standard testing procedure titanium dioxide

Storage Requirements:
Store protected from light and moisture.

Sampling:
Sample from each container / bag, if the consignment is of 03 or less than three containers / bags. If the number of containers / bags is more than 03and are up to 100, sample at randomly using the formula root (n) +1 where n is the number of containers/bags in the consignment. For the consignment of more than 100 containers/bags, sample additional containers/bags for every 100 containers/bags and thereafter. Collect a minimum of 5g from each of the randomly selected containers/bags in to individually no toxic, self sealing transparent polyethylene bearing ‘Sample For Analysis label kept in another transparent self sealing polythene bag. After completion of sampling return rest sample on the same container. Collect control sample in Pet bottle/Glass bottle.

Quantity of Composite Sample:

50 g

Quantity of Control Sample:

2 X 50 g

Description: A white or almost white infusible powder.

Solubility: Practically insoluble in water and in dilute mineral acids, slowly in hot sulphuric acid.

Identification:

A. The colour is discharged on cooling.
B. An orange-red colour is produced.
C A violet-blue colour is produced.

Appearance of solution: Solution A is not more opalescent than opalescence standard OS2, and colourless.

Acidity or alkalinity: Not more than 1.0 ml of ether 0.01M hydrochloric acid or 0.01M sodium hydroxide is required to change the colour of the solution.

Water soluble substances: NMT 0.5% w/w.

Arsenic: NMT 5 ppm.

Barium: To 10ml of this solution add 1ml of 1M sulphuric acid. After 30 minutes any opalescence is not more intense than that of a mixture of 10ml of the test solution and 1ml of distilled water.

Heavy metals: NMT 20 ppm.

Iron: NMT 200 ppm.

Assay: 98.0%w/w to 100.5%w/w of TiO2.

Description: A white or almost white infusible powder; odourless.

Solubility: Practically insoluble in water and in dilute mineral acids, slowly in hot sulphuric acid.

Identification:

A. When strongly heated it becomes pale yellow; the colour is discharged on cooling.
B. To 0.5g, add 5g of anhydrous sodium sulphate and 10ml of water and mix. Add 10ml of sulphuric acid and boil gently until clear; cool, add slowly 30mml of a 25 per cent v/v solution of sulphuric acid and dilute with water to 100ml (solution A). To 5 ml of solution A add 0.1ml of strong hydrogen
Peroxide solution; an orange-red colour is produced.
C To 5ml of solution A add 0.5g of zinc, in granules; after 45 minutes a violet-blue colour is produced.

Appearance of solution: Solution A is not more opalescent than opalescence standard OS2, and colourless.

Acidity or alkalinity: Shake 5.0 g with 50ml of carbon dioxide free water for 5 minute, and centrifuge until a clear solution is obtained. To 10ml of the solution add 0.1ml of bromothymol blue solution. Not more than 1.0 ml of ether 0.01M hydrochloric acid or 0.01M sodium hydroxide is required to change the colour of the solution.

Water soluble substances: Not more than 0.5 per cent, determined by the following method. Boil 10.0g for 5 minutes with 150ml of water containing 0.5g of ammonium sulphate. Cool, dilute to 200ml with water and filter until a clear solution is obtained. Evaporate 100ml of the filtrate to dryness ignite and weigh.

Arsenic: To 0.2g in a 100ml Kjeldhal flask, add 2g of anhydrous sodium sulphate, 7ml of sulphuric acid and 5 ml of nitric acid. Heat gently until a clear solution is obtained, cool, add 10ml of water, cool again and add 5g of hydrazine reducing mixture and 10ml of hydrochloric acid. Immediately attach an air condenser and distil into 15 ml of cooled water until a total volume of 30ml is obtained. Rinsed the condenser with 5ml of water and dilute the combined distillate and rinsing to 40ml with water. 20ml of the resulting of solution complies with the limit test for arsenic. Use a mixture of 0.5ml of arsenic standard solution (I ppm As) and 24.5ml of water to prepare the standard (5 ppm).

Barium: Shake 20.0 g with 30ml of hydrochloric acid ,add 100ml of distill water and boil. Filter while hot through a hardened filter paper until a clear filtrate is obtained. Wash the filter with 60 ml of distilled water and dilute the combined filter with 60ml of distill water and dilute the combined filtrate and washings to 200ml with distilled water. To 10ml of this solution add 1ml of 1M sulphuric acid. After 30 minutes any opalescence is not more intense than that of a mixture of 10ml of the test solution and 1ml of distilled water.

Heavy metals: Dilute 10ml of this solution prepared in the test for Barium to 20ml with water. 12ml of this solution complies with the limit test for heavy metals, Method D (20 ppm).

Iron: To 8ml of solution A, add 4 ml of water, mix and add 0.05ml of bromine water, allow standing for 5 minutes, removing the excess of bromine with a current of air and adding 3ml of potassium thiocyanate solution. Any colour in the solution is not more intense than that in a standard prepared at the same time and in the same manner using a mixture of 4ml of iron standard solution (2ppm Fe) and 8ml of a 20 per cent w/v solution f sulphuric acid (200 ppm).

Assay: Weigh accurately about 0.5g ,transfer to a 300ml Kjeldhal flask, add 5g of anhydrous sodium sulphate and 10ml of water, mix and add slowly 40 ml of cooled sulphuric acid (25 per cent), cool again and dilute with water to 100.0 ml (solution B.) To 300g of zinc, in granules, add 300ml of a 2 per cent w/v solution of mercuric nitrate and 2 ml of nitric acid shake for 10 minutes and wash with water. Pack the zinc amalgam into a glass tube (400 mm x 20 mm) fitted with a tap and a filter plate. Pass through the column, at a rate of about 100ml of water, ensuring that the amalgam is covered is covered with liquid throughout. Pass slowly through the column, at a rate of about 3 ml per minute, 200ml of 0.5m sulphuric acid followed by 100ml of water. Collect the combined eluates in a 500ml conical flask containing 50m l of a 15 per cent w/v solution of ferric ammonium sulphate in sulphuric acid (25 per cent) and titrate immediately with 0.1m ceric ammonium nitrate using ferroin solution as indicator until a greenish colour is obtained (n1 ml). Pass slowly through the column 100ml of 0.5M sulphuric acid followed by 20.0 ml of solution B, wash with 100ml of 0.5M sulphuric acid followed by 100ml of water. Collect the combined eluates in a 500-ml conical flask containing 50ml of a 15 per cent w/v solution of ferric ammonium sulphate in sulphuric acid (25 per cent, rinse the lower end of the column with water and titrate Immediately with 0.1 m ceric ammonium nitrate using ferroin solution as indicator until a greenish colour is obtained (n2 ml). Calculate the percentage content of TiO2 from the expression 3.99 (n2-n1)/w

Where w is the weight, in g, of the substance under examination used in the preparation of solution A.
per gram.

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