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IS 13840-3 (1993): Chemical analysis of ferro titanium,Part 3: Determination of titanium by cupferron(gravimetric) method [MTD 5: Ferro Alloys]

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IS13840( Part31 :I993

Indian Standard

CHEMICAL ANALYSIS OF FERROTITANIUM PART 3 DETERMINATION OF TITANIUM BY CUPFERRON

( GRAVIMETRIC ) METHOD

UDC 669’15’782-198 : 543’21 [ 546’82 ]

@ BIS 1993

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

NEW DELHI 110002

September 1993 Price Group 2

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

FOREWORD

This Indian Standard ( Part 3 1 was adopted by the Bureau of Indian Standards, after the draft finalized by the Methods of Chemical Analysis of Ferrous Metals Sectional Committee had been approved by the Metallurgical Engineering Division Council.

IS 1559 : 1961 ‘Methods of chemical analysis of ferroalloys’ covers the chemical analysis of’ different ferro alloys, namely, ferrosilicon, ferrochromium, ferromanganese and speigeleisen, silicomanganese, ferromolybdenum, ferrophosphorus, ferrotitanium, ferrovanadium and ferro- tungsten. While reviewing this standard the Sectional Committee decided that a separate series for each ferro alloy be prepared. Accordingly, IS 1559 in its various parts was published for the methods of chemical analysis of ferrosilicon.

The methods of chemical analysis of various constituents of ferromolybdenum and ferrochromium are covered in a series ofparts of IS 12614 and IS 13452 respectively. ferrotitanium is covered in a series of parts of this standard.

The chemical analysis of

the analysis of relevant constituent prescribed With the publication of these parts

for ferrotitanium in IS 1559 : 1967 will be superseded. This part covers the method for determination of titanium by the gravimetric: method. The other parts of this series are:

Part 1 Determination of carbon by the-direct combustion ( gravimetric > ‘method

Part 2 Determination of silicon by gravimetric method

Part 4 Determination of aluminium

Part 5 Determination of sulphur

During this revision the method for determination of titanium by the cupferron ( gravimetric ) method has been updated.

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 : lS60, ‘Rules for rounding off numerical values ( revised )‘.

IS 13840(Psrt3):1993

Indian Standard

CHEMICAL ANALYSIS OF FERROTITANIUM PART 3 DETERMINATION OF TITANIUM BY CUPFERRON

( GRAVIMETRIC ) METHOD

-1 SCOPE

This standard ( Part 3 ) describes the method for determination of titanium in the range from 20 to 75 percent in ferrotitanium by cupferron ( gravimetric ) method.

2 REFERENCES

The following Indian Standards are necessary .adjuncts to this standard:

IS No. Title

264 : 1976 Nitric acid ( second revision )

266 : 1977 Sulphuric acid ( second revision )

!I070 : 1992 Laboratory grade water ( third revision )

,I472 : 1977 Methods of sampling of ferroalloys for determination of chemical composition (first revision )

3 SAMPLING

The sample shall be drawn and prepared in accordance with the method prescribed in IS 1472 : 1977.

4 QUALITY OF REAGENTS

Unless specified otherwise, analytical grade reagents and distilled water ( see IS 1070 : 1992)

-shall be employed for the test.

5 DETERMINATION OF TITANIUM

5.1 Outline of the Method

The sample is dissolved in sulphuric acid, nitric acid and hydrofluoric acid. Hydrogen sulphide

‘separations are made in acid and alkali tartarate media. Titanium is then precipitated with cupferron, ignited and weighed as oxide. Corrections are applied for vanadium and zirconium, if present.

-5.2 -Reagents

5.2.1 Dilute Sulphurfc Acid, 1 : 1, 1 : 4 and 1 : 9 (( v/v )

.5.2.2 Hydrojluoric Acid, 40 percent

52.3 Nitric Acid, rd = 1’42 ( conforming to dS 264 : 1976 )

5.2.4 Turtmic Acid Solution ( 500 g/l)

Dissolve 500 g of tartaric acid in water and make up to one litre.

5.2.5 Hydrogen Sulphfde, gas

5.2.6 Hydrogen Sulphide Wash Solution

Add 20 ml of dilute sulphuric acid ( I : 1 ) to 20 ml of tartaric acid solution ( 5.2.4 ) and dilute the solution to one litre. Saturate it with hydrogen sulphids gas.

5.2.7 Ammonium Hydroxide, rd = 0’90

5.2.8 Ammonium Sulphide Wash Solution

Dissolve 20 g of ammonium chloride and 10 g of ammonium tartarate in 500 ml of water. Add ammonium hydroxide in slight excess, dilute to one litre and saturate with hydrogen sulphide gas.

5.2.9 Cupferron Solution, 6 Percent

Dissolve 6 g of cupferron in 80 ml of cold water, dilute to 100 ml and filter. Prepare fresh as required.

5.2.10 Cupferron Wash Solution

Dilute 20 ml of cupferron solution ( 5.2.9 ) to one litre with cold dilute sulphuric acid ( 1 : 9 ).

5.2.11 Potassium Bisulphatc, solid

5.2.12 Hydrogen Peroxide, 20 volumes

5.2.13 Ammonium Phosphate Solution ( 10 per- cent

Dissolve 100 g of diammonium hydrogen phosphate in water and dilute to one litre. Filter before use.

5.2.14 Sulphuric Acid, rd = 1’84 ( conforming to IS-266 : 1977 )

5.2.15 Perchloric Acid, 70 percent ( v/v )

5.2.16 Phosphoric Acid, 85 percent ( v/v )

5.2.17 Ammonium Nitrate Solution ( 50 g/l )

Dissolve 50 g of ammonium nitrate in water and dilute to 1 litre.

1

IS 13840(Part 3):1993 .

5.2.18 Iron Standard Solutfon ( 1 ml = 1’0 mg 1 050” to 1150°C for 20 minutes. Cool and weigh- Fe ) as oxides of titanium with other impurities. The

Transfer 0’20 g of iron ( purity 99’8 percent ) to ignited residue may contain oxides of vanadium. and zirconium, and therefore their mass shall be

a 250 ml beaker. Add 10 ml hydrochloric acid ( 1 : 1 ) and 1 ml bromine water. After dissolution,

deducted from the mass of impure titanium dioxide.

add 10 ml of sulohuric acid and heat to conious fumes. Cool, dilute and make up to 200 ml: 5.3.4.1 Estimation of ZrOa

5.2.19 Titanium Standard Solution ( 1 ml = 0’10 mgTi)

Fuse 0’17 g of titanium dioxide, in a covered platinum crucible with 15 g of potassium bisulphate. Cool the melt and dissolve in 200 ml of hot dilute sulphuric acid ( 1 : 1 ) stirring occasionally. Cool, transfer to a 1 000 ml volumetric flask. Dilute to volume and mix.

5.3 Procedure

5.3.1 Weigh 0’500 g of sample and transfer to a 100 ml platinum dish. Cover and add 5 ml of dilute sulphuric acid ( 1 : l.), 5 ml of hydro- fluoric acid ( see Note) and sufficient nitric acid dropwise to effect dissolution. Remove and rinse the cover and sides of the dish. Evaporate to dryness and cool. Add 30 ml of d ilute sulphuric acid ( 1 : 4 ), stir well, heat for a few minutes and transfer to a 400 ml beaker. Heat until all sulphates have dissolved. Dilute to 200 ml, add 20 ml of tartaric acid solution and pass a brisk current of hydrogen sulphide for at least 20 minutes.

NOTE - 10 ml of the hydrofluoric acid shall be taken, if silicon is over 10 percent.

5.3.2 If a precipitate forms, filter through a paper containing paper pulp, into a 600 ml beaker. Wash about 20 times with hydrogen sulphide wash solution. To the filtrate, or to the clear solution If filtration was unnecessary, add paper pulp and make alkaline by adding ammonium hydroxide in slight excess. Pass a brisk current of hydrogen sulphide through the solution for at least 7 minutes and filter as soon as the precipitate settles, through a medium textured filter paper containing paper pulp, into a 800 ml beaker. Wash the paper ar,d the precipitate about 20 times with ammonium sulphide wash solution. Preserve the paper and the precipitate.

5.3.3 Boil the filtrate for about 10 minutes, then add 25 ml of dilute sulphuric acid ( 1 : 1 ) and boil down to 150 ml. Cool at 15 to 2O”C, then add a little paper pulp and a slight excess of cold, freshly prepared cupferron solution. Stir well and filter through two superimposed medium textured filter papers containing a little paper pulp and supported in a Buchner funnel using moderate suction. Wash about 20 times with cold cupferron wash solution.

5.3.4 Ignite the paper and the precipitate in a weighed platinum dish, first at a low temperature to bura off carbonaceous matter and finally at

Fuse the oxides ( 5.3.4 ) with about 5 g of potassium bisulphate and dissolve the cold melt in 70 ml of dilute sulphuric acid ( 1 : 9 ). Add 5 ml of hydrogen peroxide and 25 ml of filtered diammonium hydrogen phosphate and allow’ to stand overnight at a temperature of 70°C stirring occasionally during precipitation.

Filter through a medium textured filter paper, containing paper pulp. Wash about 20 times with dilute hydrochloric acid ( 2 : 98 ) and finally about 5 times with ammonium nitrate solution. Ignite in a weighed platinum crucible, first at a, temperature not over 600°C until the carbonaceous matter has burnt off, and finally at 1050” to 1 100°C to constant mass. Cool and. weigh as ZrPzO,. Calculate Z,rO, as follows:

ZrPzO, X 0’464 7 = ZrOz

5.3.4.2 Estimation of Vz03

Weigh accurately 1 g of the ferrotitanium sample in a platinum dish. Treat with 20 ml of dilute sulphuric acid ( 1 : 1 ), 5 ml of hydrofluoric acid and sufficient nitric acid dropwise to effect dis- solution of sample. Evaporate until dense white fumes just begin to evolve, cool and rinse into a 600 ml beaker containing 25 ml of boric acid’ solution. ~Dilute to 200 ml, add 40 ml of nitric acid and boil for 1 h or longer so that the final volume will be 100 to 125 ml. Dilute to 300 ml with cold water. Cool to 10°C and titrate potentiometrically with 0’20 N ferrous ammonium sulphate solution. Calculate any vanadium found to Vz03 as follows:

V X 1’785 1 = VzOa

5.3.5 Place the paper and the precipitate of ferrous sulphide ( reserved under 5.3.2 ) to the beaker. Add 25 ml of nitric acid, and 10 ml each of sulphuric acid and perchloric acid. Evaporate to dense white fumes to destroy all organic matter. Add 100 ml of water and digest until salts are in solution. Transfer to a 200 ml volumetric flask, dilute to the mark and mix thoroughly.

Transfer a portion of the solution to a blank cell of a spectrophotometer. To the remaining solution in the volumetric flask add 1 ml of hydrogen peroxide and mix thoroughly. Fill the other cell with the solution. Measure the absorbance against the blank at 425 nm. Read the amount of titanium from the calibration curve.

2

IS 13840 ( Part 3 ) -: 1993

5.3.6 Calibration Curve

Transfer 0,2,5, IO and 20 ml of standard titanium solution ( 1 ml = !I’1 mg Ti ) to 200 ml volu- metric flask. Add 15 ml of standard iron solution and 80 ml of sulphuric acid ( 1 : 9 ). thtd lm;:kof hydrogen peroxlde and make up to

. MIX thoroughly. Measure the absorbance of the solution, against the first mentioned solution as 425 nm. Plot the absobance readings against mg of titanium per 200 ml of solution.

5.4 Calculation

TibayDgzspercent = ( A x 0.599 5 ) + B x loo C

where A = mass in g, of titanium dioxide

corrected for ZrOB and VzOa; B = mass in g, of titanium from

ferrous sulphide precipitate, ( 5.3.5 ); and

C = mass in g, of the sample taken.

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