1、BRITISH STANDARD BS4140-13: 1986 ISO2073:1976 Methods of test for Aluminium oxide Part 13:Preparation of sample solution by treatment with hydrochloric acid under pressure ISO title: Aluminium oxide primarily used for the production of aluminiumPreparation of solution for analysisMethod by hydrochlo
2、ric acid attack under pressure NOTEIt is recommended that this Part be read in conjunction with the general information given in BS4140-0 “General introduction” which is issued separately. UDC 546.62331:620.1BS4140-13:1986 This British Standard, having been prepared under the directionof the Chemica
3、ls Standards Committee, was published under the authority ofthe Board of BSI and comesintoeffect on 31January1986 BSI 10-1999 The committees responsible forthis British Standard are shown inPart 0 The following BSI references relate to the work on this standard: Committee reference CIC/24 Draft for
4、comment 85/52371 DC ISBN 0 580 14929 3 Amendments issued since publication Amd. No. Date of issue CommentsBS4140-13:1986 BSI 10-1999 i Contents Page National foreword ii 1 Scope and field of application 1 2 References 1 3 Principle 1 4 Reagent 1 5 Apparatus 1 6 Procedure 1 AnnexISO publications rela
5、ting to aluminium oxide primarily used for the production of aluminium 3 Publications referred to Inside back coverBS4140-13:1986 ii BSI 10-1999 National foreword This Part of BS4140 is identical with ISO2073:1976 “Aluminium oxide primarily used for the production of aluminiumPreparation of solution
6、 for analysis Method by hydrochloric acid attack under pressure” published by the International Organization for Standardization (ISO). This method supersedes clause13 of Addendum No.2(1974) to BS4140:1967. Parts 11 to 16 1)of this standard collectively supersede Addendum No. 2 (1974) to BS4140:1967
7、, which is withdrawn. 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 conventions are not identical with those used in British Standards; attention is drawn especia
8、lly 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. In British Standards it is current practice to use the symbol “L” for litre (anditssubmultiples) rather than “l”. Wherever the wo
9、rds “International Standard” appear, referring to this standard, they should be read as “British Standard”. NOTEThe other International Standards listed in the Annex are for information only. Their correspondence with British Standards is summarized in BS 4140-0 “General introduction”. This standard
10、 prescribes 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 test used complies with BS4140-13:1986. A British Standard does not purport to include all the necessary provisions of a contract
11、. 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, pagesiandii, pages1to4, an inside back cover and a
12、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. 1) Parts 14 and 15 are in preparation. Cross-references International Standard Corresponding British Standard BS4140 Meth
13、ods of test for aluminium oxide ISO 802:1976 Part 1:1986 Preparation and storage of test samples (Identical) ISO 2927:1973 Part 20:1980 Sampling (Identical)BS4140-13:1986 BSI 10-1999 1 1 Scope and field of application This International Standard specifies a method for the dissolution of aluminium ox
14、ide primarily used for the production of aluminium, by means of attack by hydrochloric acid under pressure in a sealed borosilicate glass tube, in order to obtain a test solution for certain determinations. The method is not applicable to the preparation of test solutions for the determination of si
15、licon, sodium or boron, owing to the possibility of extraction of these elements from the glass. NOTEHydrochloric acid may be replaced by another appropriate acid. In this case, the acid should be stated in the method of test of the impurity. 2 References ISO802, Aluminium oxide primarily used for t
16、he production of aluminiumPreparation and storage of test samples. ISO2927, Aluminium oxide primarily used for the production of aluminiumSampling. 3 Principle Attack of a test portion by hydrochloric acid under pressure in a sealed borosilicate glass tube heated in an electric oven controlled at250
17、 or275 C. 4 Reagent During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Hydrochloric acid, approximately1,19g/ml, about38%(m/m) solution. 5 Apparatus Ordinary laboratory apparatus and 5.1 Borosilicate glass tubing, having
18、thick walls (ofthickness about2,4mm) and an external diameter of about16mm. 5.2 Borosilicate glass rod, of diameter about 4mm. 5.3 Glass-blowing equipment, comprising: 5.3.1 Gas burner, fed by a mixture of combustible gas and oxygen, with suitable heads. 5.3.2 Normal combustible gas and oxygen. 5.3.
19、3 Glass cutter 5.3.4 Protective goggles, tinted. 5.3.5 Blower, with rubber tube connected to gas burner. 5.4 Pencil, resistant to high temperatures, for marking glass. 5.5 Tube holder, to keep tubes vertical, or alternatively 5.5.1 Tube holder, to keep tubes at an inclination of about 30 . 5.6 Funne
20、l, of diameter approximately 40mm, with short stem. 5.7 Electric oven, capable of being controlled at250 5 C and275 5 C. 5.8 Protecting steel tubes, of internal diameter about25mm and length about260 or310mm, according to the length of the glass tube(5.1) used, threaded and firmly fitted with screw
21、caps at each end. A number of holes of diameter about6 to8mm shall be made at random intervals along the length of the protective tube. This tube is necessary in order to avoid damage to the interior of the oven and to adjacent tubes in case a reaction tube should burst. The holes are necessary to a
22、llow the escape of gases in the event of breakage of a reaction tube and to avoid a rise of pressure inside the protective tube. 6 Procedure 6.1 Test portion According to the determination to be carried out, weigh, to the nearest 0,001g, 1 or2g of the test sample, dried at 300 C (see3.3 of ISO802).
23、6.2 Attack of the test portion 6.2.1 Preparation of the tubes Cut the tubing (5.1) to a length of about250mm for a1g test portion, or to a length of about300mm for a2g test portion. Clean the tubes in a cleaning solution, rinse thoroughly in distilled water, dry at approximately125 C and allow to co
24、ol. Close one end of each tube in the flame so as to give it a hemispherical shape. Avoid an increase or reduction in the thickness of the tube and anneal to eliminate stresses. For this annealing, use a reducing flame (a yellow flame, obtained by reducing the flow of oxygen, without adjusting the f
25、low of gas) until a thick coating of carbon black is deposited on the tube, and allow it to cool. A series of tubes can also be annealed by placing them in a furnace at approximately 550 C and allowing the temperature of the furnace to drop slowly to approximately 300 C. Mark the prepared tubes with
26、 the pencil (5.4). Transfer the test portion (6.1) to a tube with the aid of the funnel (5.6).BS4140-13:1986 2 BSI 10-1999 Add exactly7,20ml of the hydrochloric acid solution(4.1) and 2ml of water for a test portion of1g or14,40ml of the hydrochloric acid solution and4ml of water for a test portion
27、of2g. Prepare two or three tubes under the same conditions, sealing them as follows. Using the glass-blowing equipment(5.3), join one end of a glass tube to the opening of the tube by simultaneous heating of the two glass parts until they are soft, in order to form a joint. Allow to cool just suffic
28、iently to obtain a rigid joint. Heat the top of the tube in the full flame at about10mm from the joint (turning the tube continually) until the walls are uniformly soft. Separate the two parts in the flame, with the minimum of pulling. After separation, heat the end of the tube in order to avoid a t
29、hick, protuberant joint. Do not overheat, or a slight swelling may be caused by a rise in the internal pressure of the gaseous atmosphere. Anneal the second closure in a reducing flame until it is coated with carbon black. 6.2.2 Dissolution of the test portion Shake the sealed tubes until the test p
30、ortion is completely mixed with the acid. Place the sealed tubes in the protecting tubes (5.8) and screw up the caps. Place the assembly, using the tube holder(5.5 or5.5.1), in the electric oven (5.7), controlled at 250 5 C, and leave them for about16h. After this period, allow the furnace to cool t
31、o about50 C, then cautiously remove the tubes and leave them to cool at room temperature. NOTEThe reaction time varies according to the type of aluminium oxide and its degree of calcination. For aluminium oxides calcined at high temperature, the reaction temperature can be raised to275 5 C but preca
32、utions shall then be taken as the increase in pressure resulting from the increase in temperature of the reaction may cause the tubes to burst. 6.2.3 Opening the tube Once the protecting tubes have cooled to room temperature, open them and withdraw the sealed tubes. Carefully wipe the carbon black f
33、rom the ends of the tubes, clean with cleaning solution, rinse with water and dry. By means of the glass cutter (5.3.3), trace a line around the upper part of the tube, above the level of the liquid. In order to break the tube, moisten the line with water and touch with the glass rod(5.2) brought to
34、 red heat. 6.2.4 Transfer of the solution Transfer the solution quantitatively from the tube into a beaker of suitable capacity (forexample400ml), with hot water and using a “policeman”, if necessary, to detach all salts which may have formed. Warm the solution to dissolve the salts and transfer the
35、 solution quantitatively to a one-mark volumetric flask of the capacity specified in the method for the determination of the impurity. 6.3 Preparation of the blank test solution Prepare a blank test solution, following the same procedure as that specified in 6.2, using the same quantities of all the
36、 reagents as used for the dissolution of the test portion and proceeding, in accordance with the instructions given in the International Standard relating to the determination to be carried out, in the presence or absence of extra-pure aluminium oxide.BS4140-13:1986 BSI 10-1999 3 Annex ISO publicati
37、ons relating to aluminium oxide primarily used for the production of aluminium ISO802, Preparation and storage of test samples. ISO803, Determination of loss of mass at300 C (conventionalmoisture). ISO804, Preparation of solution for analysis Method by alkaline fusion. ISO805, Determination of iron
38、content 1,10-Phenanthroline photometric method. ISO806, Determination of loss of mass at1000 and1200 C. ISO900, Determination of titanium content Diantipyrylmethane photometric method. ISO901, Determination of absolute density Pyknometer method. ISO 902, Measurement of the angle of repose. ISO 903,
39、Determination of untamped density. ISO 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
40、method. ISO 2069, Determination of calcium 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 P
41、AN photometric method. ISO 2073, Preparation 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 phosphomoly
42、bdate spectrophotometric method. ISO 2865, 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 meth
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