1、BRITISH STANDARD BS6829-4.5: 1989 ISO4322:1977 Analysis of surface active agents (rawmaterials) Part4: Ethylene oxide adducts Section4.5 Method for determination of sulphated ash UDC661.185.1:543.2112BS6829-4.5:1989 This BritishStandard, having been prepared under the directionof the Chemicals Stand
2、ards Policy Committee, waspublished under the authorityof the Board of BSI and comes into effect on 29September1989 BSI12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft for comment88/55478DC ISBN 0 580 17669 X Committees responsible for this B
3、ritishStandard The preparation of this BritishStandard was entrusted by the Chemicals Standards Policy Committee (CIC/-) to Technical Committee CIC/34 upon which the following bodies were represented: Chemical Industries Association Consumer Policy Committee of BSI Department of the Environment Depa
4、rtment of Trade and Industry (Laboratory of the Government Chemist) London Regional Transport Ministry of Defence Royal Society of Chemistry Soap and Detergent Industry Association Society of Dyers and Colourists Amendments issued since publication Amd. No. Date of issue CommentsBS6829-4.5:1989 BSI
5、12-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope and field of application 1 2 Reference 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Sampling 1 7 Procedure 1 8 Expression of results 2 9 Test report 2 Publications referred to Inside back coverBS6829-4.5:1
6、989 ii BSI 12-1999 National foreword This Section of BS6829 has been prepared under the direction of the Chemicals Standards Policy Committee. It is identical with ISO4322:1977 “Non-ionic surface active agentsDetermination of sulphated ashGravimetric method” published by the International Organizati
7、on for Standardization (ISO). Additional information. With reference to clause4, water complying with grade3 of BS3978 “Specification for water for laboratory use” is suitable. Withreference to4.2, the sulphuric acid solution, expressed as an amount-of-substance concentration, is c(H 2 SO 4 )=3mol/L
8、. With reference to the seventh main paragraph of7.3 (“Allow to cool. . .”) in the UK it is common practice always to include this operation, in view of the high cost of platinum crucibles. Textual error. When adopting the text of the International Standard, the textual error given below was discove
9、red. It has been marked in the text and hasbeen reported to ISO in a proposal to amend the text of the InternationalStandard. The formula given in8.1 should be read as: This Section describes a method of test only, and should not be used or quoted as a specification defining limits of purity. Refere
10、nce to this Section should indicate that the method of test used is in accordance with BS6829-4.5. A British Standard does 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 d
11、oes not of itself confer immunity from legal obligations. Cross-reference International Standard Corresponding BritishStandard ISO607:1980 a BS3762 Analysis of formulated detergents Part1:1983 Methods of sample division (Identical) a Footnote1) to clause2 is no longer applicable as ISO607 has now be
12、en published. m 1 m 0 -100 Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, pages1 and 2, 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 ame
13、ndment table on the inside front cover.BS6829-4.5:1989 BSI 12-1999 1 1 Scope and field of application This International Standard specifies a gravimetric method for the determination of the sulphated ash of non-ionic surface active agents in general. 2 Reference ISO607, Surface active agentsDetergen
14、ts Methods of sample division 1) . 3 Principle Calcination of a test portion in the presence of sulphuric acid solution and weighing of the ash in the form of sulphate. 4 Reagents During the analysis, use only reagents of analytical grade and only distilled water or water of at least equivalent puri
15、ty. 4.1 Ammonium nitrate (NH 4 NO 3 ) 4.2 Sulphuric acid, approximately6N solution, free from ash. 5 Apparatus Ordinary laboratory apparatus and 5.1 Platinum crucible, capacity100ml. 5.2 Furnace, capable of being controlled at775 25 C. 5.3 Gas burner 6 Sampling The laboratory sample of the non-ionic
16、 surface active agent shall be prepared and stored according to the instructions given in ISO607. 7 Procedure 7.1 Treatment of the laboratory sample Mix the laboratory sample; if necessary, gently melt the product without overheating to make homogenization possible. NOTEThis test sample obtained sha
17、ll then be used only for this determination. 7.2 Test portion Before weighing the test portion, heat the crucible(5.1) at775 25 C for10min and, after cooling, place it in a desiccator until it reaches ambient temperature and weigh it to the nearest0,1mg. Place about30g, weighed to the nearest0,1mg,
18、of the laboratory sample(7.1) in the tared crucible. 7.3 Determination CAUTION: It is essential to wear safety goggles and to carry out the combustion in a fume cupboard. Place the crucible containing the test portion(7.2) above a low flame of a gas burner. Warm gently until a small flame played on
19、the product initiates burning at as low a temperature as possible. Then withdraw the burner and allow the combustion to proceed unaided. NOTEIt is important to allow the combustion to proceed unaided and gently because, if it is accelerated by keeping the burner under the crucible, the rapid burning
20、 which will result will give rise to spattering out of the crucible and consequent loss of product. When combustion has stopped, replace the gas burner under the crucible. If the spontaneous combustion recommences, withdraw the burner again and allow to burn until extinction and so on for as long as
21、 spontaneous combustion is produced by replacing the burner under the crucible. NOTEIn practice, the re-ignition can occur three or four times and this step in the procedure can last for30 to60min. After having obtained a carbonaceous residue, proceed to the calcination proper. Allow the crucible an
22、d its contents to cool, add several crystals (about0,1g) of the ammonium nitrate(4.1) and thoroughly wet the residue with0,5ml of the sulphuric acid solution(4.2). Place the crucible on the flame, gradually increase the temperature to dull red and maintain at this temperature until the carbon has bu
23、rnt completely. Allow to cool and if necessary add some of the ammonium nitrate and some of the sulphuric acid solution so as to avoid attack of the platinum crucible by sulphides. Again heat the crucible on the flame to dull red, then introduce it into the furnace(5.2), controlled at775 25 C, and l
24、eave for20 to30min. Cool the crucible slightly, place it in a desiccator until ambient temperature is reached and then weigh it to the nearest0,1mg. Replace the crucible in the furnace, controlled at775 25 C, and leave for20min. Allow to cool as before and re-weigh. Repeat the operations of heating
25、in the furnace, cooling and weighing until two successive weighings do not differ by more than1mg. NOTEIf the required agreement between two successive weighings is not achieved after the sequence of operations has been repeated three times, add several drops of the sulphuric acid solution(4.2) befo
26、re continuing. 1) In preparation. (Revision of ISO/R607.)BS6829-4.5:1989 2 BSI 12-1999 8 Expression of results 8.1 Method of calculation The sulphated ash is given, as a percentage by mass, by the formula 8.2 Reproducibility The difference between the results obtained on the same sample in two diffe
27、rent laboratories should not exceed0,1% for sulphated ash levels of about1%. 9 Test report The test report shall include the following particulars: a) all information necessary for the complete identification of the sample; b) the method used; c) the results obtained and the form in which they are e
28、xpressed; d) the test conditions; e) any operation not included in this International Standard or regarded as optional, as well as any incidents which may have affected the results. a a Seenational foreword for details of textual error where m 0 is the mass, in grams, of the test portion; m 1 is the
29、 mass, in grams, of the sulphated ash. m 1 m 1 -100 BS6829-4.5:1989 BSI 12-1999 Publications referred to Seenational foreword.BS6829-4.5: 1989 ISO4322:1977 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishSt
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