Indian Standard

IS 228 {Part 7 ) : 1990 ( Rednned 1996 )

METHODS FOR CHEMICAL ANALYSIS OF STEELS

PART 7 DETERMINATION OF MOLYBDENUM BY ALPHA-BENZOINOXIME METHOD IN ALLOY STEELS (FOR MOLYBDENUM > 1 PERCENT AND NOT CONTAINING TUNGSTEN)

( Third Revision )

Second Reprint NOVEMBER 1998

UDC

669.131.7-14CO83.77)

@l BIS 1990

BUREAU
MANAK

OF INDIAN
BHAVAN,

STANDARDS
ZAFAR MARG

9 BAHADUR SHAH NEW DELHI 110002

September

1990

Price Group

Methods of Chemical

Analysis of Ferrous Metals Sectional Committee,

MTD 2

FOREWORD This Indian Standard ( Part 7 ) ( Third Kevision > was adopted by the Bureau of Indian Standards on 23 February 1990, after the draft finalized by the hlethods of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical Ehgineering Division Council. IS 228 which was first-published in 1952 and subsequently revised in 1959, covered the chemical analysis of plain carbon and low alloy steels, alongwith pig iron and cast iron. It was revised again to make it comprehensive in respect of steel analysis and to exclude pig iron and cast iron which are being covered in separate standards. During its second revision, the standard was split up in several parts and 14 parts have already been published covering only chemical analysis of steels. This standard updated. IS 228 ( Part 7 ) was published in 1974. In this third revision, the part has been

In reporting the results of a test or analysis made in accordance with this standard, if the final value, observed or calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 Rules for rounding off numerical values ( revised).

IS228(Part7):1990

Indian Standard METHODS FOR CHEMICAL ANALYSIS OF STEELS

PART 7 DETERMWATION OF MOLYBDENUM BY ALPHA-BENZOINOXIME METHODIN ALLOY STEELS (FOR MOLYBDENUM > 1 PERCENT AND NOT CONTAINING TUNGSTEN ) ( 1 SCOPE 1.1This standard (Part 7 ) covers the alphabenzoinoxime method for determination of molybdenum content in low alloy and high alloy steels containing molybdenum above 1 percent and no tungsten.
2 REFERENCES 2.1 The following Indian Standards necessary adjuncts to this standard. ISJVO. 264 : 1976 265,: 1987 Specification revision ) Title for nitric acid (second acid are

Third Revision)
5.2.4 Boric Acid Solution, 4 percent. 5.2.5 Potassium Bisulphite, Solid.

5.2.6 Ferrous Sulphate Solution, 5 percent. Dissolve 5 g of ferrous sulphate in water containing 5 ml of sulphuric acid and dilute to 100 ml. 5.2.7 Alpha-Bentoinoxime Solution, 2 percent

Dissolve 2 g of alpha-benzoinoxime in 100 ml of ethanol. Filter if the solution is not clear. 5.2.8 Bromine Water Saturate 100 ml of water with bromine, adding 1 to 2 ml of bromine at a time till few drops of it remain undissolved. 5.2.9 SulpiucricAcid-Benzoinoxime Wash Solution

Specification for hydrochloric ( third rer&ion )

3 SAIVIPLING 3.1 The samples shall be drawn and prepared as prescribed in the relevant Indian Standards. 4 QUALITY

OF REAGENTS
water shall be employed

To 1 litre of dilute sulphuric acid ( 1 : 99 ), add 5 ml of alpha-benxoinoxime solution ( 2 percent ) . 5.2.10 Dilute Ammonium Hydroxide and 1 : 99 (u/o). Solution, 1 : 1 rd 116 1 : 50

4.1 Unless. specified otherwise, analytical grade

reagents and distilled in the test.

5 D3YBRNINAl?ON OF MOLYBDENUM BY ALPHA4BENZOINOYSIME METHOD 5.1 Outline

5.211 Concentrated Hydrochloric Acid, ( conforming to IS 265 : 1987 ). 5.2.12 Dilute Hydrochloric Acid, (r/v). 5.2.13 Tartaric Acid, solid.

1 : 1 and

of the Method

Molybdenum is preciptated with alpha-benxoinis ignited at oxime, .and the .precipitate 500~525C and weighed as Moos. 5.2 Reagents-

5.2.14Hydrogen Sulphide, gas.

5.2.15 Hydrogen &&hide Wash Solution acid ( 1 : 99 ) with

5.2.1Dilute Sulphuric Acid, 1 : 1, 1 : 4 and 1 : 6

(v/r)* 5.2.2 Concentrated flitric Acid, forming to IS 264 : 1976 ). rd = 142 ( con-

Saturate dilute sulphuric hydrogen sulphide. 5.2.16 Cinchonine Solution Dissolve 10 g cinchonine 100 ml of dilute hydrochloric 1

5.2.3 HydrqPouric Acid, 40 percent.

hydrochloride acid ( 1 : 1 ).

in

IS228(Part7):19!M 5.2.17 Cinchonine Wash Solutipn Dilute 30 ml with water. 5.3 Procedure 5.3.1 Dissolve 100 to 300 g of sample in 50 ml dilute sulphuric acid ( 1 : 6) in a 400-ml beaker and warm till the reaction ceases. Add drop by drop concentrated nitric acid to decompose carbides and to oxidise iron and molybdenum. Boil to expel the nitrous fumes. Add 2 to 4 drops of hydrofluoric acid and allowto react. Add 10 ml of boric acid solution. Boil for a few minutes. Dilute to 100 ml. Filter and wash with hot dilute hydrochloric acid ( 1, : 99 ). Ignite the filter paper at low temperature ( below 500C ), fuse with potassium bisulphite and dissolve in water. Add to the filtrate. 5.3.2 Dilute to 100 ml. Cool to about 10C. Add 10 ml of ferrous sulphate solution. Add a few pieces of ashless paper pulp and stir, and add slowly 10 ml of alpha-benzoinoxime solution with constant stirring. (Add 5 ml more for each 001 g of molybdenum, followed by the addition of sufficient bromine water to impart a pale yellow colour to the solution and finally 3 to 4 ml more of the reagent ). Allow the solution to remain in the cooling mixture for 10 minutes, while stirring occasionally. Filter through a medium textured ashless filter paper. If the filtrate is not clear, filter through the same filter paper. Wash six to seven times with cold sulphuric acid-benxoinoxime solution. 5.3.3 Transfer the precipitate and paper to a weighed platinum crucible, dry and ignite at 500-525X to constant mass and weigh (A). Dissolve the oxide in 5 to 10 ml of dilute ammonium hydroxide solution ( 1 : 1 ), digest and wash the residue with hot dilute ammonium hydroxide solution ( 1 : 99 ). Ignite the residue in the same platinum crucible and weigh (B). The difference of weight ( A - B) represents the weight of MoOa. 5.3.4 If the ammonical filtrate is blue in colour, indicating the presence of copper; estimate copper by diethyl dithiocarbamate - spectrophotometric method. 5.3.5 For Tungsten Steel of cinchonine solution to 1 litre for one or two minutes and allow to settle for 15 minutes. Filter through a paper pad and wash the residue thoroughly with dilute hydrachloric acid ( 1 : 50 ) and twice with hot water. Reserve the [Link] washings (Fr ). [Link] Digest the precipitate ( [Link]) with 30 ml of diiute ammonium hydroxide solution ( 1 : 1 ), filter and wash with dilute ammonium hydroxide ( 1 : 99). Add 5 g of tartaric acid to the filtrate. Neutralize the solution with dilute hydrochloric acid ( 1 : 1) and add about 10 ml of concentrated hydrochloric acid. Dilute to 100 ml and warm: Pass the hydrogen sulphide gas under pressure. Filter and wash with hydrogen sulphide wash solution. Discard the filtrate. Ignite the residue at 599-525C. Cool and dissolve in 20 ml of dilute ammonium hydroxide solution ( 1 : 1 ) [Link]. Mix the filtrate with the filtrate Fi obtained in [Link]. Dilute the combined filtrate to 290 m and follow the procedure as specified in 5.3.2 and 5.3.3. S-3.6 For High Silicon Steel [Link] Take 100 g of the sample, add 10 ml of concentrated hydrochloric acid and a few drops of concentrated nitric acid dropwise. Evaporate to syrupy consistency. To further dehydrate, add 5 ml of concentrated hydrochloric acid, evaporate and bake. Cool and add 5 ml of concentrated hydrochloric acid and dilute to 100 ml. Boil for one or two minutes and allow to settle for 15 minutes. Filter through a filter pad and wash the residue thoroughly with dilute hydrochloric acid ( 1 : 50 ) and then twice with shot water. Reserve the filtrate and washing ( Fs ). [Link] Ignite the residue in a platinum crucible at a temperature 500-525X. Cool and add 2 ml of dilute sulphuric acid ( 1 : 4) and 2 ml of hydrofluoric acid. Evaporate to fumes and add another 2 ml of hydrofluoric acid and Cool, dilute with water, evaporate again. warm again and filter through filter pad. Add this filtrate to the filtrate F, obtained in 53.6.1. Dilute the combined filtrate to 200 ml and follow the procedure as specified in 5.32 and 5.3.3. 6 CALCULATION 6.1 Calculate follows: the molybdenum content as

[Link] Take 100 g of the sample and add 10 ml of concentrated hydrochloric acid. Heat till Add concentrated nitric acid reaction subsides. in small quantity and digest till bright yellow Evapbprecipitate of tungstic oxide is formed. rate to syrupy consistency. Repeat the evaporation once more with 5 ml of concentrated hydrochloric acid. Add 5 ml of concentrated hydrochloric acid and dilute to 100 ml. Boil 3

Molybdenum, percent by mass where A -B c

= - (A --B)

x 667 C

= mass, in g, of molybdenum oxide obtained under 5.3.3, and = mass, in g, of the sample taken for the test.

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