1、BRITISH STANDARD BS 4140-4: 1986 ISO 804:1976 Methods of test for Aluminium oxide Part 4: Preparation of sample solution by alkaline fusion ISO title: Aluminium oxide primarily used for the production of aluminium Preparation of solution for analysis Method by alkaline fusion NOTEIt is recommended t
2、hat this Part be read in conjunction with the general information givenin BS4140-0 “General introduction” which is issued separately. UDC 546.623 31:620.1BS4140-4:1986 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authori
3、ty ofthe Board of BSI and comes intoeffect on 31January1986 BSI 11-1999 The Committees responsible for this British Standard are shown inPart0. The following BSI references relate to the work on this standard: Committee reference CIC/24 Draft for comment 84/55318 DC ISBN 0 580 14893 9 Amendments iss
4、ued since publication Amd. No. Date of issue CommentsBS4140-4:1986 BSI 11-1999 i Contents Page National foreword ii 1 Scope and field of application 1 2 References 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Procedure 1 Annex ISO publications relating to aluminium oxide primarily used for the produ
5、ction of aluminium 3 Publications referred to Inside back coverBS4140-4:1986 ii BSI 11-1999 National foreword This Part of BS4140 is identical with ISO804:1976 “Aluminium oxide primarily used for the production of aluminium Preparation of solution for analysis Method by alkaline fusion”, published b
6、y the International Organization for Standardization (ISO). The method supersedes clause4 of BS4140:1967. Parts1 to7 of this standard collectively supersede BS4140:1967, which is withdrawn. Terminology and conventions. The text of the International Standard has been approved as suitable for publicat
7、ion as a British Standard without deviation. Some terminology and certain conventions 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 o
8、n the baseline as the decimal marker. In British Standards it is current practice to use the symbol “L” for litre (and its submultiples) rather than “l”. Wherever the words “International Standard” appear, referring to this standard, they should be read as “British Standard”. NOTEThe other Internati
9、onal Standards listed in the Annex are for information only. Their correspondence with British Standards is summarized in BS4140-0 “General introduction”. Additional information. In6.2 and6.4.1 it is preferable in the UK to use the fusion mixture containing boric acid for solutions subsequently to b
10、e used for the determination of silica (see BS4140-5) as the results are found to be more reliable. In the UK it is preferable to use polypropylene beakers in place of the polyethylene type referred to in6.3. NOTETextual error. In line1 of clause3 “protion” should read “portion”. This standard presc
11、ribes methods of test only, and should not be used or quoted as a specification defining limits of purity. Reference to this Part should indicate that the method of preparation complies with BS4140-4:1986. A British Standard does not purport to include all the necessary provisions of a contract. Use
12、rs of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-references International Standard Corresponding British Standard BS 4140 Methods of test for aluminium oxide ISO 802:1976 Part 1:
13、1986 Preparation and storage of test samples (Identical) ISO 2927:1973 Part 20:1980 Sampling (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages1 to 4, an inside back cover and a back cover. This standard has been updated (see copyright da
14、te) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS4140-4:1986 BSI 11-1999 1 1 Scope and field of application This International Standard specifies a method for the dissolution, by alkaline fusion, of aluminium oxide primarily used
15、 for the production of aluminium, in order to obtain a principal solution (solution P) for certain, determinations. 2 References ISO 802, Aluminium oxide primarily used for the production of aluminium Preparation and storage of test samples. ISO 2927, Aluminium oxide primarily used for the productio
16、n of aluminium Sampling. 3 Principle Alkaline fusion of a test protion either with a mixture of sodium carbonate and boric acid, or with a mixture of sodium carbonate and sodium tetraborate. Dissolution of the melt in an excess of nitric acid so that the final pH of the solution is approximately1, a
17、fter dilution to500ml, or approximately0,4, after dilution to250ml. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Sodium carbonate, anhydrous. 4.2 Boric acid (H 3 BO 3 ). 4.3 Sodium tetraborate, anhydrous
18、(Na 2 B 4 O 7 ). 4.4 Aluminium oxide, extra pure. 4.5 Nitric acid, approximately8N solution. Dilute540ml of nitric acid, approximately1,40g/ml, about68% (m/m) solution, with water and dilute to1000ml. 5 Apparatus Ordinary laboratory apparatus and 5.1 Platinum dish, flat bottomed, of diameter approxi
19、mately70mm and depth approximately35mm, fitted with a platinum lid. 5.2 Electric furnace, capable of being controlled at500 50 C. 5.3 Electric furnace, capable of being controlled between1000 and1025 C. 6 Procedure 6.1 Test portion Weigh, to the nearest0,001g, exactly5g of the test sample, dried at3
20、00 C (see3.3 of ISO802). 6.2 Fusion of test portion Weigh into the platinum dish (5.1) either12g of the sodium carbonate (4.1) and4g of the boric acid (4.2), or10,3g of the sodium carbonate (4.1) and3,3g of the sodium tetraborate (4.3). Mix thoroughly. Add the test portion(6.1) and carefully mix the
21、 whole, preferably with a platinum spatula. Cover the dish with its lid and place it in the electric furnace(5.2), controlled at500 50 C, taking care to isolate it from the floor of the furnace by means of a support that cannot cause introduction of impurities. Maintain at500 50 C until the reaction
22、 subsides. Then transfer the dish to the electric furnace(5.3), controlled between1000 and1025 C, taking care to isolate it, as before, from the floor of the furnace. Keep the dish in the furnace for30min. Ensure that a temperature of between1000 and1025 C is maintained for a minimum of20min. 6.3 Pr
23、eparation of the principal solution Remove the dish from the furnace and allow to cool in air. Add boiling water to the dish, heating gently until dissolution of the melt. After slight cooling, transfer the contents of the dish to a polyethylene beaker of suitable capacity containing50ml of the nitr
24、ic acid solution(4.5). NOTEIn the cases where dissolution of the melt in nitric acid prior to obtaining the principal solution is unsuitable for the determination of certain elements, the dissolution should be made in an alternative appropriate acid which should be stated in the method of test of th
25、e element. Dissolve any residue still adhering to the walls of the dish (consisting essentially of iron(III) oxide, calcium oxide and titanium oxide) with20ml of the nitric acid solution and transfer the solution obtained to the polyethylene beaker. Carefully wash both the dish and the lid with hot
26、water and transfer the washings to the polyethylene beaker. By careful washing, transfer the contents of the polyethylene beaker to a glass beaker. Heat for a few minutes at a temperature close to the boiling point until any remaining aluminium hydroxide is completely dissolved. Allow to cool slight
27、ly. When the solution is lukewarm, transfer quantitatively to a250or500ml one-mark volumetric flask, depending on the content of the elements to be determined. Allow to cool, dilute to the mark and mix.BS4140-4:1986 2 BSI 11-1999 NOTEWhen the solution obtained is opalescent, prepare a new solution,
28、taking care to grind the aluminium oxide so as to obtain a particle size smaller than approximately50 m. 6.4 Preparation of the blank test solution Prepare a blank test solution as indicated in6.4.1 or6.4.2, proceeding, in accordance with the instructions given in the International Standard relating
29、 to the determination to be carried out, in the presence or absence of extra-pure aluminium oxide(4.4). 6.4.1 Blank test solution containing extra-pure aluminium oxide Follow the same procedure as used for the test portion (see6.2 and6.3), using exactly5g of extra-pure aluminium oxide(4.4), weighed
30、to the nearest0,001g. 6.4.2 Blank test solution free from extra-pure aluminium oxide Weigh into the same platinum dish(5.1) either12g of the sodium carbonate(4.1) and4g of the boric acid(4.2), or10,3g of the sodium carbonate(4.1) and3,3g of the sodium tetraborate(4.3). Mix carefully. Cover the dish
31、with its lid and place in the electric furnace(5.2), controlled at500 50 C, taking care to isolate the dish from the floor of the furnace. Maintain at500 50 C until the reaction subsides. Then transfer the dish to the electric furnace(5.3), controlled at a temperature of between1000 and1025 C, takin
32、g care to isolate it, as before, from the floor of the furnace. Keep the dish in the furnace for a maximum of5min. Remove the dish from the furnace and allow to cool in air. Add boiling water to the dish, heating gently until dissolution of the melt. After slight cooling, transfer the contents of th
33、e dish to a polyethylene beaker of suitable capacity containing30ml of the nitric acid solution(4.5). Wash carefully both the dish and the lid with hot water and transfer the washings to the polyethylene beaker. Transfer carefully, by washing, the contents of the polyethylene beaker to a glass beake
34、r. Heat for a few minutes at a temperature close to the boiling point. Allow to cool slightly and transfer quantitatively to either a250or a500ml one-mark volumetric flask, according to requirements. Place36,7ml of the nitric acid solution(4.5) in the platinum dish and evaporate almost to dryness. A
35、dd a small amount of hot water to the dish. Add3,3ml of the nitric acid solution. Heat if necessary, and after cooling, transfer the solution quantitatively to the one-mark volumetric flask to which the contents of the glass beaker have previously been transferred. Allow to cool, dilute to the mark
36、and mix. NOTEThis technique of partial evaporation is used to ensure the same pH values, both in the blank test and in the principal solution, in the presence of the same quantities of impurities introduced.BS4140-4:1986 BSI 11-1999 3 Annex ISO publications relating to aluminium oxide primarily used
37、 for the production of aluminium ISO 802, Preparation and storage of test samples. ISO 803, Determination of loss of mass at300 C (conventional moisture). ISO 804, Preparation of solution for analysis Method by alkaline fusion. ISO 805, Determination of iron content 1,10-Phenanthroline photometric m
38、ethod. ISO 806, Determination of loss of mass at1000 and1200 C. ISO 900, Determination of titanium content Diantipyrylmethane photometric method. ISO 901, Determination of absolute density Pyknometer method. ISO 902, Measurement of the angle of repose. ISO 903, Determination of untamped density. ISO
39、 1232, Determination of silica content Reduced molybdosilicate spectrophotometric method. ISO 1617, Determination of sodium content Flame emission spectrophotometric method. ISO 1618, Determination of vanadium content N-Benzoyl-N-phenylhydroxylamine photometric method. ISO 2069, Determination of cal
40、cium content Flame atomic absorption method. ISO/R 2070, Determination of calcium content Spectrophotometric method using naphthalhydroxamic acid. ISO 2071, Determination of zinc content Flame atomic absorption method. ISO/R 2072, Determination of zinc content PAN photometric method. ISO 2073, Prepa
41、ration of solution for analysis Method by hydrochloric acid attack under pressure. ISO 2828, Determination of fluorine content Alizarin complexone and lanthanum chloride spectrophotometric method. ISO 2829, Determination of phosphorus content Reduced phosphomolybdate spectrophotometric method. ISO 2
42、865, Determination of boron content Curcumin spectrophotometric method. ISO 2926, Particle size analysis Sieving method. ISO 2927, Sampling. ISO 2961, Determination of an adsorption index. ISO 3390, Determination of manganese content Flame atomic absorption method.4 blankBS4140-4:1986 BSI 11-1999 Pu
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