( Reaffirmed 2004 )

tndian Standard
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
P A R T 10 DETERMINATION OF MOLYBDENUM BY THIOCYANATE
(PHOTOMETRIC) METHOD IN LOW AND HIGH ALLOY STEELS
( FOR MOLYBDENUM 0'0t T O 1-50 PERCENT)

( Third Revision )

(~ )
T s;T~?W
T
Fint Reprint JUNE 1991

UDC 669'15-194'2/'3 : 543.24 [ 546'77 1

@ BIS 1990
B U R E A U OF I N D I A N S T A N D A R D S
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHl 110002
Met& of Chemical Analyds of Fvrotu Metals Sectional Committea, Ml'D 2

FOREWORD
?his Indian Standard (Part 10) ( Third Rcviiton ) war adoptud by the Bureau of Indian Standards
on 22 December 1989, after the draR 6naliied by the Methods of Chemical Analyds of Ferrous
Metals Sectional Committee had becn approved by the Metadurgicd Engineering Division
Council.
IS 228 which was flrat published in 1952 and ~ b ~ e q ~ e nrevised
t l y in 1959, covered the chemical
analysis of plain carbon and low alloy steals, alongwith pi iron and can iron. Thisstmdard w u
again revised to make it comprehensive in respast of r t d annlyais and to exclude pi iron and
caat iron which are bein covered in separate standards. 14 parn have already &en issued
f
covering only chemical ana pis of steel#.
Tbis standard IS 228 ( Part 10) war published in 1976. I n this revidon the wave length at which
_
the intensity of the molybdenum complex u mruured has been modified and the rtproducibflity
of the method haa been inmpqratsd.
I n reporting the result8 of a test or analyak made in accordance with this standard, if the anal
value, observed or calculated, h to be rounded off, it shall be done in accordanw with IS 2 : 1960
'Rules for rounding off numerical value^ ( noirrd 1'.
 Indian Standard
METHODS FOR
CHEMICAL ANALYSIS OF STEELS
PART 10 DETERMINATION OF MOLYBOLNUM OY THIOCYANATE
(PHOTOMETRIC) METHOD IN LOW AND nlan ALLOY STEELS
(FOR'YOLYODENUM 0'01 T O 1.50 PERCENT)

( Third Revision )
1 SCOPE 53.3 Dihk Su@huric Acid, 1 : 1 and 1 : 5 ( u/v ).

1.1 This standard (Part 10) covers the method 52.4 Potar~itun Thimyanals Solulimr, 100 g/litre in
for the determination of molybdenum in the water.
range 0'01 to 1'50 rcent by thiocyanate
(photometric) matho rin low and high alloy 5.2.5 Stannous Chlmon&
Solution ( 100 g/l )
steels.
Dissolve 20 of stannous chloride dihydrate
6
( SnCl,, 2H, ) in 25 ml concentrated hydro-
chloric acid ( rd = 1'16) with gentle stirring.
2.1 The following Indian Standard is a necea-
sary adjunct to this standard: and dilute to 200 ml with water. Ad a few J'.
Heat to 60 to 70°C to dissolve complete1 Cool
pieces of metallic tin and store in a stoppered
IS No. TiIh bottle.
265 : 1987 Specification for hydrochloric
acid ( thitd rroirion )

S.1 Samples shall be drawn and prepared aa

prescribed in the relevant Indiin Standard.
52.8 Standard MoIJbdnum Solution ( 1 ml
mg Mo
- 0'01

4 QUALITY OF REAGENTS Transfer 0'100 0 g of molybdenum metal ( 9'99

ed otherwisq an.lytical rade
rSsclfi
Unienan di&lled water &all be emp eyed
t
in t e test.
5D-ATION OF MOLYBDENUM
BY TIlIOQPAruATz (PEOToMgTRIO)
METHOD
Sam e aliquot u treated with thiocyanate to
dl'
d w op molybdenum and iron c o m p l u e and
reduced with stannous chloride. Molybdenum
complex u extracted with butyl acetate and
meuured at 470 nm.
150 ml of phosphoric acid ( r d -
To 700 ml d panhloric acid ( rd = 1'67 ) add
1'70) and
150 ml of nitric acid ( r d P 1'42). Mix
thoroughly while adding the acids.
S2.2 C o m a l r d &&ochloric Acid, rd
(conforming to IS 265 :1987).
percent pure) to a 250 ml conical flank apd
dissolve in 10 ml concentrated hydrochloric acid
't and 10 ml water. Add' 1 ml of concentrated
nitric acid and heat to dissolution. Cool, dilute
to 1 litre in a volumetric flask. Take 100 ml of
this solution and dilute to 1 litre with water.
5.3 Procedure
5.3.1 Traafer 0'500 g of the sample to a 250 ml
conical fk*.Add 25 ml of the acid mixture.
Heat gently to d i l v e the sample. Evaporate
the solution till firma of perchloric acid evolves
and continue heating further till all the
chromium, if pruent, is oxidisad. Add d r o p h e
conwntrated hydrochloric acid till moat of the
chromium is volatilised. Cool, add 50 ml of
dilute sulphuric acid ( 1 : 1 ), heat to boiling ( to
expel any free chlorine ) and cool. Tramfu the
solution to a 100 ml volumetric flask and dilute
to mark with water. Mix thoroughly.
5.33 Pipette out a suitable aliquot containing
0'05 to 0'1 mg molybdenum into a 250 ml
separating funnel. Add 15 ml of potassium
= 1'16 thiocyanate solution and 15 ml of stannoua
chloride solution. Mix thoroughly after each
addition. Add 25 ml of butyl acetate, nopper taken u blank and the haorb- d u r are
and hake vigorody for one minute. Allow the plotted y a i n n milligram of molybdenum.
phuea to separate. Remove the rtopper and
drain out the aqueous p b w . Add to the organic
layer 50 ml of dllute rulphwic acid ( 1 :5 ), 5 ml
of potassium tlaioc mate and 5 ml of numoo, Dedu* the abwrbmee value of blank from the
chloride solution. Jtopper and ahake vigorously test mlution m d the cnlibration curve. Rnd out
for one minute. Allow the ph.ru to reporate the of mdybd.wm p r a m t in the aliquot
and drain off the aqueour l a y 6 and discard. portion of the teat rducioll taken. Cdculate the
p e m t . g e of molybdenum u follow:
5.3.3 Collect the organic hue in a funad after
d
paaiing through a dry ter paper. T r u u b r a
suitable portion of butyl acetote n ref-
Molybdenum, percent
by m u -
- - xA 1
aolution to a 1 cm cell and m-e tbe B 10
rborbance of t a t laluion a g a h t it at 470 nm.
where
A man in of Mo in the aliquot
Carry out a blank detarminadon using all the
7
porrion o the t a t se~utieqa d
reagents and 0'5 g iron instaad of the umple.
Record the h r h o e s of the btrrL wlurioo
using butyl acetate aa reference solution.

Take 0'5000 of iron in eath of seven 250 ml f 0'005 at 0'05 percant level
4r
conica1 &rL. ransfex 0,1,2,4,6, 8 a d 10 ml
of atandad molybdenum d u t i o n ( 1 ml = 001 f 0'02 at 0'15 parcent level
mg Mo) to each of these. Add 25 ml of theacid f 0'04 at 0'5 percent level
mixture and roceed ar apaci6ed in S.S.1
i'
to 533. The a J containing ssro d of Ma h i 0'06 a t 1 perant level
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Act, 1986and the Rula and R.gulatiom made thereunt;er. The Standard Mark on producta
covered by an Indian Standard convaya the amurance that they have been produced to comply with
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harmonious development of the lotivitia ofrtandardi9tion. marking and quality miecation oF
goods and attending to wancctcd rmttcn in the country.

BIS hsr the copyright of all its publications. No part of thew publications may ba reproduosd in
any form without the prior permiasion in writing of BIS. This does not preclude the free ure.in
the course of implememiu the Uandard, of ncceuuy details, auch as symbola and sizes, type or
grade dcrignationa. Enquidw relatins to wpyright be addre~edtothe Ditsctor (Publications), BIS.

Indian Standards are reviewed periodially and rwised, when newrruy and amuaendmentr, if any,
are iasued from time to time. U m of Indiin Standardr rhould u a r t d n that they are in porlada
of the latest amendmentd or edition. Cornmenu on this Indian Standard may be mat to BE3
dving the following reference :
Doc :No. MTD 2 ( 3541 )
Amdmeuts Irma Slow h b l l a t t m

Awnd No. Date of larue Text Affected

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