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IS 228-5 (1987): Methods of chemical analysis of steels,

Part 5: Determination of nickel by dimethyl glyoxime
(gravimetric) method (for nickel greater than or equal to
0.1 percent [MTD 16: Alloy Steels and Forgings]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
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“Knowledge is such a treasure which cannot be stolen”
 IS : 228 (Part Q-1987
( Reaffirmed 1997
( Reaffirmed 2002) )

Indian Standard
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
PART 5 DETERMINATION OF NICKEL BY
DIMETHYLGLYOXIME (GRAVIMETRIC) METHOD
(FOR NICKEL)O~l PERCENT)

( Third Revision )
Third Reprint OCTOBER1998

UDC 669’1%194.2/*3
: 543’21[546*74]

Q Copyright 1987

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAPAR MARO
NEW DBLHI 1loooZ

Gr 3 August 1987
 IS : 228 ( Part 5 ) - 1987

Indian Standard
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
PART 5 DETERMINATION OF NICKEL BY
DIMETHYLGLYOXIYE (GRAVIMETRIC) METHOD
(FOR NICKEL > 0’1 PERCENT)

( Third Revision)

Methods of Chemical Analysis of Ferrous Metals

Sectional Committee, SMDC 2

Chairman Repesmting
DR C. S. P. IYER Bhabha Atomic Research Centre, Bombay

M#fIlb#W
Sunr G. M. APPABAO Steel Authority of India Ltd ( Bhilai Steel Plant ),
Bhilai
Snnx R. D. A~ABWAL ( Allnnalc )
SHBI S. V. BEA~WAT Khandelwal Ferro Alloys Ltd, Nagpur
SERI D. N. GUPTA ( AZ~crauZr)
S~HI P. CHAKRA Indian Metals & Ferro Alloys Ltd, Koraput
CHE~ST & METALL~B~I~T Ministry of Transport ( Department of Railways )
AIWSTMT REBEABCH OBPIOEB
(MET-2) RDSO, LV~KNOW
( Alternate )
CEIEB CHPYIST Tata Iron & Steel Co Ltd. Jamshedpur
ASSISTANT CHIEF CHEMIST ( Ahnatr )
SBRI M. K. CHAKRAVA~TY Ministry of Defence (DGI)
SRRI P. K. SEN ( Attrrnata )
DH M. M. CHAKRABORTY Indian Iron & Steel Co Ltd, Burnpur
SERI M. S. CHATTEBJLE ( Aftsrnatr )
SERI C. K. DIKBHIT Ordnance Factory Board ( Ministry of Defence ).
Calcutta
Sam S. N. MOITRA ( Altnnotr)
SHRI V. B. KBANNA Directorate General of Supplies 8t Dirposals,
New Delhi
9nn1 J. N. MVKEERJEE Steel Authority of India Ltd ( Durgapur Steel
Plant ), Durgapur
( Continuedon pap 2 )

Q Copyighf 1987
BUREAU OF INDIAN STANDARDS
This publication is protected under the Zadiaa Coplright Act ( XIV of 1957) and
reproduction in whole or in part by any means except with written permtion of the
publisher shall be deemed to be an infringement of copyright under the said Act.
IS : 228 ( Part 5) - 1987
( Centinucd/rempugt I )

Md8TJ Rqmmting
Sanx P. NARAIN Mahindra Ugine Steel Co Ltd, Bombay
SARI G. R. SIRMA ( Alfrmatr )
SHRI N. P. PANDA Steel Authority of India Ltd (Rourkela Stee
Plant ), Rourkela
SBHI B. MASIAPATRA( Alfrrnala)
Da L. P. PANDEY National Metallurgical Laboratory ( CSIR)
NatcJa;;hedPur
DR D, C. PflAaXAR Physical Laboratory (CSIR j
New Delhi
SHRI J. RAI ( Altwarr )
SHRI G. RAJANAO Ferro Alloyr Corporation Ltd, Shreeramnagar
SARI K. RAMAPRIBRNAN Essc-n & Co, Bangalore
DR J. RAJAIXAM( AIlrrnolr )
SHRXA. P. SINHA Steel Authority of India Ltd (Bokaro Stec
Plant ), Bokaro
SBRI K. ANWIAH ( Alfrrnatr )
SARI N. V. SUBBARAYAPPA Visveevaraya Sron & Steel Ltd, Bhadravati
DR P. SUBRAIIMANIAM Dcfence Metallurgical Rcrearch Laboratory
Hyderabad
SRR~ T. H. RAO ( Alfrr~f# )
DR CR. VRNXATEBWARLU Bhabha Atomic Research Centre Bombay
Snnx K. RAORAVENUI~AN, Director General, BIS ( Ex-o#cio Mamba )
Director ( Strut & Met )
S#nrto~
SHRI M. L. SHARMA
Atristant Diwctor ( Metalr ), BIS

Ferrous Metals Analysis Subcommittee, SMDC 2 : 3

Convenrr
DR C. S. P. IYER Bhabba Atomic Reeearcb Centre, Bombay

Mtmbrrr
Sa~x S. EA~~KARAN Bbarat Heavy Electricale Ltd, Hydcrabad
SHRI MATA SARAN ( Alfrr~t 1)
SERI B. RARA ( Alfrrnalr II )
SHRI U. P. Bean Stee~~$ority of India Ltd ( Bbilai Strel Plant )

SHRI E. M. Ve~xmmm ( Ahrnalr )

CHIEF CII~MIW Tata Iron & Steel Co Ltd, Jamshedpur
AUE:ETANTCntEp CBEWST ( Allrrnolr )
Da M. M. CHARRABORTY Indian Iron dr Steel Co Ltd, Burapur
SHRI L. N. DAN ( Ahmalt )
SHRI H. K. DAB Steel Authority of India Ltd (Rourksla Stee
Plant ).
,. Rourkela
SHRI K. Bra~~ot ( Altrmat~ )
SEYRIA, K. GUPTA National Physical Laboratory ( CSIR )
New Delhi
( Conttnwd ea pap 9

* 2
 IS t 228 ( Part 5 ) - 1987

Indian Standard
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
PART 6 DETERMINATION OF NICKEL BY
DIMETHYLGLYOXIME ( GRAVIMETRIC ) METHOD
( FOR NICKEL > 0’1 PERCENT)

( Third Revision )
0. FOREWORD
0.1 This Indian Standard ( Part 5 ) ( Third Revision ) was adopted by
the Indian Standards Institution on 16 January 1987, after the draft
finalized by the Methods of Chemical Analysis of Ferrous Metals
Sectional Committee had been approved by the Strtictural and Metals
Division Council.

0.2 IS : 228, which was issued as a tentative standard in 1952 and

revised in 1959, covered the chemial analysis of pig iron, cast iron and
plain carbon and low alloy steels. For the convenience it was decided
to publish a comprehensive series on chemical analysis of steels includ-
ing high alloy steels. Accordingly, revision of IS : 228 was taken up
and new series on methods of chemical analysis of steels
&zsing high alloy steels was published in various parts as IS : 228
( Parts 1 to 13 ) ( see Appendix A ) covering separate method of
analysis for each constituent in steels. However, IS : 228-1959* version
has been retained for the analysis of pig iron and cast iron till a
separate standard for analysis of pig iron and cast iron is published.
0.2.1 This revision of IS : 228 ( Part 5 )-1974t has been undertaken on
the basis of experience gained during the implementation of the
standard by the manufacturers and testing laboratories.

0.3 In this revision major modifications are:

a) scope of the method has been modified by lowering the limit
of nickel for determination from 0’5 to 0’1 percent, and
--_
*Methods of chemical analyric of pig iron, cmt iron and plain carbon md low alloy
Iterlc (rcuircd).
tMethod# of chemical analyG# of rtacla: Part 5 Determination of nickel by
iimetbylglyorime ( gravimetric ) method ( for nickel > 0’5 percent) ( wand rruision
).

3
IS t 228 ( Part 5 ) - 1987

1)) inclusion of reproducibility of the method at the various levels

of nickel content.

0.4 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*.

1. SCOPE

1.1 This standard ( Part 5 ) covers method for determination of nickel

content of low alloy and high alloy steels containing more than or equal
to 0’1 percent nickel.

2. SAMPLING

2.1 The samples shall be drawn and prepared as prescribed in the

relevant Indian Standard.

3. QUALITY OF REAGENTS

3.1 Unless specified otherwise, analytical grade reagents and distil!ed

water ( see IS : 1070-1977t ) shall be employed in the test.

4. OUTLINE OF THE METHOD

4.1 After complexing interfering elements, nickel in the solution of the

sample is precipitated as nickel dimethylglyoximate and weighed.

5. REAGENTS

5.1 Dilate Hydrochloric Acid - 1 : 1 and 1 : 19 ( v/v).

5.2 Dilute Nitric Acid- 1 : 1 (v/v).

5.3 Perchloric Acid - 70 percent.

5.4 Tartaric Acid Solution - 50 percent ( m/v ).

5.5 Dilute Ainmonium Hydroxide - 1 : 1 (v/v).

5.6 Dimethylglyoxime Solution - 1 percent ( m, u ). Dissolve 1 g of

the solid reagent in 100 ml of rectified spirit.

-;Ruler for rounding off numerical valuer ( revised ).

tSprcification for water for general laboratory use ( second rmirim ).

4
 IS:228(Part5)-1987

5.7 Ammoniacal Ammonium Nitrate Solution - Dissolve 1 g of

ammonium nitrate in 100 ml of water and make it slightly alkaline to
methyl red with dilute ammonium hydroxide.

5.8 Acid Mixture - Make up as follows:

Concentrated hydrochloric acid ( rd = 1’16 400 ml

conforming to IS : 265-1976’ )
Concentrated nitric acid ( rd == 1’42 180 ml
conforming to IS : 264-1976t )
Perchloris acid (rd = 1’56 ) 600 ml

Water 680 ml

5.9 Hydrofiuoric Acid - 40 percent.

5.10 Concentrated Hydrochloric Acid - Relative density 1’16

( conforming to IS : 265-1976* ).

6. PROCEDURE

6.1 For Low Alloy Steels - Weigh accurately about 2 to 3 g of the

sample for nickel < 0’5 percent and 1 g for nickel up to 5 percent
and transfer to a 400-ml beaker. Add 60 ml of dilute hydrochloric
acid(1 :l). Cover the beaker and digest till the decomposition is
complete. Add cautiously dropwise nitric acid. Boil until iron and
carbides are oxidized and brown fumes have been expelled. Add
15 to 20 ml of perchloric acid and fume, evaporate to syrupy
consistency.

6.1.1 Cool and add 100 ml of water. Heat to boiling, filter to remove
silica, if any, and wash with dilute hydrochloric acid ( 1 : 19 ). Cool
and dilute to 250-ml in a volumetric flask.

6.1.2 Take a suitable aliquot containing about 15 to 20 mg of nickel

and dilute to 200 ml. Add 10 to 15 ml of tartaric acid solution,
neutralize with dilute ammonium hydroxide and add 1 ml in excess.
If the solution is not clear, add more tartaric acid solutton and
neutralize with dilute ammonium hydroxide. Add dilute hydrochloric
acid (1 : 19) until slightly acidic and warm to 60 to 80°C. Add 25
to 30 ml of dimethylglyoxime solution ( too much reagent should not be
used ). Add dilute ammonium hydroxide until slightly alkaline ( avoid
addition of excess dilute ammonium hydroxide ). Keep the beaker on

*Specification for hydrochloric acid ( smnd rcvirion ).

tsoecification for nitric acid ( semndrctiim).
IS:!228(Part5)-1987

hot-plate at 6O’C with occasional stirring for 30 minutes. Cool to room

temperature.

6.1.3 Filter through previously cleaned, dried and weighed sintered

glass crucible No. 3, wash the precipitate with 10 ml cold ammoniacal
ammonium nitrate solution 6 to 8 times and then with the cold water.
‘When the precipitate has been washed, discontinue the suction and dry
the precipitate at 15O’C to constant weight. Cool in a desiccator and
weigh as nickel dimethylglyoximate.

6.2 For High Nickel and High Chromium Steels -Take 0’5 to
1 g of sample in a 400-ml be.lker, add 40 ml of the acid mixture and
heat gently first and when the sample has dissolved, allcw it to fume
and continue fuming for 7 to 10 minutes. In case the sample does not
dissolve, add few drops of hydrofluoric acid and fume, and cool, ’
dilute with 75 ml of water and filter. Wash the residue with dilute
hydrochloric acid (1 : 19). Collect the filtrate and washiugs in a
beaker, transfer to 250-ml volumetric flask and make up the volume of
the filtrate to 250 ml. Complete the determination as in 6.1.2 and 6.1.3.

6.3 For Tungsten Steels - If the steel contains tungsten, add 10 ml

concentrated hydrochloric acid to solution obtained under 6.1 and
dilute to 150 ml; add some ashless paper pulp, digest at 60°C and allow
the precipitate to settle and filter through aper pulp pad and wash
with hot dilute hydrochloric acid (1 : 19). 6 iscard the residue. Cool
the filtrate and dilute to a known volume with water. Follow further
the procedure given under 6.1.1 to 6.1.3.
NOTE-If appreciable cobalt ( over 1 percent ) or copper ( over 1 percent ) is
prenent, dialolve the precipitate obtained under 6.13 into the original beaker with
amall quantitv of alternate w-her of hot dilute hydrochloric acid and warm water.
Re-precipitate nickel aa under 6.1.2.

7. CALCULATION

7.1 Calculate the nickel content of the steel as follows:

A .’ 20’32
Nickel, percent = B

where

A = mass in g of nickel dimethylglyoximate in the aliquot,

and

B - mass in g of the sample or aliquot representing the

rample taken.

6
 IS I 228 ( Part 5) l 1987

7.2 Reproducibility
a) f 0’025 percent at 0’5 percent nickel and below,
b) f 0’050 percent for nickel between 0’5 to 5 percent,
c) f 0’120 percent for nickel between 5 to 10 percent, and
cl) f 0’160 percent for nickel above 10 percent.

APPENDIX A
( czuuse 0.2 )
INDIAN STANDARDS ON METHODS FOR CHEMICAL
ANALYSIS OF STEELS

IS : 228 Methods for chemical analysis of steels:

(Part 1 )-1972 Determination of carbon by volumetric method

( for carbon > 0’1 percent ) ( second rev&ion )
( Part 2 )-1972 Determination of manganese in plain carbon and
low alloy steels by arsenite method ( second revision )
( Part 3 )-1972 Det.ermination of phosphorus by alkalimetric
method ( second revision )
( Part 4)-1974 Determination of carbon by gravimetric method
( for carbon > 0’ 1 percent ) ( second revision )

( Part 5 )-I974 Determination of nickel by dimethyl lyoxime

ravimetric ) method ( for nickel > 0’5 percent 5 (second
Iefision )

( Part S)-1974 Determination of chromium by persulphate

oxidation method ( for chromium > 0’5 percent ) (second
revision )

( Part 7 )- 1974 Determination of molybdenum by a-benzoinoxime

method ( for molybdenum > 1 percent ) (second reubion)
( Part 8)-1975 Determination of silicon by the gravimetric method
( for silicon ) 0’1 percent ) ( second revision )

( Part 9 )-I975 Determination of sulphur in plain carbon steels by

evolution method (second revision )

7
IS : 228 ( Part 5 ) - 1987

(Part lo)-1976 Determination of molybdenum by thiocyanate

( photometric) method ( for molybdenum up to 1 percent )
in low and high alloy steels ( second revision )

(Part 11 )-1976 Determination of silicon by photometric method in

carbon steels and low alloy steels (for silicon 0’01 to
0’05 percent ) ( second revision )

( Part 12 )-1976 Determination of manganese by periodate

( photometric ) met;-.od in low and high alloy steels ( for
manganese up to 2 percent ) ( second revision )

(Part 13)-1982 Determination of arsenic

 IS : 228 ( Part 5) - 1987

( Cmtinarcdfran pap 2 )

Manbars Rcpe&wUin~
Smu J. MIJKHRRJEE Steel Authority of India Ltd (Durgapur Steel
Plant ), Durgapur
SHXI P. I;. BANEBJES ( Altrrnate 1
SERI P. NARMN kahindra Ugine Steel Co Ltd, Bombay
&RI G. R. t&UUA (Altematr)
SHEU R. S. NATE Steel Authority of India Ltd (Rokaro Steel
Plant ), Bokaro
SERI N. GUNDAPPA ( Aftrrmte )
DR L. P. PANIIEY National A*-tallurgical Laboratory ( CSIR ),
Jamshedpur
SHRI G. R~ntnnlr Vbvavaraya Iron & Steel Ltd, Bhadravati
S~nr R. D. VANUMWALLA Italab Pvt Ltd, Bombay
SARI J. C. DEY ( Aftmatr)

9
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