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YS/T 575.6-2007 English PDF (YST575.6-2007)

YS/T 575.6-2007 English PDF (YST575.6-2007)

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YS/T 575.6-2007: Methods for chemical analysis of bauxite. Part 6: Determination of titanium dioxide content. Diantipyrylmethane photometric method

This Part specifies the determination of titanium dioxide content in bauxite. This Part is applicable to the determination of titanium dioxide content in bauxite; the determination range is 0.50%~8.00%.
YS/T 575.6-2007
NON-FERROUS METAL INDUSTRY STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
ICS 71.100.10
Q 52
Replacing YS/T 575.6-2006
Methods for Chemical Analysis of Bauxite -
Part 6: Determination of Titanium Dioxide Content -
Diantipyrylmethane Photometric Method
ISSUED ON: NOVEMBER 14, 2007
IMPLEMENTED ON: MAY 01, 2008
Issued by: National Development and Reform Commission
Table of Contents
Foreword ... 3
1 Scope ... 6
2 Method Principle ... 6
3 Reagents ... 7
4 Apparatus ... 8
5 Specimen ... 8
6 Analysis Procedures ... 8
7 Calculation of Analysis Results ... 11
8 Precision ... 11
9 Quality Assurance and Control ... 12
Foreword
YS/T 575-2007 Methods for Chemical Analysis of Bauxite is a modification to YS/T 575-2006 (formerly GB/T 3257-1999). It has 24 parts in total:
--- Part 1: Determination of aluminum oxide content - EDTA titrimetric method; --- Part 2: Determination of silicon dioxide content - Gravimetric-molybdenum blue photometric method;
--- Part 3: Determination of silicon dioxide content - Molybdenum blue photometric method;
--- Part 4: Determination of iron oxide content - Potassium titrimetric method; --- Part 5: Determination of iron oxide content - Orthophenanthroline photometric method;
--- Part 6: Determination of titanium dioxide content - Diantipyrylmethane photometric method;
--- Part 7: Determination of calcium oxide content - Flame atomic absorption spectrophotometric method;
--- Part 8: Determination of magnesium oxide content - Flame atomic absorption spectrophotometric method;
--- Part 9: Determination of potassium oxide, sodium oxide content - Flame atomic absorption spectrophotometric method;
--- Part 10: Determination of manganese oxide content - Flame atomic absorption spectrophotometric method;
--- Part 11: Determination of chromium oxide content - Flame atomic absorption spectrophotometric method;
--- Part 12: Determination of vanadium pentoxide content - N-benzoyl-N- phenylhydroxylamine photometric method;
--- Part 13: Determination of zinc content - Flame atomic absorption
spectrophotometric method;
--- Part 14: Determination the total content of rare earth oxide Tribromo-arsenazo photometric method;
--- Part 15: Determination of gallium oxide content - Rhodamine B-extraction Methods for Chemical Analysis of Bauxite -
Part 6: Determination of Titanium Dioxide Content -
Diantipyrylmethane Photometric Method
1 Scope
This Part specifies the determination of titanium dioxide content in bauxite. This Part is applicable to the determination of titanium dioxide content in bauxite; the determination range is 0.50%~8.00%.
2 Method Principle
a) Treat with a mixed acid among hydrochloric acid, nitric acid and sulfuric acid. This method is suitable for gibbsite or boehmite. It is required that after the dissolution of the sample, the residue after volatile of silicon dioxide is less than 1% of the amount of the specimen.
b) Sintered with sodium peroxide, melted briefly, and dissolved with sulfuric acid. This method is suitable for diaspore. It is required that after the dissolution of the sample, the residue after volatile of silicon dioxide is greater than 1% of the amount of the specimen.
c) Melt with sodium carbonate and sodium tetraborate, and extract with sulfuric acid. This method is applicable to all types of ore.
Silicon dioxide dehydrates, dissolves salts, filters, and burns the residue. It is evaporated with hydrofluoric acid and sulfuric acid to disperse the silicon dioxide; melted with sodium carbonate and sodium tetraborate; dissolved with sulfuric acid, and incorporated into the main solution. Reduce Fe3+ with ascorbic acid; develop color by diantipyrylmethane; then measure the absorbance of the solution at about 390nm.
3 Reagents
3.1 Sodium peroxide.
NOTE: Sodium peroxide should prevent moisture absorption and it cannot be used once it is agglomerated.
3.2 Sodium carbonate and sodium tetraborate flux: use 3 parts of anhydrous sodium carbonate (Na2CO3) and 1 part of anhydrous sodium tetraborate (Na2B4O7) to mix thoroughly.
3.3 Hydrofluoric acid.
3.4 Sulfuric acid (1+1).
3.5 Sulfuric acid (1+9).
3.6 Hydrochloric acid (1+1).
3.7 Mixed acid: pipette 225 mL of water into a 1000 mL beaker; carefully add 175 mL of sulfuric acid, and mix well. Cool to room temperature; add 150mL of hydrochloric acid and 50mL of nitric acid; and mix well (prepared when it is used).
3.8 Ascorbic acid solution: 100g/L (prepared on the day when this solution is used). 3.9 Diantipyrylmethane solution (15g/L): dissolve 15g of diantipyrylmethane (C23H24N4O2) into 1L of sulfuric acid (1+49); prepare on the day of use. 3.10 Ammonium ferric sulfate solution: Dissolve 6 g of ferric ammonium sulfate [Fe2 (NH4)2 (SO4) 4 ?€? 24H2O] in 1L of water containing 10mL sulfuric acid solution (3.5). 3.11 Titanium standard storage solution: 1mL solution contains 1mg titanium dioxide. In use, any of the following methods can be used:
3.11.1 Take 0.300g of high-purity titanium (99.9%), accurate to 0.001g. Put in a conical flask; add 50mL of water and 50mL sulfuric acid solution (3.4); dissolved by heating. Add nitric acid (1+4) drop by drop to oxidize the solution until the purple color disappears. Cool off, transfer to a 500mL volumetric flask; dilute to the scale and mix evenly.
3.11.2 Take 0.500g of high-purity titanium dioxide (99.9%), accurate to 0.001g (burned in a platinum crucible at 980??C for 30min before cooling in a dryer). Put it into a 250mL conical flask; add 8g of ammonium sulfate and 25mL of sulfuric acid (3.4). Insert a short-neck glass funnel on the bottle mouth; carefully heating continuously to a slight boiling; continue heating to complete dissolution; and cool to room temperature. Add 200mL of water in one portion and cool. Quantitatively transfer 100mL of sulfuric acid If the specimen is decomposed by acid; it shall be performed according to analytical procedure 6.5.1.1. If the specimen is decomposed by alkaline sintering, it shall be performed by analytical procedure 6.5.1.2. If the specimen is decomposed by melting, it shall be performed by the analysis steps of 6.5.1.3.
6.4.1.1 Acid decomposition
Put the specimen (6.1) in a 400mL beaker; moisten it with water. Add 60mL of mixed acid (3.7); cover with a watch glass and decompose by heating at 80??C (when the amount of Fe2O3 in the specimen is greater than 15%, heating time shall be extended a bit). After the brown smoke is gone, wash the watch glass and the wall of the beaker. Remove the watch glass; heat and evaporate until the thick sulfuric acid smoke appears. Cover the watch glass again; and heat it on hot plate to keep the temperature of the solution at 210??C??10??C. Heat the strong reflow for 60min. In another beaker containing sulfuric acid, measure the temperature by inserting a thermometer and immersing it at 10 mm in sulfuric acid.
6.4.1.2 Alkaline sintering decomposition
Put the specimen (6.1) in a dry zirconium crucible; add 10 g of sodium peroxide (3.1); mix thoroughly by a dry metal spoon; and then put it in a muffle furnace for sintering at 490??C for 45 minutes. Remove the crucible and material from the furnace; heat the molten sintered material (about 30s) on a torch. In the molten state, heat the crucible for 2min as rotate it; cool it to room temperature. Place the crucible side in a 400mL beaker and cover the watch glass; carefully add 140mL of sulfuric acid solution (3.5) to the back of the crucible; and then add 20mL of sulfuric acid solution (3.4); heat and leach the molten material in the crucible. When the specimen in crucible is completely leached, take out the crucible and wash the watch glass and beaker wall; remove the watch glass; heat and evaporate the solution to emit thick sulfuric acid smoke; cover the watch glass; and heat the solution on a hot plate to keep the temperature of the solution at 210??C??10??C, strongly reflux for 60min.
6.4.1.3 Melting decomposition
Place the specimen (6.1) in a dry platinum-yellow alloy crucible; add 2g of sodium carbonate and sodium tetraborate mixed flux (3.2); mix thoroughly by a dry metal spoon; then cover the platinum lid. Put it in a muffle furnace, keep it at 480??C~500??C for 5min; then move it into another muffle furnace; maintain it at 900??C for 10min; take out the crucible; put it in a 400mL beaker after cooling; add 40mL water and 35mL sulfuric acid solution(3.4). Cover the watch glass, heat and leach the specimen in the crucible. After the specimen in the crucible is completely leached, take out the crucible and wash the watch glass and the beaker wall. Heat and evaporate solution to emit thick sulfuric acid smoke; cover the watch glass; heat on the hot plate and keep the solution temperature at 210??C??10??C, strongly reflux for 60min.

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