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भारतीय मानक IS 228 (Part 3) : 2024

Indian Standard

इस्पात के रासायनिक निश्ले षण की पद्धनतयााँ

भाग 3 क्षारनितीय पद्धनत द्वारा फास्फोरस का
निर्ाारण
( चौथा पनु रीक्षण )

Methods for Chemical Analysis of

Steels
Part 3 Determination of Phosphorus by
Alkalimetric Method
( Fourth Revision )

ICS 77.080.20

© BIS 2024

भारतीय मानक ब्यरू ो

BUREAU OF INDIAN STANDARDS
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NEW DELHI - 110002
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Methods of Chemical Analysis of Metals Sectional Committee, MTD 34

FOREWORD

This Indian Standard (Part 3) (Fourth Revision) was adopted by the Bureau of Indian Standards after the draft
finalized by the Methods of Chemical Analysis of Metals Sectional Committee had been approved by the
Metallurgical Engineering Division Council.

This standard was first published in 1952 and subsequently revised in 1959, 1972 and 1987.This revision has been
brought out to bring the standard in the latest style and format of the Indian Standards.

This part covers method for the determination of phosphorus content of plain carbon steel and alloy steels by
alkalimetric method. The other parts of this series are:

Part 1 Determination of carbon by volumetric method (for carbon 0.05 to 2.50 percent)
Part 2 Determination of manganese in Plain-carbon and low alloy steels by arsenite method
Part 4 Determination of total carbon by gravimetric method (for carbon ≥ 0.1 percent)
Part 5 Determination of nickel by dimethylglyoxime (gravimetric) method (for nickel ≥ 0.1 percent)
Part 6 Determination of chromium by persulphate oxidation method (for chromium ≥ 0.1 percent )
Part 7 Determination of molybdenum by alpha-benzoinoxime method in alloy steels (for molybdenum
> 1 percent and not containing tungsten)
Part 8 Determination of silicon by the gravimetric method (for silicon 0.05 to 5.00 percent)
Part 9 Determination of sulphur by evolution method (for sulphur 0.01 to 0.25 percent)
Part 10 Determination of molybdenum by thiocyanate (photometric) method in low and high alloy steels
(for molybdenum 0.01 to 1.5 percent)
Part 11 Determination of total silicon by reduced molybdosilicate spectrophotometric method in carbon
steels and low alloy steels (for silicon 0.01 to 0.05 percent)
Part 12 Determination of manganese by periodate spectrophotometric method in plain carbon, low alloy
and high alloy steels (for manganese 0.01 to 5.0 percent)
Part 13 Determination of arsenic
Part 14 Determination of carbon by thermal conductivity method (for carbon 0.005 to 2.000 percent)
Part 15 Determination of copper by thiosulphate iodide method (for copper 0.05 to 5 percent)
Part 16 Determination of tungsten by spectrophotometric method (for tungsten 0.1 to 2 percent)
Part 17 Determination of nitrogen by thermal conductivity method (for nitrogen up to 0.04 percent)
Part 18 Determination of oxygen by instrumental method (for oxygen 0.01 to 0.100 0 percent)
Part 19 Determination of nitrogen by steam distillation method (for nitrogen 0.02 to 0.50 percent)
Part 20 Determination of total carbon and sulfur content — Infrared absorption method after combustion
in an induction furnace (routine method)
Part 21 Determination of copper by spectrometric method (for copper 0.02 to 0.5 percent)
Part 22 Determination of total hydrogen in steel by thermal conductivity method (hydrogen 0.1 ppm to
50 ppm)
Part 23 Determination of total nitrogen in steel by optical emission spectrometer (nitrogen 0.002 to
1.0 percent)
Part 24 Determination of nitrogen in steel by inert gas fusion — Thermal conductivity method (nitrogen
0.001 to 0.2 percent)

(Continued on third cover)

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IS 228 (Part 3) : 2024

Indian Standard
METHODS FOR CHEMICAL ANALYSIS OF STEELS
PART 3 DETERMINATION OF PHOSPHORUS BY ALKALIMETRIC
METHOD
( Fourth Revision )

1 SCOPE 5.1.2 Potassium Permanganate Solution

This standard (Part 3) covers method for Dissolve 2 g of potassium permanganate in 100 ml
determination of phosphorus content of plain carbon of water.
steel and alloy steels by alkalimetric method.
5.1.3 Sodium Nitrite Solution ― 5 percent (m/v)
2 REFERENCES
5.1.4 Concentrated Ammonium Hydroxide ―
The standards given below contain provisions, relative density 0.90
which through reference in this text, constitute
provision of this standard. At the time of the 5.1.5 Concentrated Nitric Acid ― relative density
publication, the editions indicated below were valid. 1.42 (conforming to IS 264)
All the standards are subject to revision, and parties
to agreement based on this standard are encouraged 5.1.6 Ammonium Molybdate Solution
to investigate the possibility of applying the most
recent edition of these standards: Add Solution A (see 5.1.6.1) slowly and with
constant stirring to Solution B (see 5.1.6.2) kept cool
IS No. Title in a cold waterbath. Add 10 ml of ammonium
IS 264 : 2005 Nitric acid ― Specification phosphate solution (1 g/l) and keep the solution at
(third revision) least for 24 h. Filter the solution through Whatman
filter paper No. 40 before use.
IS 265 : 2021 Hydrochloric acid ―
Specification (fifth revision) 5.1.6.1 Solution A
IS 1070 : 2023 Reagent grade water ―
Specification (fourth revision) Dissolve 100 g of molybdic acid
(MoO3, 85 percent), or 118 g of ammonium
molybdate in a mixture of 145 ml of ammonium
3 SAMPLING
hydroxide (rd = 0.90) and 270 ml of water. Cool the
solution.
The samples shall be drawn and prepared as
prescribed in the relevant Indian Standard. 5.1.6.2 Solution B
4 QUALITY OF REAGENTS Add 490 ml of concentrated nitric acid to 1 150 ml
of water and cool.
Unless specified otherwise, analytical grade
reagents and distilled water (see IS 1070) shall be 5.1.7 Potassium Nitrate Solution ― 1 percent (m/v)
employed in the test.
5.1.8 Phenolphthalein Solution ― 1 percent
5 OUTLINE OF THE METHOD
Dissolve 1 g of powder phenolphthalein in 100 ml
Phosphorus is converted to orthophosphoric acid of rectified spirit or methyl alcohol.
and precipitated as ammonium phosphomolybdate.
The precipitate is dissolved in known excess of 5.1.9 Sodium Hydroxide Solution ― 0.1 N
standard sodium hydroxide solution and the excess
is titrated against standard nitric acid solution. Dissolve 4.5 g of sodium hydroxide in one litre of
freshly boiled and cooled distilled water and
5.1 Reagents
standardize against standard nitric acid (see 5.1.10).
5.1.1 Dilute Nitric Acid ― 1 : 1, 1 : 3, 1 : 5 and
2 : 98 (v/v)
To access Indian Standards click on the link below:
https://www.services.bis.gov.in/php/BIS_2.0/bisconnect/knowyourstandards/Indian_standards/isdetails/

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5.1.10 Standard Nitric Acid Solution ― 0.1 N 6.4 Warm the solution to about 60 °C to 80 °C and
add 50 ml of ammonium molybdate solution,
Dilute 7 ml of concentrated nitric acid to one litre stopper the flask, shake vigorously for a few minutes
with freshly boiled distilled water. Standardize and allow to stand for half an hour.
against sodium carbonate previously ignited at
350 °C and cooled. 6.5 Filter the precipitate through a filter paper pulp pad
by suction. Wash the flask, precipitate and filter pad
5.1.11 Dilute Hydrochloric Acid ― 1 : 1 (v/v) and twice with 5 ml portions of dilute nitric acid
2 percent (v/v) (2 : 98) and five times with 5 ml portions of potassium
nitrate. Continue washing of the precipitate and filter pad
5.1.12 Hydrofluoric Acid ― 40 percent with potassium nitrate solution until the washings are
acid free (10 ml portion of the washings in presence of
5.1.13 Perchloric Acid ― 70 percent phenolphthalein should turn pink on adding one drop of
0.1 N sodium hydroxide solution).
5.1.14 Sodium Carbonate ― 5 percent (m/v)
6.6 Transfer the pulp along with the precipitate to
5.1.15 Ferrous Sulphate Solution the flask. Add about 25 ml of water, few drops of
phenolphthalein and a known volume of sodium
Dissolve 100 g of ferrous sulphate crystals hydroxide solution (which should be 1 ml to 2 ml in
(FeSO4.7H2O) in one litre of dilute sulphuric acid excess) and shake to dissolve the precipitate. Dilute
(5 : 95). to about 100 ml and titrate with standard nitric acid
solution to the disappearance of pink colour.
5.1.16 Dilute Ammonium Hydroxide ― 1 : 1,
1 : 20 (v/v) 7 PROCEDURE FOR ALLOY STEELS

5.1.17 Sulphurous Acid 7.1 Stainless Steel, High Chromium, Nickel

Chromium and Similar Alloy Steel without
Saturate water with sulphur dioxide gas. Tungsten or Vanadium

5.1.18 Concentrated Hydrochloric Acid ― relative Transfer 2 g of the sample in a 400 ml beaker. Add
density 1.16 (conforming to IS 265) 50 ml of a 1 : 1 mixture of concentrated hydrochloric
acid and nitric acid and a few drops of hydrofluoric
5.1.19 Dilute Hydrobromic Acid ― 1 : 4 (v/v) acid. Place the beaker at low heat until the reaction
subsides and then add 15 ml of perchloric acid.
6 PROCEDURE FOR PLAIN CARBON STEEL Evaporate to copious fumes and fume for a few
AND LOW ALLOY STEEL WITHOUT minutes. Cool, take up with 40 ml of water and
VANADIUM 10 ml of concentrated nitric acid, boil for few
minutes, filter through paper pulp and wash with hot
6.1 Transfer 2 g of the sample in a 250 ml conical dilute nitric acid (1 : 5). Collect the filtrate in 500 ml
flask. Add 30 ml of dilute nitric acid (1 : 1) till the conical flask and proceed as in 6.2 to 6.6.
vigorous reaction subsides. Keep the flask at low
heat till it dissolves. 7.2 Steel Containing High Silicon, Titanium or
Zirconium
6.2 Add 5 ml to 10 ml of potassium permanganate
solution and boil for few minutes. If manganese 7.2.1 Follow the procedure given in 7.1 up to
dioxide does not precipitate add further filtration and proceed as follows.
permanganate solution till a precipitate of
manganese dioxide appears and boil for few 7.2.2 Collect the filtrate in a 500 ml conical flask and
minutes. Add sodium nitrite solution dropwise till preserve it. Take the precipitate and pulp (as in 7.1)
the brown precipitate is dissolved. Boil to expel in a platinum crucible and ignite, fume with 1 ml
oxides of nitrogen. hydrofluoric acid and a few drops of concentrated
nitric acid at low temperature. Fuse the residue with
6.3 Add ammonium hydroxide till brown precipitate sodium carbonate. Dissolve the melt in water, filter
of ferric hydroxide appears. Dissolve the precipitate through paper pulp and wash with sodium carbonate
adding dilute nitric acid (1 : 1) drop wise and add solution. Acidify the filtrate with concentrated nitric
2 ml to 3 ml of concentrated nitric acid. acid and add to the main filtrate. Proceed further as
NOTE ― Quantity of nitric acid added at this stage will
in 6.2 to 6.6.
depend upon the actual volume of the solution. The analyst
will ensure that the acidity of the solution before
precipitation of phosphomolybdate complex is maintained
at 5 percent to 10 percent.

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7.3 Chromium Vanadium Steels or other Steels 7.5 Austenitic Manganese Steels
Containing Vanadium but no Tungsten
Decompose 2 g of the sample in a 400 ml beaker in
7.3.1 Proceed as in 7.1 when the solution is ready for 40 ml of dilute nitric acid (1 : 3). Add 15 ml of
the precipitation of phosphomolybdate complex. perchloric acid and evaporate just to white fumes.
Add hydrofluoric acid drop by drop until all the
7.3.2 Cool the solution to 10 ºC to 20 ºC, add 5 ml hydrated silica is dissolved and a few drops in
of ferrous sulphate solution and 2 to 3 drops of excess. Heat so that perchloric acid refluxes on the
sulphurous acid and shake to mix well. Add 50 ml sides of the beaker for about 25 min. Cool, add about
of ammonium molybdate solution, stopper the flask, 40 ml of water and 10 ml concentrated nitric acid
shake vigorously for a few minutes and allow to and boil for few minutes. Proceed further as in 6.2
stand overnight. Proceed further as in 6.5 to 6.6. to 6.6.

7.4 High Speed Steels or Other Steels Containing 7.6 Steels Containing High Arsenic up to
Tungsten with or without Vanadium 0.1 Percent

7.4.1 Transfer 2 g of the sample to a 400 ml beaker. Decompose 2 g of the sample in 400 ml beaker in
Decompose the sample in 60 ml of dilute nitric acid 40 ml of dilute nitric acid (1 : 3). Add 20 ml of
(1 : 3) and a few drops of hydrofluoric acid, if perchloric acid and fume to expel nitric acid. Cool,
required. Add 20 ml concentrated hydrochloric acid add about 80 ml of dilute hydrobromic acid and
60 ml concentrated nitric acid and few drops of evaporate to copious fumes. Cool, add about 40 ml
hydrofluoric acid and evaporate to dryness. Digest of water and 10 ml nitric acid. Proceed further as in
with 20 ml of concentrated hydrochloric acid, dilute 6.2 to 6.6.
to 50 ml with water and boil. Filter through a paper
pulp as far as possible by decantation, keeping back 8 BLANK DETERMINATION
the precipitate of tungstic acid in the beaker. Wash
twice with hot dilute hydrochloric acid (2 percent). Make a blank determination following the same
Collect the filtrate in a 500 ml conical flask and procedure and using the same quantity of all
evaporate to a small volume. Add 30 ml reagents.
concentrated nitric acid, and evaporate to syrupy
liquid. Add 5 ml concentrated nitric acid, dilute to 9 CALCULATION
about 25 ml and boil for a few minutes.
9.1 Calculate phosphorus, percent, as:
7.4.2 To recover phosphorus from the precipitate of (𝐵 – 𝐴) × 𝐶
tungstic acid, dissolve the precipitate in the beaker Phosphorus (percent) = × 100
𝐷
with minimum quantity of dilute ammonium
hydroxide (1 : 1) and pour it through the filter pad where
collecting the solution in a beaker, wash the beaker B = millilitres of standard nitric acid solution
and the filter pad with dilute ammonium hydroxide required in the blank determination
(1 : 1) until all of the tungstic acid has been dissolved (see 8);
and collected. Add a few ml of the main filtrate (end
of 7.4.1) to this solution and slightly acidify with A = millilitres of standard nitric acid solution
dilute nitric acid (1 : 1). Add dilute ammonium required in the sample in the titration of
hydroxide (1 : 1) in slight excess and heat to the excess sodium hydroxide (see 6.6);
flocculation. Filter through Whatman filter paper C = phosphorus equivalent of 1 ml standard
No. 42 and wash with dilute ammonium hydroxide nitric acid solution; and
(1 : 20). Dissolve the precipitate in minimum hot
dilute nitric acid (1 : 5) and add to the main filtrate D = quantity of sample, in g.
(7.4.1).
9.2 Reproducibility
7.4.3 Treat the filtrate as in 6.2 and 6.3. If the sample
contains vanadium, proceed further as in 7.3.2. In the ± 0.001 5 percent.
absence of vanadium, complete the determination as in
6.4 to 6.6.

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IS 228 (Part 3) : 2024

ANNEX A
(Foreword)
COMMITTEE COMPOSITION
Methods of Chemical Analysis of Metals Sectional Committee, MTD 34
Organization Representative(s)
CSIR - National Metallurgical Laboratory, Jamshedpur DR SANCHITA CHAKRAVARTY (Chairperson)

Arcelor Mittal Nippon Steel, Mumbai SHRI MANOJ GUPTA

SHRI KIRIT TAILOR (Alternate)

Bhabha Atomic Research Centre, Mumbai MS SANJUKTA A. KUMAR

SHRI M. V. RANA (Alternate)

CSIR - National Metallurgical Laboratory, Jamshedpur DR ASHOK K. MOHANTY

Defence Metallurgical Research Laboratory, Ministry of SHRI S. S. KALYAN KAMAL

Defence, Hyderabad

Directorate General of Quality Assurance, Ministry of SHRI A. MITRA

Defence, New Delhi SHRI D. KARTIKEY (Alternate)

Dr Jawaharlal Nehru Aluminium Research Development DR UPENDRA SINGH

and Design Centre, Nagpur

Geological Survey of India, New Delhi SHRI NITIN PURUSHOTTAM

SHRIMATI SANJUKTA DEY PAL (Alternate)

Hindalco Industries Limited, Mumbai SHRI KRISHANU MAHAPATRA

SHRI ASHUTOSH ACHARYA (Alternate)

Indian Metals and Ferro Alloys Limited, Bhubaneswar SHRI DINESH KUMAR MOHANTY

JSW Steel Limited, Mumbai SHRI KOTRABASAVARAJU

SHRI MARULASIDDESHA U. M. (Alternate)

National Aluminium Company Limited, Bhubaneswar SHRIMATI SUKLA NANDI

SHRI DEBANANDA BHATTACHARYYA (Alternate)

National Test House, Kolkata DR RAJEEV KUMAR UPADHYAY

SHRI AKBAR H. (Alternate)

Shriram Institute for Industrial Research, Delhi DR LAXMI RAWAT

SHRI PUNEET KAPOOR (Alternate)

Steel Authority of India Limited - Salem Steel Plant, SHRI L. SIVAKUMAR

Salem SHRI VIVEKANANDHAN G. (Alternate)

Tata Steel Limited, Kolkata DR JATIN MOHAPATRA

DR RAVIKRISHNA CHATTI (Alternate)

BIS Directorate General SHRI SANJIV MAINI, SCIENTIST ‘F’/SENIOR DIRECTOR

AND HEAD (METALLURGICAL ENGINEERING)
[REPRESENTING DIRECTOR GENERAL (Ex-officio)]

Member Secretary
SHRI ASHISH PRABHAKAR WAKLE
SCIENTIST ‘C’/DEPUTY DIRECTOR
(METALLURGICAL ENGINEERING), BIS

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(Continued from second cover)

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, is to be rounded off, it shall be
done in accordance with IS 2 : 2022 ‘Rules for rounding off numerical values (second revision)’. The number of
significant places retained in the rounded off value should be same as that of the specified value in this standard.
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should ascertain that they are in possession of the latest amendments or edition by referring to the website-
www.bis.gov.in or www.standardsbis.in.
This Indian Standard has been developed from Doc No.: MTD 34 (21384).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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