1、BRITISH STANDARD BS 4140-8: 1986 ISO 901:1976 Methods of test for Aluminium oxide Part 8: Determination of absolute density using a pyknometer ISO title: Aluminium oxide primarily used for the production of aluminium Determination of absolute density Pyknometer method NOTEIt is recommended that this
2、 Part be read in conjunction with the general information given in BS 4140-0 “General introduction” which is issued separately. UDC 546.623 31:620.1BS4140-8:1986 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authorityofth
3、e Board of BSIandcomes into effect on 31 January 1986 BSI 11-1999 The committees responsible for this British Standard are shown inPart 0. The following BSI references relate to the work on this standard: Committee reference CIC/24 Draft for comment 85/52363 DC ISBN 0 580 14918 8 Amendments issued s
4、ince publication Amd. No. Date of issue CommentsBS4140-8:1986 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 2 7 Expression of results 4 8 Test report 4 Annex ISO Publications relating to alumini
5、um oxide primarily used for the production of aluminium 5 Figure 1 Pyknometer (5.1) 1 Figure 2 Degassing apparatus (5.2) 2 Publications referred to Inside back coverBS4140-8:1986 ii BSI 11-1999 National foreword This Part of BS4140 is identical with ISO901:1976 “Aluminium oxide primarily used for th
6、e production of aluminium Determination of absolute density Pyknometer method” published by the International Organization for Standardization (ISO). This method supersedes clause8 of Addendum No.1(1970) to BS4140:1967. Parts8to10 of this standard collectively supersede Addendum No.1(1970) to BS4140
7、:1967, which is withdrawn.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 es
8、pecially 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 (and its submultiples) rather than“l”. Wherever
9、the words “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 BS4140-0 “General information”. This stan
10、dard 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 BS4140-8:1986. A British Standard does not purport to include all the necessary provisions of a contr
11、act. Users 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
12、 Part 1:1986 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 6, an inside back cover and a back cover. This standard has been updated (see copy
13、right date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS4140-8:1986 BSI 11-1999 1 1 Scope and field of application This International Standard specifies a pyknometer method for the determination of the absolute density of alumin
14、ium oxide primarily used for the production of aluminium. 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 production of aluminium Sampling. 3 Principle Determination, by a p
15、yknometer method, of the absolute density of aluminium oxide after complete degasification. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Xylene, 0,860to0,865g/ml, distilling between138and144 C. NOTETo ens
16、ure absence of a volatile fraction, the xylene shall distil within the given range. 4.2 Ethanol, 95% (V/V) solution, approximately0,81g/ml. 4.3 Diethyl ether, approximately0,715g/ml. 5 Apparatus Ordinary laboratory apparatus and 5.1 Pyknometer (seeFigure 1), consisting of 5.1.1 Flask (A), of capacit
17、y approximately 25ml, fitted with a side arm with a ground glass cover (F). 5.1.2 Thermometer (B), covering the range15to25 C, graduated in intervals of0,1 C, which can be fitted to the flask by a ground glass joint. 5.2 Degassing and filling apparatus (seeFigure 2), consisting of a tap funnel (C) o
18、f capacity about50ml, fitted with a side arm, with a tap (D) for connecting to the vacuum pump(5.4). This can be fitted to the pyknometer flask (A) by means of a conical ground glass joint (E). Figure 1 Pyknometer (5.1)BS4140-8:1986 2 BSI 11-1999 5.3 Water bath, capable of being controlled at20 0,1
19、C. 5.4 Vacuum pump, capable of giving a vacuum below 1,33kPa (10mmHg). 5.5 Mercury manometer 6 Procedure 6.1 General 6.1.1 Always weigh the pyknometer with the thermometer and the side tube cover in position. 6.1.2 Always weigh to the nearest0,0001g. 6.1.3 When the pyknometer contains liquid, stabil
20、ize its temperature at20 0,10 C. 6.2 Determination 6.2.1 Determination of the mass of the pyknometer Wash the pyknometer (5.1), including its accessories, with lukewarm chromic-sulphuric acid, taking all necessary precautions. Thoroughly rinse, first with tap water, then with distilled water and eth
21、anol (4.2) and finally with diethyl ether (4.3). Thoroughly dry the apparatus and weigh. Let m 0be the mass, in grams, of the dry pyknometer. Figure 2 Degassing apparatus (5.2)BS4140-8:1986 BSI 11-1999 3 6.2.2 Determination of the volume of the pyknometer Fill the pyknometer (5.1) with distilled wat
22、er and connect via the degassing apparatus (5.2) to the vacuum pump (5.4), the mercury manometer (5.5) being inserted to control the vacuum. Close the side tube of the pyknometer with its cover (F) and slowly open tap (D) and apply the vacuum for approximately15min. Occasionally tap the walls of the
23、 pyknometer to facilitate the release of any air bubbles. Restore atmospheric pressure in the pyknometer, disconnect it from the degassing apparatus (5.2) and put the thermometer (B) in position. Stabilize the temperature of the pyknometer in the water bath (5.3), previously adjusted to20 0,1 C. Com
24、pletely fill the side tube with water, using a length of narrow glass tubing. Remove the pyknometer from the water bath, cool slightly under running cold water and close the side tube with its ground glass cover (F). Carefully dry the pyknometer and weigh. The volume V, in millimetres, of the pyknom
25、eter, is given by the formula where m 0 is the mass, in grams, of the dry pyknometer; m 1 is the mass, in grams, of the pyknometer filled with degassed distilled water; 0,998 2 is the absolute density of water, in grams per millilitre, at20 C. 6.2.3 Determination of the absolute density of xylene Fi
26、ll the pyknometer (5.1) with xylene (4.1) after having determined its mass as in6.2.1. Carry out the procedure specified in6.2.2,i.e.degas, stabilize the temperature at20 0,1 C in the water bath(5.3), fill, cool and finally weigh. The weighing shall be carried out quickly to avoid loss of xylene by
27、evaporation. The mass m x , in grams, of xylene equivalent to the volume V of the pyknometer is given by the formula where m 0 is the mass, in grams, of the dry pyknometer; m 2 is the mass, in grams, of the pyknometer full of xylene. The absolute density x , in grams per millilitre, of xylene is giv
28、en by the formula where m x is the mass, in grams, of xylene equivalent to the volume V of the pyknometer; V is the volume, in millilitres, of the pyknometer. 6.2.4 Test portion Transfer to the flask of the pyknometer (5.1), previously weighed in accordance with6.2.1, about10g of the test sample, dr
29、ied at300 C (see3.3 ofISO802) and weigh. The mass m e , in grams, of the test portion is given by the formula m e= m 3 m 0 where m 0 is the mass, in grams, of the dry pyknometer; m 3 is the mass, in grams, of the pyknometer and test portion. 6.2.5 Determination of the absolute density of the alumini
30、um oxide Moisten the ground glass joints of the pyknometer containing the test portion (6.2.4) with a little xylene (4.1) and insert the degassing apparatus(5.2). Connect the latter to the vacuum produced by the pump (5.4) and controlled by means of the mercury manometer (5.5). Close the side tube w
31、ith its cover (F), gently open tap (D) and apply vacuum for15min. Close tap (D) and slowly run in xylene from the tap funnel (E) until the test portion is just covered. Carefully re-open tap (D), still connected to the vacuum pump, and occasionally tap the walls of the pyknometer to facilitate the r
32、elease of any air bubbles adhering to the walls. NOTEWhen the test portion is placed with the xylene in the pyknometer, the expulsion of air trapped in the aluminium oxide covered with xylene is facilitated by the use of high-frequency (for example,120kHz) vibrations. Then fill the pyknometer with t
33、he xylene (4.1) up tothe ground glass joint and insert the thermometer (B). Stabilize the temperature of the pyknometer in the water bath (5.3), previously adjusted to20 0,1 C. Completely fill the side arm with xylene, using a length of narrow glass tubing. Remove the pyknometer from the water bath,
34、 cool slightly under running cold water and close the side arm with its ground glass cover (F). Dry thoroughly and weigh the pyknometer quickly, because of the tendency for xylene to evaporate. V m 1 m 0 () 0,998 2 - = m x m 2 m 0 = x m x V - =BS4140-8:1986 4 BSI 11-1999 The total mass m e + x , in
35、grams, of the test portion and additional xylene required to fill the pyknometer is given by the formula m e + x= m 4 m 0 where m 0 is the mass, in grams, of the dry pyknometer; m 4 is the mass, in grams, of the pyknometer containing the test portion and filled with xylene. 7 Expression of results T
36、he absolute density , in grams per millilitre, of aluminium oxide is given by the formula where m e is the mass, in grams, of the test portion(6.2.4); m x is the mass, in grams, of xylene required to fill the pyknometer volume V; m e + x is the mass, in grams, of the test portion and of the addition
37、al xylene required to fill the pyknometer volume V; x is the absolute density, in grams per millilitre, of xylene. Indicate the absolute density to three places of decimals, two of which should be significant figures. 8 Test report The test report shall include the following particulars: a) the refe
38、rence of the method used; b) the results and the method of expression used; c) any unusual features noted during the determination; d) any operation not included in this International Standard or in the International Standards to which reference is made, or regarded as optional.BS4140-8:1986 BSI 11-
39、1999 5 Annex ISO Publications relating to aluminium oxide primarily used 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.
40、ISO 805, Determination of iron content 1,10-Phenanthroline photometric method. 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
41、 of the angle of repose. ISO 903, 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-
42、N-phenylhydroxylamine photometric 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 207
43、2, Determination of zinc content PAN 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 phos
44、phorus content Reduced phosphomolybdate 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 co
45、ntent Flame atomic absorption method.6 blankBS4140-8:1986 BSI 11-1999 Publications referred to See national foreword.BS 4140-8: 1986 ISO 901:1976 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. I
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