g of the sample taken.
“-
18
IS 504 (Part 6): 2002
Indian Standard
PART 6 DETERMINATION OF MAGNESIUM
(Second Revision)
1 SCOPE 5.2.4 Sodium Carbonate Solution — 5 gll.
This standard (Part 6) describes the method for deter- 5.2.5 Met~lRedIndicator Solution — 0.1 percent (mIv)
mination of magnesium in the range from 0.0 I to 12
Dissolve 0.1 g of methyl red in 3.72 ml of sodium
percent by the oxine method.
hydroxide solution (O.1 N) and dilute to 250 ml with
2 REFERENCES water. Filter, if necessary.
The Indian Standards listed below contain provisions 5.2.6 Ammonium Hydroxide (20 percent)
5.2.7 Ammonium Chloride Wash Solution
the editions indicated were valid. All standards are Dissolve 10 g of ammonium chloride in water, dilute
subject to revision, and parties to agreements based to one Iitre, and make just yellow to methyl red with
on this standard are encouraged to investigate the ammonium hydroxide.
standards indicated below : 5.2.8 Ammonium Chloride — Solid:
IS No. Title 5.2.9 Hydrochloric Acid — rd. = 1.16.
265:1987 Hydrochloric acid (third revision) 5.2.10 Ammonium Sulphide Solution

Methods of sampling of non-ferrous Saturate ammonium hydroxide (1:9) with hydrogen
1817:1961
metals for chemical analysis sulphide gas.
3 SAMPLING 5.2.11 Ammonium Persu[phate — Solid.
The sample shall be drawn and prepared in accordance 5.2.12 Ammonium Sulphide Wash Solution
1;
with IS 1817.
Add 10 ml of ammonium sulphide solution to one litre.
4 QUALITY OF REAGENTS of water containing 10 g of ammonium chloride and
a few drops of ammonium hydroxide.
Unless specified otherwise, analytical grade reagents
and reagent grade water (see IS 1070) shall be 5.2.13 Bromine Water — Saturated.
employed for the test.
5.2.148 Hydroxyquinoline Solution
5 DETERMINATION OF MAGNESIUM BY
Dissolve 5 g of 8 hydroxyquinoline in 10 ml of glacial
THE OXINE METHOD (FOR MAGNESIUM
acetic acid and dilute to 100 ml with water.
CONTENT BETWEEN 0.01 TO 12 PERCENT)
5.2.15 Dilute Ammonium Hydroxide — 1:99 (vIv].
5.1 Outtine of the Method
5.2.16 Methyl Orange Indicator Solution
After the removal of interfering elements, magnesium in
the solution of the sample is precipitated with Dissolve 0.05 g of methyl orange in 100 ml of alcohol.
8 hydroxyquinoline and determined either ~mvimetrically
or volumetrically. 5.2.17 Potassium Bromate — Potassium Bromide
Solution
5.2 Reagents
Dissolve 2 g of potassium hydroxide, 80 g of potassium
5.2.1 Sodium Hydroxide — Solid. bromide, and 9 g of potassium bromate, in 700 ml of
water and dilute to one Iitre.
5.2.2 Hydrogen Peroxide — 20 volumes.
5.2.3 Sodium Carbonate — Solid. 5.2.18 Potassium Iodide Solution — 300 gfl (mIv).
19
—...4
IS 504 (Part 6) :2002
5.2.19 Starch Solution hydrochloric acid (1: 1) and wash the filter with hot
water.
Make a suspension of one gram of soluble starch in
about 10 ml of water and add it carefully to 100 ml of NOTES
boiling water. Boil for 2 to 3 min and cool. Prepare 1 In case of high silicon alloys, sample should be first attacked
with weak alkali and subsequently by strong alkal i. B y the former
the solution fresh as needed.
treatment alrrminium will dissolve almost completely and with
the latter treatment silicon will dissolve without precipitation of
5.2.20 Standard Potassium Iodate Solution (0.33 N)
silicates.
Dissolve 11.771 g of the potassium iodate dried at 2 If chromium-bearing constituents are not completely
180”C to constant mass in 200 ml of water, containing decomposed, an insoluble residue containing some magnesium
will remain tier treatment with concentrated hydrochloric acid.
1 g of sodium hydroxide and add 10 g of potassium
iodide; when solution is complete, dilute to one Iitre 5.3.3 If the sample does not contain manganese, nickel
in a volumetric flask. or more than 3 mg of copper, add few drops of methyl
red indicator and then add ammonium hydroxide and
5.2.21 Standard Sodium Thiosulphate Solution
about 5 g of ammonium chloride until the solution is
(0.33 N)
yellow to methyl red. Allow the precipitate to
Dissolve 81.84 g of sodium thiosulphate (Na2SzO~. coagulate, filter and wash with hot ammonium
5H20) in one litre of freshly boiled and cooled water chloride wash solution. If the magnesium content is
in a sterile glass bottle. Standardize as follows: over 0.02 g, place the paper with the precipitate in the
original container and dissolve with 15 ml of dilute
Pipette 25 ml of the standard potassium iodate solution
hydrochloric acid. Dilute to 50 ml with hot water.
(see 5.2.20) into a 125 ml flask. Add 30 ml of water,
Precipitate as before, filter and wash with hot
one gram of the potassium iodide and 10 ml of dilute
ammonium chloride wash solution. Make the
sulphuric acid (1 : 4). Titrate with sodium thiosulphate
combined filtrate just acid to methyl red and precipitate
solution to a light straw colour. Add 2 ml of starch
magnesium as before.
solution and continue titration to the disappearance
of the blue colour. 5.3.4 In case the sample contains manganese, nickel
and more than 3 mg of copper, neutralize the acid
5.3 Procedure solution as obtained under 5.3.2. with ammonium
5.3.1 Depending upon the magnesium content of the hydroxide and add about 5 g of ammonium chloride.
sample, transfer an accurately weighed sample as Add 5 ml of ammonium sulphide solution (see Note).
given below to a 250 ml wide mouthed Erlynmeyer Filter into a 250-ml beaker, and wash with ammonium
flask: sulphide wash solution. If more than 20 mg of
magnesium are present in the sample, some
Magnesium Content, Mass in g of the Sample magnesium may be carried down with the sulphides.
Percent to be Taken In that case, dissolve the precipitate with 15 ml of
Over 2.0 0.5 or less dilute hydrochloric acid and re-precipitate as under
5.3.3. Filter and wash the sulphides. Combine the
Over 0.2 up to 2.0 1
filtrates and boil vigorously to drive off the ammonium
Over 0.01 up to 0.2 2 sulphide. If a noticeable sulphide precipitate forms as
It is recommended that for high magnesium content, the solution boil and becomes acid (usually indicating
such a mass of sample be taken that it does not contain nickel or tin), filter, wash and boil the filtrate. Oxidize
more than 0.05 g of magnesium. the remaining sulphur by adding an excess of bromine
water, and continue boiling until the colour disappears.
5.3.2 Dissolve the sample in sodium hydroxide
NOTE — In case of alloys with manganese content over one
solution (see Note 1), using about 6 g of sodium
percent manganese may not completely precipitate by ammonium
hydroxide per gram of the sample. After violent sulphide. In Mat case, add a few grams of ammonium persulphate
reaction has subsided, heat the flask to hasten the to the filtrate to separate manganese completely.
decomposition of the sample. When visible evolution
5.3.5 Adjust the volume of the solution obtained
of hydrogen ceases, cautiously add few drops of
under 5.3.3 or 5.3.4 to 75 ml. Remove from the hot
hydrogen peroxide to the hot concentrated solution to
plate, add 10 ml of bromine water, and while stirring
complete the oxidation of silicon, zinc and chromium
make the solution alkaline with ammonium
(see Note 2). Dilute to 150 ml and add 3 to 5 g of
hydroxide and add 15 drops in excess. Digest until
sodium carbonate. Stir well, and allow the precipitate
any manganese present precipitates as manganese
to settle. Filter and wash the residue with hot sodium
dioxide, keeping the solution ammoniacal. Stir just
carbonate solution. Dissolve the magnesium in the
as the solution begins to boil to aid coagulation. Filter
residue, into original container, with 40 ml of dilute
and wash with hot water.
20
IS 504 (Part 6) :2002
5.3.6 Make the filtrate acidic to methyl red with hot dilute hydrochloric acid. Wash with cold dilute
hydrochloric acid. If the indicator does not hold its hydrochloric acid (90 ml of water plus 35 ml of dilute
colour, boil the solution until the bromine is gone. hydrochloric acid) and then with hot water so as to
Make the volume of the solution to about 150 ml, give an acid ratio of 1:4 at a volume of approximately
neutralize the solution with ammonium hydroxide. 150 ml. Add a few drops of methyl orange indicator
Add 5 ml of ammonium acetate and 4 ml of acetic solution. Run in potassium bromate-potassium
acid. Warm to 70°C, treat with slight excess of oxine bromide solution from a burette, until the indicator
solution. Filter and to the filtrate add ammonium is declourized (indicating that bromate is present in
hydroxide in excess. Add 5 ml of oxine solution, while excess) and add 5 ml more. Note the volume of the
stirring (5 ml is enough for 0.015 g of magnesium; potassium bromate-potassium bromide solution
for larger amounts of magnesium up to 0.03 g, add added. Then add 10 ml of potassium iodide solution.
10 ml). Heat the solution just to boiling, remove from Titrate immediately with the standard sodium
the source of heat and allow to stand for 15 to 20 min. thiosulphate solution using 2 ml of starch solution
Filter and wash with hot dilute ammonium hydroxide. as an indicator near the end of the titration. The time
Since only magnesium oxinate is present, the amount from the addition of potassium bromate-potassium
may be determined either gravimetrically or volume- bromide solution to the end of the titration should
trically as described under 5.3.7 and 5.3.8 respectively. not exceed 2 min.
5.3.7 Gravimetric Method 5.3.8.1 Carry out a blank using the same quantity of
the reagents. Titrate the blank through each step of
Filter the magnesium oxinate precipitate on a weighed
procedure.
sintered-glass funnel, washing with hot weakly
ammoniacal water, dry at 100 to 105°C and weigh as 5.3.8.2 Calculation
the dihydrate. If the quantity of the oxinate is small,
proceed as under 5.3.8. (A- B) CXO.3
Magnesium, percent by mass =
5.3.7.1 Calculation D
where
Magnesium, percent by mass = $ x 6.98 A= volume in ml of the standard sodium
thiosulphate solution required to titrate the
where blank;
B= volume in ml of the standard sodium
A = mass in g of the oxinate, and
thiosulphate solution required to titrate the
B = mass in g of the sample taken. sample;
5.3.8 Volumetric Method c= normality of the standard sodium thiosul-
phate solution; and
Dissolve the precipitate of oxinate as obtained under
5.3.7 into a 400 ml stoppered bottle using 30 ml of D= mass, in g of the sample taken.
21
—
IS 504 (Part 7) :2002
Indian Standard
PART 7 DETERMINATION OF NICKEL
(Second Revision)
1 SCOPE 5.2.4 Dilute Sulphuric Acid — 1:1 (v/v).
This standard (Part 7) describes the method for deter- 5.2.5 Hydrogen Sulphide — Gas.
mination of nickel up to 4 percent by the dimethyl-
glyoxime (gravimetric) method.
Saturate dilute sulphuric acid (1:99) with hydrogen
2 REFERENCES sulphide.
The Indian Standards listed below contain provisions 5.2.7 Tartaric Acid Solution
provisions of this standard. At the time of publication, Dissolve 25 g of tartaric acid in 60 ml of water, filter,
the editions indicated were valid. All standards are add 1 ml of nitric acid and dilute to 100 ml.
subject to revision, and parties to agreements based 5.2.8 Ammonium Chloride — Solid.
possibility of applying the most recent editions of the 5.2.9 Ammonium Hydroxide (20 percent)
standards indicated below: 5.2.10 Dimethylglyoxime Solution
IS No. Title Dissolve 1 g of dimethylglyoxime in 100 ml of
264:1976 Nitric Acid (second revision) ammonium hydroxide and filter.
5.3 Procedure
metals for chemical analysis 5.3.1 Depending upon the nickel content of the sample,
3 SAMPLING transfer an accurately weighed sample and the volume
of alkali to the beaker as per the schedule give below:
with IS 1817. Nickel Content, Mass in g of Volume in ml
Percent the Sample to be of Sodium
4 QUALITY OF REAGENTS Taken Hydroxide
Solution
Required
and reagent grade water (see IS 1070) shall be
employed for the test. From 0.5 up to 4 2 20
From 0.1 up to 0.5 5 40
5 DETERMINATION OF NICKEL BY THE
DIMETHYLGLYOXIME (GRAVIMETRIC) Less than 0.1 10 100
METHOD 5.3.2 Dissolve the sample in the required amount of
5.1 Outline of the Method sodium hydroxide solution. When the reaction is
complete, dilute to 150 ml with hot water, allow the
After removal of the interfering elements, nickel
residue to settle for a short time, filter and wash with
present in the sample solution is precipitated in
hot water. Dissolve the residue with a minimum
ammoniacal medium by dimethylglyoxime, filtered,
amount of hot hydrochloric acid together with a little
washed, dried and weighed.
nitric acid, wash the paper thoroughly with hot water.
5.2 Reagents Add 10 ml of dilute sulphuric acid, evaporate to dense
white fumes, dilute to 100 ml with hot water, and
5.2.1 Sodium Hydroxide Solution — 20 percent (v/v). saturate with hydrogen sulphide gas, filter and wash
5.2.2 Dilute Hydrochloric Acid — 1:1 (vIv]. with hydrogen sulphide wash solution.
5.2.3 Nitric Acid — rd. = 1.42. 5.3.3 Boil the filtrate to remove the hydrogen sulphide
22
IS 504 (Part 7) :2002
gas. Add 5 ml of nitric acid, and boil to oxidize iron. dimethylglyoxime,

Dilute to 200 ml, add 10 ml of tartaric acid solution
5.4 Calculation
and 5 g of ammonium chloride. Neutralize with
ammonium hydroxide. Acidify with dilute hydro-
AX 20.32
chloric acid (1: 1). Heat nearly to boiling and while Nickel, percent by mass = ~
stirring add dimethylglyoxime solution (20 ml for
nickel up to 0.02 g and 5 ml for each additional 0.01 where
g). Allow to stand for 1 h. Filter and wash with cold
water. Dry the precipitate at 110 to 120°C to constant A = massing, of nickel dimethylglyoxime, and
mass. Cool in a desiccator and weigh as nickel B = mass in g, of the sample taken.
23
IS 504 (Part 8) :2002
Indian Standard
PART 8 DETERMINATION OF CHROMIUM
(Second Revision)
1 SCOPE 5.2.2 Nitric Acid — rd. = 1.42.
This standard (Part 8) describes the method for deter- 5.2.3 Swphuric Acid — Nitric Acid Mixture
mination of chromium in aluminium and its alloys.
Slowly stir 100 ml of sulphuric acid into one Iitre of
2 REFERENCES water, cool and add 400 ml of nitric acid, dilute to
two litres.
The Indian Standards listed below contain provisions
which through reference in this text, constitute 5.2.4 Silver Nitrate Solution — 8 gll.
provisions of this standard. At the time of publication, 5.2.5 Hydrofluoric Acid (40 percent)
subject to revision, and parties to agreements based 5.2.6 Ammonium Persulphate — Solid.
on this standard are encouraged to investigate the 5.2.7 Dilute Hydrochloric Acid — 1:1 (vIv).
standards indicated below: 5.2.8 Standard Ferrous Ammonium Sulphate Solution
(0.03 N)
IS No. Title
Dissolve 3.2 g of [Fe(NHJ2. (SOJZ. 6HZO] in 500 ml
264:1976 Nitric acid (second revision) of cold dilute sulphuric acid (5:95) and dilute to one
266: 1993 Sulphuric acid (third revision) litre with this sulphuric acid. Standardize against re-
1070:1992 Reagent grade water (third revision) crystallized potassium bichromate solution.
metals for chemical analysis 5.2.9 Standard Potassium Permanganate Solution
(0.03 N)
3 SAMPLING
Dissolve 0.958 g of potassium permanganate in one
Iitre of water. Store in a dark coloured stoppered glass
with the method prescribed in IS 1817.
bottle. Standardize against pure re-crystallized sodium
4 QUALITY OF REAGENTS oxalate or oxalic acid.
Unless specified otherwise, analytical grade reagents 5.3 Procedure

and reagent grade water (see 1070) shall be employed
5.3.1 Transfer 1 g of accurately weighed sample to a
for the test.
400 ml beaker. Add 30 ml of the sulphuric acid-nitric
5 DETERMINATION OF CHROMIUM BY THE acid mixture and 20 ml of silver nitrate solution. Heat
PERSULPHATE OXIDATION (VOLUMETRIC) gently until the sample is dissolved. If free silicon is
METHOD present, add few drops of hydrofluoric acid. Boil until
brown fumes have been expelled.
5.3.2 Dilute to 300 ml with hot water, add 2 g of
Chromium is oxidized to chromate by means of
ammonium persulphate and heat to boiling. After the
ammonium persulphate in presence of silver nitrate
chromium is oxidized, boil for 10 min. Add 0.5 ml of
and the potassium permanganate formed is destroyed
dilute hydrochloric acid and continue boiling until any
with hydrochloric acid. [t is then reduced with a
manganese present is reduced. [f necessary, add an
measured volume of ferrous ammonium sulphate
additional 0.5 ml portions of dilute hydrochloric acid
solution and the excess ferrous solution is titrated with
and boil for 15 min after the final addition.
standard permanganate solution.
5.3.3 Cool and add a measured volume of ferrous
5.2 Reagents ammonium sulphate solution until colour changes
5.2.1 Sulphuric Acid — rd. = 1.84. from yellow to green (7 ml of ferrous amonium
24
IS 504(Part 8):2002
sulphate will reduce about 0.01 g of chromium). Ti- where

trate with standard potassium permanganate solution
VI = volume, in ml of the standard ferrous
until a faint pink end point is obtained which persists
ammonium sulphate solution used;
for one minute.
!,.
N, = normality of the standard ferrous ammo-
5.4 Calculation nium sulphate used;
V, = volume, in ml, of the standard potassium !:
(vlN, - V*N*) x 1.734 perrnanganate solution used;

Chromium, percent by mass=
m N, = normality of the standard potassium
permanganate solution used; and
m = mass, in g of the sample taken.
.-
25
Free Standard provided by BIS via BSB Edge Private Limited to Swaptul Enterprises - ‘8
.
1S 504 (Part 9) :2002
Indian Standard -.
“-”-
PART 9 DETERMINATION OF TIN
(Second Revision )
1 SCOPE the reduction is complete, the flow shall be increased
to maintain a protective cover of carbon dioxide during
This standard (Part 9) describes the method for deter-
cooling and titration (see Fig. 1).
mination of tin by iodimetric method.
5.3 Reagents
2 REFERENCES
5.3.1 Antimony — Metallic powder.
which through reference in this text, constitute 5.3.2 Aluminium Sheet or Rolled Foil — Tin free.
5.3.3 Dilute Hydrochloric Acid — 1:2 (vIv).
subject to revision, and parties to agreements based 5.3.4 Carbon Dioxide — Gas,
5.3.5 Starch — Potassium Iodide Solution
standards indicated below: Make a paste of 1 g of soluble starch in about 5 ml of
water and add to 100 ml of boiling water. Cool and
IS No. Tit[e
add 40 g of potassium iodide and stir until the
1070:1992 Reagent grade water (third revision) potassium iodide is dissolved. Prepare fresh as needed.
5.3.6 Standard Potassium Iodate Solution (0.025 N)
3 SAMPLING Dissolve 0.892 g of potassium iodate (dried at 180°C)
in 200 ml of water, containing 1 g of sodium hydroxide
The sample shall be drawn and prepared in accordance and add 10 g of potassium iodide. When solution is
with IS 1817. complete, dilute to one litre in a volumetric flask.
Standardize against tin solution as prepared
under 5.3.7.
$3.7 Standard Tin Solution
employed for the test. Dissolve 1 g of tin in a covered 400 ml beaker in
300 ml of dilute hydrochloric acid (1:1) by warming
5 DETERMINATION OF TIN BY IODIMETRIC gently until the metal dissolves. If the solution is
METHOD diftlcult, add 0.05 to 0.1 g of potassium chlorate. Cool
and dilute to one Iitre in a volumetric flask.
Tin in the sample is completely dissolved in 5.4 Procedure
hydrochloric acid in the presence of antimony. 5.4.1 Transfer 2 to 5 g of the accurately weighed
Stannous chloride thus formed is titrated with standard sample to a 500 ml flask and add 0.25 g of powdered
potassium iodate solution in carbon dioxide antimony and 150 ml of dilute hydrochloric acid. After
atmosphere. the reaction ceases, heat the flask finally, boiling for
about 10 rein, to ensure complete solution of tin. Filter
5.2 Apparatus
and wash with dilute hydrochloric acid. Discard the
A 500 ml conical flask titted with a three-holed rubber residue and return the filtrate to the original flask.
stopper containing an inlet tube for carbon dioxide,
5.4.2 Add 0.25 g of powdered antimony and 0.5 g of
an air condenser, and a hole for a burette that shall be
aluminium sheet or rolled foil free from tin. (If silicon
kept closed by means of a glass rod, until the titration
content is low then the addition of aluminium may
is started. During the reduction, a very slow stream of
not be required). Stopper the flask and assemble the
carbon dioxide shall be passed through the flask. When
26
IS 504 (Part 9) :2002
apparatus as shown in Fig. 1. Start passing slow cur-

rent of carbon dioxide gas through the flask. Heat AIR CONDENSER
gently until the aluminium is completely dissolved and
boil for 10 min. Increase the flow of the gas so as to
prevent back pressure and cool. As soon as cold, with
the current of carbon dioxide gas still passing, open
290mm
the stoppered-hole and add from a pipette 5 ml of fresh
starch potassium iodide solution. Insert the tip of the
burette containing standard potassium iodate solution
of suitable strength and titrate to a blue colour.
,_CARBON
5.4.3 Carry out a blank determination, following the (f DIOXIDE
procedure given in 5.4.1 and 5.4.2 and using the same
8URETTE
amounts of all reagents, but without the sample. TIP HOLE
5.5 Calculation
(A- B)CXIOO 500.m 1

Tin, percent by mass = ;W&NKMEYER
D
where
A= volume in ml of the standard potassium
iodate solution required to titrate the
sample,
B= volume in ml of the standard potassium
iodate solution required to titrate the FIG. 1 APPARATUS
FORREDUCTION
OFTIN
blank,
c= tin equivalent of the standard potassium
iodate solution in g/ml, and ,’
D= mass in g of the sample taken. ----
27
IS 504 (Part 10) :2002
Indian Standard
PART 10 DETERMINATION OF ANTIMONY
(Second Revision)
1 SCOPE 5.2.3 Dilute Nitric Acid — ]: 1 (vIv).
This standard (Part 10) describes the method for 5.2.4 Hydrazine Sulphate — Solid.
determination of antimony by the potassium iodide-
5.2.5 Thiourea — Solid.
thiourea (photometric) method.
5.2.6 Potassium Iodide Solution — 50 percent (mIv).
2 REFERENCES
5.2.7 Standard Antimony Solution
which through reference in this text, constitute Dissolve 2.0037 g of potassium antimonious tartrate
provisions of this standard. At the time of publication, (dried at 100”C for an hour) in 100 ml of hydrochloric
the editions indicated were valid. All standards are acid and make up to one litre. Alternatively dissolve
subject to revision, and parties to agreements based 0.400 g of pure antimony in aqua regia, add 100 ml of
on this standard are encouraged to investigate the hydrochloric acid and make up to one litre.
possibility of applying the most recent editions of the NOTE—Check the antimony content by iodimetric titration.
standards indicated below:
5.3 Procedure
IS No. Title
5.3.1 Dissolve 0.40 g of an accurately weighed sample
1070:1992 Reagent grade water (third revision) in 10 ml of sodium hydroxide solution. Warm and
1817:1961 Methods of sampling of non-ferrous after the attack is complete, add 15 ml of dilute
metals for chemical analysis sulphuric acid followed by 10 ml of dilute nitric acid.
3 SAMPLING Boil, cool for about 1 rein, add 0.25 g of hydrazine ;..-
,
sulphate to reduce ferric iron to ferrous state. Boil for j
2 rein, cool to room temperature and transfer to a
with IS 1817.
200 ml volumetric flask. Add 2 to 3 g of thiourea fol-
4 QUALITY OF REAGENTS lowed by 40 ml of potassium iodide solution. Make
up to the mark and mix.
and reagent grade water (see IS 1070) shall be 5.3.2 Take a suitable aliquot, filter through medium
employed for the test. textured filter paper, transfer it to an absorption cell
and adjust the photometer to the initial setting. Take
5 DETERMINATION OF ANTIMONY BY THE the spectrophotometric readings using a light filter at
POTASSIUM IODIDE-THIOUREA approximately 15 min after the addition of thiourea
(PHOTOMETRIC) METHOD as otherwise turbidity by decomposition of thiourea
5.1 Outline of the Method may occur.
In acid solution of the sample, a strong yellow colour 5.3.3 Calibration Curve
is produced by the addition of excess potassium iodide. Take a series of standard antimony solutions and a
In the presence of thiourea, copper is kept in solution reagent blank. Using the same quantities of reagents,
as a colorless complex, carry through all the stages as described under 5.3.1
NOTE— Interference due to bismuth is ignored as this chemical and 5.3.2 and record the photometric readings of the
is normally not found in aluminium alloys. standard solutions along with the blank. Draw
calibration curve by plotting the spectrophotometric
5.2 Reagents
readings of standard solutions against milligrams of
5.2.1 Sodium Hydroxide Solution — 40 percent (v/v). antimony per 100 ml of the solution.
5.2.2 Dilute Sulphuric Acid — 1:1 (v/v). Convert the spectrophotometric readings of the sample
to milligrams of antimony by means of calibration
28
Free Standard provided by BIS via BSB Edge Private Limited to Swaptul Enterprises - ,&
IS 504(Part 10):2002
curve and calculate the percentage of antimony. where
5.4 Calculation A = mass in mg, of antimony found in the sam-

ple represented by the aliquot solution
used; and
Antimony, percent by mass = ~ x ~ B = mass in g, of the sample represented by
the aliquot taken.
---
29
IS 504( Part 11) :2002
Indian Standard
PART 11 DETERMINATION OF TITANIUM
(Second Revision)
1 SCOPE Add 50 ml of nitric acid (rd. = 1.42) to 600 ml of
water, then add 350 ml of sulphuric acid (rd. ==1.84),
This standard (Part I 1 ) describes the photometric
method for determination of titanium, in aluminium slowly, while stirring and cool the mixture.
and its alloys. It also describes an alternate 5.2.3 Dilute Sulphuric Acid — 1:9 (vIv).
spectrophotometric method for determination of
titanium in the range 0.001 to 1.0 percent using 5.2.4 Hydrogen Peroxide — 20 volumes.
Diantipyrylmethane. 5.2.5 Standard Titanium Solution (1 ml= 0.0015 g of Ti)
2 REFERENCES Fuse 0.25 g of titania in a covered crucible with 15 g of

The Indian Standards listed below contain provisions potassium pyrosulphate and dissolve the cold melt in
which through reference in this text, constitute 200 ml of hot dilute sulphuric acid (1:1). Cool to room
provisions of this standard. At the time of publication, temperature and dilute to one litre in a volumetric flask.
5.3 Procedure
subject to revision, and parties to agreements based
on this standard are encouraged to investigate the 5.3.1 Transfer one gram of the accurately weighed
possibility of applying the most recent editions of the sample to a 400-ml beaker, cover and add in small
standards indicated below: installments30 ml of sodium hydroxide solution. When
IS No. Title the reaction subsides, wash down the cover and sides
of the beaker, boil to complete the reaction and cool.
1070:1992 Reagent grade water (fhirdrevisiorr) Add 50 ml of nitric acid-sulphurie acid mixture. Boil
1817:1961 Methods of sampling of non-ferrous to dissolve salts, expel brown fumes and cool. Transfer
metals for chemical analysis to a 100 ml volumetric flask. Dilute to the mark and
3 SAMPLING mix. FiIter through a dried fine textured filter paper
The sample shall be drawn and prepared in accordance discarding the first few millilitres of filtrate. Preserve
with [S 1817. the filtrate.
5.3.2 Transfer a suitable alilquot from 25 ml portion
of the solution preserved under 5.3. I to an absorption
Unless specified otherwise, analytical gmde reagents cell and adjust the spectrophotometer to the initial
and reagent grade water (see IS 1070) shall be setting, using a light filter at approximately 410 nm.
employed for the test. To the rest of remaining portion of the filtrate
preserved under 5.3.1, add few drops of phosphoric
5 DETERM1NATION OF TITANIUM BY THE acid.and two drops of hydrogen peroxide and mix.
HYDROGEN PEROXIDE (PHOTOMETRIC)
While maintaining the spectrophotometer adjustment, .
METHOD
take the spectrophotometric reading of a suitable
5.1 Outline of the Method portion of the solution.
The sample is subjected to the action of sodium hydroxide 5.3.3 Calibration Curve
and acidified with nitric acid-sulphuric acid mixture. The
yellow coloured complex produced in acid solution of Take a series of standard titanium solutions and the
the sample by the addition of hydrogen peroxide is reagent blank. Using the same quantities of the
determined photometrically at approximately410 nm. reagents carry through all the stages as described
under 5.3.2. Record the spectrophotom etric readings
5.2 Reagents of the standard solutions along with the blank. Draw
5.2.1 Sodium ~vdroxide Solution — 20 percent (ndv). a calibration curve by plotting the spectrophotomet-,
ric reading of the standard solutions against
5.2.2 Nitric Acid-Sulphuric Acid Mixtwe milligrams of titanium per 100 ml of the solution,
30
[S 504(Partll) :2002
Convert the spectrophotometric readings of the sam- 6.2.4.1 Titanium standard so/ution ( I ml = 10 pg Ti)
ple and the blank solutions to milligrams of titanium Pipette 10 ml of titanium standard solution ( 6.2.4) to
by means of the calibration curve and calculate the a 500-ml volumetric flask, dilute to volume and mix.
percentage of titanium.
6.3 Procedure
5.4 Calculation
6.3.1 Weigh accurately 0.250 g of aluminium sample
(in the form of drillings or millings) and transfer to a
Titanium, percent by mass = -$ x ~ 100 ml beaker, add slowly 5 ml hydrochloric acid (1: 1).
Heat to dissolve. Wash the sides of the beaker with
where minimum water. Add 3.75 ml of sulphuric acid (1:1)
A = mass in mg, of titanium found; and and mix. Add 1.25 ml of ascorbic acid and mix
thoroughly. Add 2-3 drops of copper sulphate solution
B = mass in g, of the sample taken,
and 2.5 ml diantipyrylmethane solution and mix.
6 DETERMINATION OF TITANIUM BY
6.3.2 Transfer quantitatively the contents of the beaker
SPECTROPHOTOMETRIC METHOD USING
to 25 ml standard flask and make up the volume with
DIANTIPYRYLMETHANE
water and mix. Wait for 15 min for colour development
6.1 Outline of the Method to complete.
6.3.3 Measure the absorbance of the complex at
Titanium in the sample is converted into Ti4+ which 380 nm on a spectrophotometer using 10 mm glass
in the presence of chromotropic acid forms a yellow cell against reagent blank.
coloured complex with diantipyrylmethane between
the pH range 1.8 to 2.4. Absorbance of the coloured 6.3.4 Reagent blank is prepared by following the
complex is measured at 280 nm. procedure specified in 6.3.1 (except aluminium
sample) to 6.3.3.
NOIT — The elements ordinarily present in the aluminium and
6.3.5 Read the titanium concentration from the
its alloys do not intertkrc. Interference of Fe3’ is eliminated by
calibration curve.
reducing it is Fez+ by ascorbic acid in the sample solutions prior
to colour development.
6.4 Calibration Curve
6.4.1 Pipette 1,2,3,4,5 and 6 ml of titanium standard

6.2 Reagents ,...
solution (6.2.4.1) to a 25-ml standard flask in
6.2.1 Diantipytylmethane Solution sequence. Transfer 5 ml hydrochloric acid (1:1) and
3.75 ml sulphuric acid ( 1:1) and cool. Mix slowly by
Dissolve 5 g of diantipyrylmethane in hydrochloric swirling. Add 1.25 ml of ascorbic acid solution and
acid (5N) and make up with hydrochloric acid (5N) 2 to 3 drops of copper sulphate solution and mix
to 100 ml in a volumetric flask. Store the solution in a thoroughly. Add 2.5 ml ofdiantipyrylmethane reagent
polyethylene bottle and use a freshly prepared solution. solution and mix. Make up the volume with water and
6.2.2 Ascorbic Acid So[ution ( 20 gll)
mix. Leave the flask for 15 min after colour
development. Run the reagent blank.
Dissolve 2 g of ascorbic acid in water and make
6.4.2 Measure the absorbance of the coloured complex
up to 100 ml.
at 380 nm against reagent blank on a spectrophotometer
6.2.3 Copper ,Yulphu[e Solzition — 1.25 percent (m/v). using 10 mm glass cell. Plot the graph of absorbance
against concentration of titanium in pg.. This graph is
Dissolve 1.25 g of copper sulphate (CuSO~. 5H,0) in used for finding the titanium concentration in the
water and make up to 100 ml. samplz
6.2.4 Ti[anium S[andurd Sohttiojq ( I m I = 0.5 mg Ti) .,
6.5 Calculation
Dissolve 3.68 g of potassium titanyl oxalate
dihydrate [KzTiO(C30d)~. 2H,0] with 8 g of Titanium, percent by mass = *
ammonium sulphate in 100 ml su-lphuric acid. Heat
to dissolve and quantitatively transfer the contents to where
one Iitre volumetric flask, containing about 750 ml
water. Cool and make up to volume and mix. Take A4 = mass in p: of titanium found in the aliquot
necessary safety precautions while handling and taken; and
diluting sulphuric acid. m = mass. in g of the sample taken.
31
IS 504 (Part 12) :2002
Indian Standard
PART 12 DETERMINATION OF VANADIUM
(Second Revision)
1 SCOPE Dissolve 0.50 g of potassium perrnanganate in water
and make up to volume in 100 ml flask.
This standard (Part 12) describes the method for
determination of vanadium in the range from 0.005 5.2.2 N- Cinnamoyl 1-N Phenyl Hydroxylamine
to 0.02 percent in ahtminium and its alloys. (CPHA), 0.5 percent (m/v) in Chloroform
2 REFERENCES Weigh 0.50 g of N-Cinnamoyl-N-phenyl

hydroxylamine in a dry beaker, add 70 ml Chloroform
The Indian Standards listed below contain provisions and dissolve the salt. Transfer quantitatively in a dry
which through reference in this text, constitute 100 ml flask with Chloroform and makeup to volume
provisions of this standard. At the time of publication, with Chloroform.
subject to revision, and parties to agreements based 5.2.3 Dilute Hydrochloric Acid — 1:1 (v/v).
on this standard are encouraged to investigate the 5.2.4 Hydrochloric Acid r.d.=1: 16.
standards indicated below: 5.2.5 Chloroform
IS No. Title 5.2.6 Dilute Sulphuric Acid — 10 percent (v/v).
1070:1992 Reagent grade water (thirdrevisiorr) 5.2.7 Standard Vanadium Solution

1817:1961 Methods of sampling ofnon-ferrous 5.2.7.1 Standard vanadium solution A (500 pg/ml)
Weigh 0.5742 g of ammonium metavanadate and
3 SAMPLING
dissolve in water (allow to stand overnight to dissolve)
The sample shall be drawn and prepared in accordance transfer quantitatively to a 500 ml standard flask and
with IS 1817. make up to volume.
4 QUALITY OF REAGENTS Alternatively a little dilute sulphuric acid is added to

the salt and the solution is warmed gently to dissolve
Unless specified otherwise, analytical grade reagents the solution. Cool and make up to 500 ml in a flask.
employed for the test. 5.2.7.2 Standard vanadium solution — B (50 pg/ml)
Pipette out 20 ml of solution A in a 200 ml flask and
5 DETERMINATION OF VANADIUM BY
make up to volume with water and mix well. The
N-CINNAMOYL-N-PHENYL-HYDROXAMIC
solution should be prepared just before use.
ACID (SPECTROPHOTOMETRIC) METHOD
5.3 Procedure
5.3.1 Weigh accurately 0.500 g of sample (drillings
The sample is dissolved in dilute hydrochloric acid
or turnings) and transfer to a 250 ml beaker. Add
and is extracted with N-cinnamoyl-N-phenyl-
20 ml hydrochloric acid (1:1).
hydroxamic acid in chloroform. The absorbance of the
coloured extract is measured at 545 nm using a NOTE— If reaction is too vigorous, add a small amount of
distilled water down the sides of beaker to moderate the reaction.
spectrophotometer.
NOTE— Elements ordinarily present in alurninium metal do not 5.3.2 When reaction is complete place h on a hot plate
interfere, however, iron interferes during extraction, if present, in and (not to dryness) until salts crystallize
evaporate
high percentage in an alloy. out. Remove from the hot plate and wash down the
sides of beaker with 10 to 15 ml of water. Warm the
5.2 Reagents
solution on a hot plate to dissolve crystals.
5.2.1 Potassium Permanganate — 0.5 percent (m/v)
32
U&
.@’
IS 504 (Part 12) :2002
q
5.3.3 Remove from hot plate. Cool and transfer to 5.3.8.2 Follow rest of the procedure as specified ,,
in 5.3.4. f‘[
100 ml separating funnel with 5-10 ml of washings.
Add potassium pennanganate dropwise until a pink
5.3.8.3 Wash the funnel with 5 ml Chloroform twice
colour persists. Add 20 ml of hydrochloric acid and
and transfer all washings to the same 25-ml standard
mix well. ~%
“,!,,,
flask. Wash the funnel with little Chloroform and make
I.,1.
~.,*
5.3.4 Add 10 ml of hydrochloric acid and mix well. up the volume with Chloroform.
Add 20 ml CPHA solution (5.2.2) and mix well. Allow
5.3.8.4 Prepare a reagent blank by taking 10 ml
the organic layer to separate and after drying the stem
distilled water (in place of vanadium solution) and
of the funnel, carefully transfer the organic layer to a
following the procedure as given in 5.3.8.1 to 5.3.8.3.
clean and dry 25 ml standard flask with the help of a
small filter funnel. Repeat the extraction several times Measure the absorbance of the vanadium extract
until the organic layer is colorless and transfer the 5.3.8.3 against the reagents blank obtained in 5.3.8.4
extract into the same flask. using 10 mm glass cells at 545 nm.
5.3.5 Prepare a process reagent blank (without sample) 5.3.8.5 Plot the graph of absorbance against con-
and following the procedure as given in 5.3.1 to 5.3.4. centration of vanadium per 25 ml of chloroform extract.
This graph is used for finding the concentration of
5.3.6 Measure the absorbance of the sample extract in
vanadium in aluminium sample solution.
chloroform as obtained in 5.3.4 against a process
reagent blank at 545 nm using 10 mm glass cells. 6 CALCULATION
5.3.7 Find the concentration in ~g of the extract from
M
the calibration curve.
Vanadium, percent by mass= m ~ ,06
5.3.8 Calibration Curve
5.3.8.1 Pipette 5.0, 10.0 and 20.0 ml of vanadium where

solution (5.2.7.2) into three 100-ml flasks and make M= mass, in pg of vanadium obtained from
up to volume with water and mix. Pipette 10 ml the aliquot taken, and
solution of these into three different 10-ml separating m= mass, in g of the sample taken.
funnels. Add potassium permanganate solution
(0.5 percent) dropwise until pink colour persists. “-.
33
IS 504( Parts 1 to 12) :2002
ANNEX A
(Foreword)
COMMITTEE COMPOSITION
Methods of Chemical/Instrumental Analysis of Non-Ferrous Metals Sectional Committee, MTD 28

Organization Representative (s)
Nuclear Fuel Complex, Hyderabad Stnu SY,4h4smDm (Chairman)

Bhabba Atomic Research Centre, Mumbai DR M. SUDSRSANAN
Smu M. M. Rmmrwtdurcmv (Alterrute)
Bharat Aluminium Co Ltd, Korba Smu K. P. Pm

(Alternate)
StrsuTHIAGARAJAN
Bharat Heavy Electrical Ltd, Hyderabad Sma S. Bmssarrm
Binani Zinc Ltd, Binanipuram Smr B. B.Mr

(Alternate)
SscwN. SRINNASAN
Central Electrochemical Research Institute, Karaikudi DR C. O. AUGUSIM
Control lerate of Metals, Ichapur SHRlS.K. KHILNANEV

SmI E.V. lbo (Akernute)
Defence Metraliurgical Research Laboratory, Hyderabad StrmS. V. Amwvu

DR (M@ Rmcrmrr Dt?srrum(Alternate)
Hindalco Industries Ltd, Renukoot SHSUD. D. MISm

DRY. V. RMWANA(Alternate)
Hhdustan Copper Ltd, Khetri DRSHVAMW

India Government Mint, Mumbai SHRrs. s. SAHA
Indian Aluminium Co Ltd. Kolkata SHSUs imutmxmGtmA
Indian Copper Development Centre, Kolkata LRM. Vrswmwmm
Indian Lead Zinc Development Centre, New Delhi StauL.Rmmmnw
Indian Metals and Ferro Alloys Ltd, Tberubeli DsiR.N.Mnwv
SrtroP.C~ (Alternate)
.lawabadal Nehru Ahrminium Research and Development, Centre, Nagpur IX K. V. KRM0L04
Stuu P. Durwosw (Alternate)
Mishra Dhatu Nigam Ltd, Hyderabad b M. KRISHNAMUMHV

SsuuR. P. TIwmY (Alternate)
Multimetals Ltd, Kota SHRIRAIESHD.moms
National Aluminium Co Ltd, Angul SHRIP. R. PAw’rm,4r4
National Institute ot_Foundry and Forge Technology, Rancbi DRH. S. MOHANTV

StrruP. T. Pussrr (Alterrrute)
National Metallurgical Laboratory, Jamshedpur DR L. P. PANOEY

Suu K. K. GUPTA(Alternate)
National Test HoLIse, Ghaziabad SHRIB. M. SGDD

.%rruP. MUZUMDAR(Alternate)
Ordnance Factory, Katni DRA. S. BALGtR

Smu J. Z. WARADE(Alternde)
RDCIS, (SAIL), Ranchi SW J, BANERJEE

Regional Research Laboratory, Thiruvaoanthapuram MO
DRT. PRASAOA
Saru Smelting (P) Ltd, Meerut SHRIDsm.m Jm

SW S. C. Smmm (Alternate)
Shriram Institute of Industrial Research, Delhi SHRIAVINASH

KUMAR
.%au L.B. SRNASJAVA(Alternate)
Durgapur Steel Plant (SAIL), Durgapur Sr+ruK. Goswmn

%ro R. P. &mA (Alternate)
The Institute oflndian Foundrymen, Pune Ssw MANESH.%
The Indian Smelting & Refining Co Ltd, Mumbai SHRIG. M. KRWLNAMURIHY
}31SDirectorate General SHRIN. MITRA,DIRECTOR

ANOHEm (MTD)
[Representing Director General (Ex-oficio Member)]
Member-Secretary
SHIUA. S. Jmnwmnxm
Director (MTD), BIS
34
Free Standard provided by BIS via BSB Edge Private Limited to Swaptul Enterprises - . A
A...l.l
Bureau of Indian Standards
BIS is a statutory institution established under the Bureau of Indian Standards 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 t~ copyright be addressed to the Director (Publications), BIS.
Review of Indian Standards i

I
Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed
periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are
needed; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standards
should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of
‘BIS Catalogue’ and ‘Standards: Monthly Additions’.
This Indian Standard has been developed from Doc : No. MTD 28 (3887).
Amendments Issued Since Publication
Amend No. Date of Issue Text Affected
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June 2002 Price Group 11

Methods of Chemical/ Instrumental Analysis of Non-Ferrous Metals Sectional Committee, MTD 28

IS 504 (part 1) :2002

4 QUALITY OF REAGENTS Take 1000 g aluminium wire of purity 99.9 percent

1S 504 (Part 1) :2002

of the beaker with distilled water. To it add 5 ml of

blank. To each of it add 10 ml of aluminium solution

1S 504 (Part 1) :2002

7.2.12 HydrojZuoric Acid (40 percent)

IS 504 (Part 1) :2002

7.3 Procedure lead retained in the residue may be removed as

IS 504 (Part 1) :2002

under 7.3.5 to a 100 ml Nessler tube. Add water to 8.4 Calculation !4

IS 504 (Part 2) :2002

2 REFERENCES 5.2.21-10 Phenanthroline Solution (0.25 percent)

Dissolve 1 000 g of aluminium metal (purity

5 DETERMINATION OF IRON BY 5.2.5 Stock Iron Solution (1 000 mg/1)

1S 504 (Part 2) :2002

5.3 Procedure complete mixing. It is desirable to add a small volume

5.3.5 Calculation 6.2.6 Phosphoric-Sulphuric Acid Mixture

In a cleaned 1-Iitre beaker take 500 ml of distilled

1S 504( Part 2):2002

10 ml phosphoric–sulphuric acid mixture and 5-8 where

10ml ml~f bichromate consumed x FX 100”

2 REFERENCES 5.2.5 Hydrogen Sulphide Wash Solution

4 QUALITY OF REAGENTS 5.2.12 Sodium Sulphate — Solid.

1S 504 (Part 3) :2002

of dilute sulphuric acid (1:1) and 8 to 10 ml of solution, and

Copper, percent by mass = X x ~

6.2.20 Sulphurous Acid 6.3.4 Calculation

Saturate water with sulphur dioxide. Prepare fresh as AxB

IS 504 (Part 3) :2002

4 QUALITY OF REAGENTS 5.2.7 Standard Zinc Solution ( 1 ml= 0.01 mg of Zn)

IS 504 (Part 4) :2002

5.4 Calculation 6.2.9 Formic Acid Wash Solution

6.2.11 Nitric Acid — rd. = 1.42.

where 6.2.13 Methylated Spirit

IS 504 (Part 4) :2002

6.4.2 Calculation B = volume in ml, of the standard potassium

IS 504 (Part 5) :2002

IS 504 (Part 6): 2002

IS No. Title 5.2.9 Hydrochloric Acid — rd. = 1.16.

265:1987 Hydrochloric acid (third revision) 5.2.10 Ammonium Sulphide Solution

3 SAMPLING 5.2.11 Ammonium Persu[phate — Solid.

IS 504 (Part 6) :2002

IS 504 (Part 6) :2002

IS 504 (Part 7) :2002

gas. Add 5 ml of nitric acid, and boil to oxidize iron. dimethylglyoxime,

IS 504 (Part 8) :2002

Unless specified otherwise, analytical grade reagents 5.3 Procedure

sulphate will reduce about 0.01 g of chromium). Ti- where

(vlN, - V*N*) x 1.734 perrnanganate solution used;

1S 504 (Part 9) :2002

IS 504 (Part 9) :2002

apparatus as shown in Fig. 1. Start passing slow cur-

(A- B)CXIOO 500.m 1

IS 504 (Part 10) :2002

curve and calculate the percentage of antimony. where

5.4 Calculation A = mass in mg, of antimony found in the sam-

(vlN, - VN) x 1.734 perrnanganate solution used;