BS 6870-2 7-1987 Analysis of aluminium ores Chemical methods Method for determination of titanium content spectrophotometric method《铝矿石分析 化学方法 钛含量测定方法 分光光度分析法》.pdf
《BS 6870-2 7-1987 Analysis of aluminium ores Chemical methods Method for determination of titanium content spectrophotometric method《铝矿石分析 化学方法 钛含量测定方法 分光光度分析法》.pdf》由会员分享,可在线阅读,更多相关《BS 6870-2 7-1987 Analysis of aluminium ores Chemical methods Method for determination of titanium content spectrophotometric method《铝矿石分析 化学方法 钛含量测定方法 分光光度分析法》.pdf(12页珍藏版)》请在麦多课文档分享上搜索。
1、BRITISH STANDARD BS 6870-2.7: 1987 ISO 6995:1985 Analysis of aluminium ores Part 2: Chemical methods Section 2.7 Method for determination of titanium content: spectrophotometric method ISO title: Aluminium ores Determination of titanium content 4,4-Diantipyrylmethane spectrophotometric method UDC 55
2、3.492:543BS6870-2.7:1987 This British Standard, having been prepared under the directionof the Non-ferrous Metals Standards Committee, waspublished under the authorityof the Board of BSI andcomes into effect on 28August1987 BSI 01-2000 The following BSI references relate to the work on this standard
3、: Committee reference NFM/31 Draft for comment 83/76596 DC ISBN 0 580 16060 2 National foreword This Section of BS 6870 has been prepared under the direction of the Non-ferrous Metals Standards Committee. It is identical with ISO6995:1985 “Aluminium ores Determination of titanium content 4,4-Diantip
4、yrylmethane spectrophotometric method”, published by the International Organization for Standardization (ISO). Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation. Some terminology and certain conve
5、ntions are not identical with those used in British Standards; attention is drawn especially to the following. The comma has been used as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. Wherever the words “International Standar
6、d” appear, referring to this standard, they should be read as “Section of BS6870”. Additional information. When adopting the text of the International Standard, it was noticed that in4.6 and4.7 hydrochloric acid with a density of1.17g/ml is specified, whereas in the UK hydrochloric acid with a densi
7、ty of1.18g/ml is normally used. This difference, which will not affect the determination, has been brought to the attention of ISO in a proposal to amend the International Standard by specifying a wider range for the density of the hydrochloric acid required. A British Standard does not purport to i
8、nclude all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pa
9、gesi andii, pages1 to6, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Cross-reference International Standard Corresponding British Standard
10、ISO 5725:1986 BS 5497 Precision of test methods Part 1:1987 Guide for the repeatability and reproducibility for a standard test method by inter-laboratory tests (Identical) Amendments issued since publication Amd. No. Date of issue CommentsBS6870-2.7:1987 BSI 01-2000 i Contents Page National forewor
11、d Inside front cover 1 Scope and field of application 1 2 Reference 1 3 Principle 1 4 Reagents 1 5 Apparatus 2 6 Sampling and preparation of samples 2 7 Procedure 2 8 Expression of results 4 9 Test report 5 Table 1 Intermediate dilutions 4 Table 2 Mass of TiO 2in titanium solutions 4 Table 3 Precisi
12、on data for titanium determinations 4 Publication referred to Inside back coverii blankBS6870-2.7:1987 BSI 01-2000 1 1 Scope and field of application This International Standard specifies a 4,4-diantipyrylmethane spectrophotometric method for the determination of the titanium content of aluminium or
13、es. The method is applicable to ores containing between0,5 and 8% (m/m) of titanium dioxide. 2 Reference ISO 5725, Precision of test methods Determination of repeatability and reproducibility by inter-laboratory tests. 3 Principle Decomposition of the test portion by: a) Treatment with a mixture of
14、hydrochloric acid, nitric acid and sulfuric acid. NOTEThis method is recommended for ores containing gibbsite and/or boehmite and when the residue from the dissolution of the test portion after silica volatilization is less than 1% of the mass of the test portion; or b) Sintering with sodium peroxid
15、e followed by a brief fusion. Dissolution of the melt with sulfuric acid. NOTEThis method is recommended for ores containing diaspore and when the residue after silica volatilization for acid decomposition is greater than 1% of the mass of the test portion; or c) Fusion with sodium tetraborate/sodiu
16、m carbonate flux followed by treatment with sulfuric acid. NOTEThis method is suitable for all types of ores. Dehydration of silica, dissolution of salts, and filtration and ignition of the residue. Removal of the silica by evaporation with hydrofluoric and sulfuric acids. Fusion of the residue with
17、 sodium carbonate/sodium tetraborate flux, dissolution of the melt with sulfuric acid and addition to the main solution. Reduction of the iron with ascorbic acid; colour development with 4,4-diantipyrylmethane and measurement of the absorbance at about390nm. 4 Reagents During the analysis, use only
18、reagents of analytical reagent grade and only distilled water or water of equivalent purity. 4.1 Sodium peroxide NOTESodium peroxide should be protected against humidity and should not be used once it has begun to agglomerate. 4.2 Sodium carbonate/sodium tetraborate flux Mix 3 parts by mass of anhyd
19、rous sodium carbonate and1 part by mass of anhydrous sodium tetraborate. 4.3 Hydrofluoric acid, 40% (m/m), 201,13g/ml. 4.4 Sulfuric acid, 201,84g/ml, diluted 1 +1. 4.5 Sulfuric acid, 201,84g/ml, diluted 1 + 9. 4.6 Hydrochloric acid, 201,17g/ml, diluted 1 + 1. 4.7 Acid mixture Measure into a one-litr
20、e beaker 225ml of water and add cautiously, with mixing, 175ml of sulfuric acid ( 201,84g/ml). Cool to room temperature and add150ml of hydrochloric acid ( 201,17g/ml) and50ml of nitric acid ( 201,42g/ml). Prepare this solution fresh for each series of determinations and discard any unused solution.
21、 4.8 Ascorbic acid, 100g/l solution. Prepare this solution as required. 4.9 4,4-Diantipyrylmethane, 15g/l solution. Dissolve 15 g of 4,4-diantipyrylmethane (C 23 H 24 N 4 O 2 ) in 1l of sulfuric acid solution ( 20 1,84g/ml, diluted 1 + 49). Prepare fresh as required. 4.10 Ammonium iron(III) sulfate
22、solution. Dissolve 6g of ammonium iron(III) sulfate 24 water Fe 2 (NH 4 ) 2 (SO 4 ) 4 .24H 2 O in1litre of water containing10ml of the sulfuric acid solution (4.5). 4.11 Titanium, standard solution, corresponding to1,0g of TiO 2per litre. One of the following methods may be used: a) Weigh, to the ne
23、arest 0,001g, 0,300g of high purity (99,9%) titanium metal into a conical flask, add50ml of water and50ml of the sulfuric acid solution (4.4) and heat to dissolve the metal. Oxidize the solution until the purple colour disappears by adding, drop by drop, nitric acid solution ( 201,42g/ml, diluted 1
24、+ 4). Cool and transfer quantitatively to a500ml one-mark volumetric flask. Dilute to the mark and mix thoroughly.BS6870-2.7:1987 2 BSI 01-2000 b) Weigh, to the nearest 0,001g, 0,500g of high purity (99,9%) titanium dioxide (previously ignited in a platinum crucible at950 to1000 C for 30min and drie
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