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IS 1917-7 (2001): Chemical Analysis of Quartzite and HighSilica Sand, Part 7: Determination of Titania bySpectrophotometric Method [MTD 13: Ores and Raw Materials]

,~!

Indian Standard

CHEMICAL ANALYSIS OF QUARTZITE ANDHIGH SILICA SAND

PART 7 DETERMINATION OF TITANIA BY SPECTROPHOTOMETRIC METHOD

( First Revision)

ICS 71.040.50:73.080

. .

.

0 BIS 2001

BUREAU OF IN DIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

June 2001 Price Group 1

/

-. .?$

Methods of Chemical Analysis of Ores, Minerals and Allied Materials for Metallurgical Industry SectionalCommittee, MTD 29

FOREWORD

This Indian Standard (Part 7) (First Revision) was adopted by the Bureau of Indian Standards, after the draftfinalized by the Methods of Chemical Analysis of Ores, Minerals and Allied Materials for Metallurgical IndustrySectional Committee had been approved by the Metallurgical Engineering Division Council.

IS 1917:1962 ‘Methods of chemical analysis of quartzite and high silica sand’ covers the methods for thedetermination of silica and other constituents of quartzite and high silica sand. The committee decided to revisethis standard into different parts and covering determination of each element in a separate part, which onpublication would supersede the determination of that element given in IS 1917. The determination of loss onignition, silica, sodium, potassium, rduminium, iron, crdcium, magnesium and titanium oxide in quartzite andhigh silica sand have been covered in this series.

This part covers the determination of titania. The other parts in this series are:

Part 1 Determination of loss on ignition

Part 2 Determination of sodium and potassium

Part 3 Determination of silica

Part 4 Determination of aluminium

Part 5 Determination of iron

Part 6 Determination of calcium and magnesium

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance withIS 2:1960 ‘Rules for roundkg off numerical values (revised)’. The number of significant places retained inthe rounded off value should be the same as that of the specified value in this standard.

IS 1917 (Part 7) :2001

Indian Standard

CHEMICAL ANALYSIS OF QUARTZITE ANDHIGH SILICA SAND

PART 7 DETERMINATION OF TITANIA BY SPECTROPHOTOMETRIC METHOD

(First Revision)

1 SCOPE

This standard (Part 7) describes the method fordetermination of titania up to 0.2 percent.

2 REFERENCES

The following Indian Standards contain provisionswhich through reference in this text, constituteprovisions of this standard. At the time of publication,the editions indicated were valid. All standards aresubject to revision, and parties to agreements based onthis standard are encouraged to investigate thepossibility of applying the most recent editions of thestandards indicated below:

IS No. Title

1070:1992 Reagent grade water (third revision)

1811:1984 Methods of sampling foundry sands@rst revision)

2245:1962 Methods of sampling quartzite

3 SAMPLING

3.1 The sample shall be drawn and prepared afterquartering in accordance with IS 2245 or IS 1811 asthe case may be.

3.2 Grind 3 to 5 g of the sample so that it passesthrough IS sieve 150 microns opening. Dry the samplein a weighing tube at 105°C for 2 h. Keep the weighingtube stoppered in a desiccator and cool to roomtemperature. The sample is ready for chemicalanalysis.

4 QUALITY OF REAGENTS

Unless specified otherwise, analytical grade reagentsand distilled water (see IS 1070) shall be employed forthe test.

5 DETERMINATION OF TITANIA

5.1 Outline of the Method

An aliquot of the sample solution is treated withchromotrophic acid at pH 3.5, The orange colourproduced is measured with spectrophotometer at470 nm. The amount of titania is evaluated from thecalibration curve obtained under similar conditions.

Alternatively titania can be deka-mined by completingwith hydrogen peroxide at410 nm.

5.2 Reagents

5.2.1

5.2.2

5.2.3

5.2.4

5.2.5

Dilute Hydrochloric Acid, 1:1 (v/v)

Hydrojluoric Acid, 40 percent (v/v)

Sulphuric Acid, 95-97 percent, rd = 1.84

Potassium Bisulphate, solid

Chromotrophic Acid

Dissolve 0.5 g of chromotrophic acid in 100 ml ofdilute sulphuric acid (0.3 N) in a dark coloured bottle.

NOTE — The solution is stable for one week.

5.2.6 Ascorbic Acid, 10 percent (tiv).

5.2.7 Ferric Ammonium Sulphate Solution (1 ml=1 mg Fe)

Dissolve by heating 4.3 g of ferric ammonium sulphatein water, containing 10 ml of dilute sulphuric acid(1 : 1). Cool, filter and dilute to 500 ml in a volumetricflask.

5.2.8 Sodium Hydroxide Solution, 2 N

5.2.9 Buffer Solution (pH 3.5)

Dissolve 10 g of sodium acetate in water and adjustthe pH to 3.5 by adding acetic acid and dilute to1000 ml.

5.2.10 Standard Titania Solution (1 ml= 1 mg TiOz)

Dissolve 0.5 g of calcined titania in hydrofluoric acidin a platinum dish. Then add carefully 25 MI ofsulphuric acid and heat to strong fumes to removefluoride. Cool, dilute with cold water stirringcontinuously and make up to 500 ml in a volumetricflask. This will be 1000 ppm titania solution. Take50 ml aliquot and make up to 500 ml in a volumetricflask to get 100 ppm titania solution.

5.2.11

5.2.12

5.2.13

1

Sulphuric Acid, 1:3 (v/v), 1: l(v/v).

Orthophosphoric Acid, 1:3 (v/v).

Hydrogen Peroxide, 6 percent (v/v).

IS 1917 (Part 7) :2001

5.3 Procedure

53.1 Weigh accurately 1.000 g of the prepared sampleas per3L2 into a platinum crucible. First heat gently andthen raise the temperature slowly to 1 OOO°C.Finallyignite at 10OO°Cfor half an hour and cool.

53.2 To the residue (5.3.1) add slowly 5 ml of water, 2drops of sulphuric acid (1 : 1)and 20 ml of hydrofluoricacid. Cover the crucible with its lid and keep at roomtemperature for 10 min. Remove the lid and place it ona sand bath for evaporation of silica as SiF4and continueup to copious fuming. Cool the crucible and add further5 ml of hydrofluoric acid and repeat theproeess. Finallyignite the contents of the crucible containing theresidue at 1000”C for half an hour.

5.3.3 Fuse the residue with 4-5 g of potassiumbisulphate at low temperature and finally at highertemperature to get a clear melt. Cool and extract themelt with cold water and add 10 to 15 ml of dilutesulphuric acid (1: 1). Boil the extracted mass to get aclear solution. Cool and make up to 250 ml in avolumetric flask.

5.3.4 Take 5 to 10 ml of solution (5.3.3) in a 50-mlvolumetric flask. Add 2 ml of chromotrophic acidsolution and then 2 ml of ascorbic acid solution. Add5 ml of ferric ammonium sulphate solution andneutralize it by dropwise addition of sodium hydroxide

solution (2 N) until a slightly green colour appears orwhite precipitate just forms. Add 10 ml of buffersolution (pH 3.5) and dilute to 50 ml mark. Shakethoroughly and measure absorbance at 470 nm againstreference test blank prepared in the same way butwithout the sample.

5.3.5 Calibration Curve

Draw a calibration curve by taking O, 1,2,3,4 and 5ml from 100 ppm standard titania solution preparedunder 5.2.9 in 50 ml volumetric flasks and followingthe procedure given in 5.3.4. Determine the titaniacontent of the test solution with reference to thecalibration curve.

5.4 Calculation

Titania, percent by mass =AX10-GX50X 100

Bwhere

A= Concentration of titania in ppm (fromgraph) in the aliquot of the mainsolution, and

B = weighting, of the sample represented bythe aliquot taken.

NOTE — Attemate procedure for determination of titania up to0.2 percent is ah given in Annex A.

ANNEX A

(Clause 5.4)

ALTERNATE PROCEDURE FOR

A-1 PROCEDURE

A-1.l Weigh accurately 1.000 g of the prepared sampleas per 3.2 into a platinum crucible. First heat gently andthen raise the temperatutv slowly to 1000”C. Finallyignite at 10OO°Cfor half an hour and cool.

A-1.2 To the residue A-1.l add slowly 5 ml of water, 2drops of sulphuric acid (1:1) and 20 ml of hydrofluoricacid. Cover the crucible with its lid and keep at roomtemperature for 10 min. Remove the lid and place it ona sand bath for evaporation of silica as SiFQand continueup to copious fuming. Cool the crucible and add further5 ml of hydrofluoric acid and~peat theproeess, Finallyignite the contents of the crucible containing the residueat 10OO°Cfor half an hour.

A-13 Fuse the residue after hydrofluorization ofsilica with 1:1 borex and sodium carbonate anddissolve in hydrochloric acid. Precipitate iron andalumina (R203) as hydroxide by adding drop by dropammonium hydroxide with constant stirring. Filter offthe precipitate. Transfer the funnel containing theprecipitate into a 100 ml volumetric flask, wash theRzos precipitate with distilled water and dissolve in

DETERMINATION OF TITANIA

25 ml hot 1:3 sulphuric acid. Finally rinse the filterpaper with hot water until the final volume reachesabout 85 ml, cool and add 5 ml of orthophosphoricacid (1 : 3) and 5 ml of 6 percent hydrogen peroxideand make up the volume to 100 ml with distilled waterShake the contents of the flask thoroughly andmeasure the optical density (absorbance) at 410 nm.

Draw a calibration curve by taking O, 1,2, 3,4,5 mlfrom 100 ppm standard titania stock solution preparedunder 5.2.9 in 100 ml volumetric flasks. Add 5 ml of1:3 O-phosphoric acid, 5 ml of 6 percent hydrogenperoxide and make up to the mark. Shake the contentsof the flask thoroughly and measure the optical density(absorbance) at 410 nm.

A-1.4 Calculation

Titania, percent by mass =AX IO+ XIOOXIOO

Bwhere

A= concentration of titaniagraph), and

B = weight of sample in g,

in ppm (from

2

. .

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This Indian Standard has been developed tlom Doc f No. MTD 29( 3865)

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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