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IS 13840-4 (1998): Chemical analysis of ferro titanium,Part 4: Determination of aluminium by phosphate method [MTD5: Ferro Alloys]

Indian Standard

CHEMICAL ANALYSIS OF FERROTITANIUM PART 4 DETERMINATION OF ALUMINIUM BY CUPFERRON (GRAVIMETRIC) METHOD

ICS 77.100; 77.120.50

0 BIS 1998

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC

NEW DELHI I 10002

Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2

FOREWORD

This Indian Standard (Part 4) was adopted by the Bureau of Indian Standards, after the draft finalized hy the Methods of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical Engineering Division Council.

IS 1559: 196 I ‘Methods of chemical analysis of ferroalloys’ covers the chemical analysis of’ different ferro- alloys, namely, ferrosilicon, ferrochromium, ferromanganese and speigeleiscn, silicomanganesc, fr~rromolyhdenum, ferrophosphorus, ferrotitnnium, ferrovanadium and I’crrotungstcn. While reviewing this standard, the Sectional Committee decided that a scparatc series for each ferro alloy he prepared. Accordingly, IS 1559 in its various parts, was puhlished for the methods of chemical analysis of fen-osilicon.

The methods of chemical analysis of various constituents of ferromolyhdcnum and ferrochromium are covered in a series of parts of IS I2614 and IS 13452 respectively. The chemical analysis of ferrotitanium is covered in a series of‘ parts of this standard. With the publication of these parts, the analysis of relevant constituent prescribed for fcrrotitanium in IS 1559: 1961 will he superseded. This part covers the method for determination 01‘ aluminium hy cupferron (gravimctric) method. The other parts of this scrics arc.

Pal-1 I Dckrmination of carbon by the direct combustion (grnvimctric) method

Part 2 Determination of silicon by gravimetric method c

Part 3 Dctcrmination of titanium by the gravimetric method

Part 5 Dctcrmination of sulphur by direct combustion method

Pal-1 6 Dctcrmination of titanium by XRF method

During this revision, the method for dclcrmination 01’ aluminium hy cupl’crron (gravimetric) method has hccn updarcd.

For the ~LII-pox 01' clccidin, (7 whether a particular requirement of this standard is complied with. the I‘inal value, ohscrvccl or calculated, expressing the result of a test or analysis, shall hc rounded off in accordance with IS 2 : I960 ‘Rules for rounding off numerical values (~visetl)‘. The numhcr 01‘ signil‘icant places rctaincd in ~hc rounded off value should be the same as that of the specified value in this standard.

.

IS 13840 (Part 4) : 1998

Indian Standard

CHEMICAL ANALYSIS OF FERROTITANIUM PART 4 DETERMINATION OF ALUMINIUM BY CUPFERRON (GRAVIMETRIC) METHOD

1 SCOPE 5.2.6 Cupferron Wash Solution

This standard (Part 4) describes the method for determination of aluminium in the range from 1 to 10 percent in ferrotitanium.

Dilute 20 ml of cupferron solution (see 52.5) to 1 litre of cold dilute sulphuric acid (1:99).

5.2.7 Perchloric Acid, 70 percent. 2 REFERENCES

5.2.8 Ammonium Chloride, solid. The following Indian Standards are necessary adjuncts to this standard: 5.2.9 Bromocresol Purple, 0.2 g/50 ml water.

IS No.

264: 1976

1070:1992

1472: 1977

Title

Nitric acid (second revision)

Reagent grade water (third revision)

Methods of sampling of ferro- alloys for determination of chemical composition (first revision)

5.2.10 Ammonium Hydroxide Solution, 1:l (v/v).

5.2.11 Ammonium Chloride Wash Solution, 2 percent.

5.3 Procedure

3 SAMPLING

The sample shall be drawn and prepared as per the method given in IS 1472.

4 QUAL-ITY OF REAGENTS

Unless specified otherwise, analytical grade reagents and reagent grade water (see IS 1070) shall be employed for the test.

5 DETERMINATION OF ALUMINIUM

5.3.1 Weigh accurately 0.5 g of finily powdered sample and transfer to a 1OO~ml platinum dish. Add 20 ml of dilute sulphuric acid (1:l) and 5 ml of hydrofluoric acid. Add nitric acid drop by drop to effect dissolution. Cover and warm till reaction is over. Remove from hot plate, wash the cover and sides of the dish and evaporate to fumes at low temperature. Cool and add 50 ml of dilute sulphuric acid (1 : 9) or 50 ml of dilute hydrochloric acid ( 1: 1) and digest to dissolve salts. Transfer to 400-ml beaker, rinse and wash the dish. Cool below 5 to 10°C and add little -paper pulp. Slowly add freshly -pFepared cupferron solution (see 5.2.5) till the precipitation is complete and a little excess as seen by white colour of precipitate and stir vigorously for 2 to 3 min. Filter through medium texture filter paper. Wash thoroughly with cupferron wash solution (see 5.2.6). Reserve the filtrate.

5.1 Outline of the Method

Sample is dissolved in acid mixture, and after cupferron separation, aluminium is precipitated, filtered and ignited as oxide and weighed.

5.2 Reagents

5.2.1 Dilute Sulphuric Acid, 1:l and 1:9 (v/v).

5.2.2 Hydrojluoric Acid

5.3.2 Return the precipitate to the original beaker and add 10 ml of sulphuric acid and 50 ml of nitric acid and evaporate to fumes. Add more nitric acid, if necessary, and repeat the evaporation to oxidize all organic matter. Cool, add 100 ml of water and digest until all salts are in solution, Cool below 20°C and reprecipitate with cupferron solution, filter and wash as in 5.3.1. Combine this filtrate with that reserved in 5.3.1.

5.2.3 Nitric Acid, rd=l.42 (conforming to IS 264).

52.4 Dilute Hydrochloric Acid, 111 (v/v).

5.2.5 Cupferron Solution (6 percent)

Weigh 6 g of cupferron and dissolve in 80 ml of cold water. Dilute to IOO~ml, filter and prepare fresh.

5.3.3 To the combined filtrate add 40 ml of nitric acid and 20 ml of perchloric acid. Evaporate to fumes and remove all organic matters. If organic matter still remains, add 10 ml more of perchloric acid and fume again. Cool, dilute to 200 ml with water and add 5 ml of dilute hydrochloric acid (1: 1). Boil for 5 min and filter. Wash with water. Add 10 g of ammonium chloride, 5 drops of bromocresol purple indicator and ammonium hydroxide solution

IS 13840 (Part 4) : 1998

(1:l) till the colour changes to purple. Add paper pulp and boil for 1 min. Filter through a medium texture filter paper and wash thoroughly with ammonium chloride wash solution (2 percent).

Transfer the precipitate with paper to a beaker. Redissolve in 100 ml of dilute hydrochloric acid (1: 1) and add 10 g of ammonium chloride. Boil and carry out the precipitation and filtration, followed by washing as before. Dissolve precipitate in 50 ml HCl (1:3). Wash filters with hot water. To the filtrate, add 0.5 g (NH,) 2 HPO,, a little pulp and two drops of methyl red (0.4 g/l). Make first ammoniacal, restore pink colour by adding HCl(1: 19) drop by drop. Heat to boil, add 20 ml ammonium acetate (200 g/l). Continue boiling for 5 min, allow the precepitate for settle. Filter, wash with hot ammonium nitrate (50 g/l) till free of chloride. Ignite in a platinum/porcelain, crucible cover, heat at 1 000°C to constant weight. Weigh as aluminium phosphate.

5.3.4 Ignite the precipitate slowly, in a platinum crucible and then at 1 100°C to constant mass. Cool in a desiccator and weigh.

5.4 Calculation

(A-B) x 0.228 x 100

c - where,

A = weight of aluminium phosphate,

B = weight of blank solution, and

C = weight of sample.

5.4.1 Precision has to be established by analysing same sample in different laboratories.

Expected + 0.15 at 5 percent level.

2

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This Indian Standard has been developed from Dot: No. MTD 2(3794).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected c

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