1、BRITISH STANDARD BS 6092-6: 1981 ISO 2122:1972 Incorporating Amendment No. 1 Methods of Sampling and test for sodium and potassium silicates for industrial use Part 6: Preparation of solutions of not readily soluble products and determination of matter insoluble in water ISO title: Sodium and potass
2、ium silicates for industrial use Preparation of solution of products not easily soluble in boiling water and determination of matter insoluble in water NOTEIt is recommended that this Part be read in conjunction with the information in the “Generalintroduction” published separately as BS 6092-0. UDC
3、 661.683/.684:546.32284 + 546.33284:66.061.1 + 543.725BS6092-6:1981 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, waspublished under the authorityofthe Executive Boardand comes into effect on 27 February 1981 BSI 12-1999 The following BSI refere
4、nces relate to the work on this standard: Committee reference CIC/22 Draft for comment 73/55424 DC ISBN 0 580 12040 6 Amendments issued since publication Amd. No. Date of issue Comments 3875 December 1981 Indicated by a sideline in the marginBS6092-6:1981 BSI 12-1999 i Contents Page National forewor
5、d ii 1 Scope 1 2 Field of application 1 3 References 1 4 Principle 1 5 Reagents 1 6 Apparatus 1 7 Procedure 1 8 Expression of results 2 9 Special case 2 10 Test report 3 Figure Suitable autoclave for the preparation of an aqueous solution of silicates not easily soluble 3 Publications referred to In
6、side back coverBS6092-6:1981 ii BSI 12-1999 National foreword This Part of BS6092 is identical with ISO2122 “Sodium and potassium silicates for industrial use Preparation of solution of products not easily soluble in boiling water and determination of matter insoluble in water”, published in1972by t
7、he 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 conventions are not identical with those used in British St
8、andards; attention is especially drawn to the following. Wherever the words “International Standard” appear, referring to this standard, they should be read as “British Standard”. There is no British Standard corresponding directly to ISO1686 which is referred to in this standard as ISO/R1686 and to
9、 which reference is made in7.1. Technically equivalent information on sampling is given in BS6092-0. Additional information WARNING. It is essential that autoclaves (see6.1 and9.3.1) are properly maintained and regularly tested in accordance with manufacturers instructions. In use (see7.2 and 9.4.2)
10、, it is essential that the liquid in the autoclave is cooled to room temperature before the autoclave is opened. Water. Water complying with the requirements of BS3978 “Water for laboratory use” is suitable for the preparation of carbon dioxide-free water as described in5.1. A British Standard does
11、not purport to include 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. Cross-references International Standard Corresponding British Sta
12、ndard BS 6092 Methods of sampling and test for sodium and potassium silicates for industrial use ISO 1690:1976 a Part 3:1981 Determination of silica content (Identical) ISO 1691:1976 b Part 4:1981 Determination of carbonate content (Identical) a Referred to in this standard as ISO/R 1690. b Referred
13、 to in this standard as ISO/R 1691. 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 date) and may have had amendments incorporated. This will be indicated
14、in the amendment table on the inside front cover.BS6092-6:1981 BSI 12-1999 1 1 Scope This International Standard specifies a method for dissolving sodium or potassium silicates that are not easily soluble in boiling water at atmospheric pressure, and also a method for the determination of matter ins
15、oluble in water. NOTEWhen the method described in this International Standard is used, the masses of sample laid down in ISO/R1690 and ISO/R1691 must be replaced by taking corresponding quantities of the solution, and the expression of the results must be modified accordingly. 2 Field of application
16、 The method is applicable to the treatment of products corresponding to the general formula M 2 O.xSiO 2 , where the values of x lie between: 1.5 and 3.5 in the case of sodium silicates; 1.9 and 3.9 in the case of potassium silicates. 2.1 Special case Preparation of solution of products correspondin
17、g to the general formula M 2 O.xSiO 2 , where the values ofx are greater than the values shown above. Because of the difficulty encountered in dissolving fine particles of these products, the sample is first sieved to remove these fines. The homogeneity of the fused material is considered to be suff
18、icient to allow this size segregation. 3 References ISO/R 1686, Sodium and potassium silicates for industrial use Samples and methods of test General. ISO/R 1690, Sodium and potassium silicates for industrial use Determination of silica content Gravimetric method by insolubilization. ISO/R 1691, Sod
19、ium and potassium silicates for industrial use Determination of carbon dioxide content expressed as sodium or potassium carbonate Gas-volumetric method. 4 Principle Dissolution of the test portion in carbon dioxide-free water, by treatment in an autoclave. Filtration and weighing of the insoluble ma
20、tter on a tared filter crucible. Dilution of the filtrate to a given volume, from which aliquot samples are taken in order to carry out the different determinations. 5 Reagents 5.1 Carbon dioxide-free water This can be obtained either by boiling for10min, followed by cooling, with protection from at
21、mospheric carbon dioxide by means of a soda lime tube, or by bubbling nitrogen or carbon dioxide-free air through distilled or demineralized water for approximately10min, and storage under protection from atmospheric carbon dioxide. 5.2 Indicator paper, covering neutral range (pH6to8). 6 Apparatus O
22、rdinary laboratory apparatus and 6.1 Stainless steel autoclave, approximately300ml effective capacity allowing a pressure of the order of600kN/m 2(i.e.6bars) to be reached. (SeetheFigure, for an example of a suitable autoclave.) 6.2 Filter crucible, with sintered disk of porosity between15and404m. 7
23、 Procedure 7.1 Test portion Weigh, to the nearest0.1g, 100g of the laboratory sample (see ISO/R1686) in the form of grains not exceeding904m in size. A different quantity may be taken, if using an apparatus of suitable capacity, provided that the ratio of product to water is maintained. 7.2 Preparat
24、ion of solution Place the test portion (7.1) in the autoclave (6.1), and add200ml of the water(5.1). Heat the autoclave, immersed in an oil bath, at a temperature between 135and160 C for3h in the case of sodium silicate, and at150 C (maximum) for90min in the case of potassium silicate. Measure the t
25、emperatures in the oil bath. Allow to cool to ambient temperature. 7.3 Determination of matter insoluble in water Empty the autoclave. Rinse inside with water (5.1). Filter together under vacuum the solution and rinsing water on the filter crucible (6.2), previously tared to the nearest0.1mg after d
26、rying for1h at between110 and120 C and cooling in a desiccator. Wash the insoluble matter with the water (5.1) until the pH of the filtrate, measured with the aid of the indicator paper (5.2), is not greater than7. Dry the filter crucible and its contents for1h at a temperature between110and120 C, a
27、nd reweigh the whole to the nearest0.1mg, after cooling in a desiccator to room temperature.BS6092-6:1981 2 BSI 12-1999 7.4 Preparation of the sample solution Transfer the filtered solution quantitatively to a1000ml one-mark volumetric flask. Dilute to themark with water (5.1) and mix. This solution
28、, which should be used in carrying out the various determinations, contains approximately0.1g of sample per millilitre. 8 Expression of results Water insoluble matter is given, as a percentage by mass, by the formula: (m 2 m 3 ) where m 1 is the mass, in grams, of the test portion; m 2 is the mass,
29、in grams, of the filter crucible containing the insoluble matter; m 3 is the mass, in grams, of the filter crucible alone. 9 Special case Preparation of solution of products corresponding to the general formula M 2 O.xSiO 2 , where the values ofx are greater than3.5in the case of sodium silicates an
30、d3.9in the case of potassium silicates. 9.1 Principle See section4, the filter crucible, however, being replaced by filter paper. 9.2 Reagents See section5. 9.3 Apparatus Ordinary laboratory apparatus and 9.3.1 Stainless steel autoclave, approximately150ml effective capacity, capable of being heated
31、 to150 C (the internal pressure at this temperature is of the order of480kN/m 2 , i.e.4.8bars). 9.3.2 Ashless filter papers, medium texture, 125mm diameter, resistant to the action of silicates. 9.4 Procedure 9.4.1 Test portion Grind100to200 g of the laboratory sample (seeISO/R1686). Sift the materi
32、al through two superimposed sieves of7104m and1804m mesh respectively, and regrind if necessary until the whole of the sample has passed through the7104m mesh sieve. Weigh, to the nearest0.01g, 30g of the fraction of sample having a particle size between180 and7104m. The method described below invol
33、ves the dissolution of30g of the sample, when using the autoclave (9.3.1). A different quantity may be taken, if using an apparatus of suitable capacity, provided that the ratio of product to water is maintained. 9.4.2 Preparation of solution Place the test portion (9.4.1) in the autoclave (9.3.1),
34、add100ml of water (5.1) in the case of sodium silicate or75ml of water in the case of potassium silicate, and close the apparatus. Rotate the autoclave on a suitable device for90min in a thermostatically controlled bath set at about150 C, then take it out and allow it to cool to room temperature. 9.
35、4.3 Determination of matter insoluble in water Open the apparatus and add to the contents about50ml of water heated to about70 C. Mix, then filter on a Bchner funnel under vacuum through a filter paper (9.3.2) which has been previously dried for1h at between110and120 C, cooled in a desiccator to roo
36、m temperature and weighed to the nearest0.1mg in a weighing bottle. Wash the insoluble matter in water (5.1) until the pH of the filtrate, measured with the aid of the indicator paper (5.2), is not greater than7. Remove the filter paper from the funnel and weigh it again in the same weighing bottle
37、to the nearest0.1mg after drying it for1h at between110and120 C and cooling in a desiccator to room temperature. 9.4.4 Preparation of the sample solution Transfer the filtered solution quantitatively to a1000ml one-mark volumetric flask, dilute to the mark with water (5.1) and mix. This solution, wh
38、ich serves for carrying out the various determinations, contains about0.03g of the sample per millilitre. 9.5 Expression of results Use the formula of section8, where m 2 is the mass, in grams, of the weighing bottle containing the filter paper and the insoluble matter; m 3 is the mass, in grams, of
39、 the weighing bottle containing the filter paper only.100 m 1 - BS6092-6:1981 BSI 12-1999 3 10 Test report The test report shall include the following particulars: a) the reference of the method used; b) the results and the method of expression used; c) any unusual features noted during the determin
40、ation; d) any operation not included in this International Standard, or regarded as optional. Figure Suitable autoclave for the preparation of an aqueous solution of silicatesnot easily soluble4 blankBS6092-6:1981 BSI 12-1999 Publications referred to See national foreword.BS 6092-6: 1981 ISO 2122:19
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