1、BRITISH STANDARD BS 549:1970 Specification for Diacetone alcoholBS549:1970 This British Standard, having been approved by the Chemicals Industry Standards Committee, was published under the authorityof the Executive Boardon 28August1970 BSI 12-1999 First published May1934 First revision March1950 Se
2、cond revision March1957 Third revision December1964 Fourth revision August1970 The following BSI references relate to the work on this standard: Committee references CIC/4 andCIC/4/5 Draft for comment 69/27345 ISBN 580 06013 6 Co-operating organizations The Chemicals Industry Standards Committee und
3、er whose supervision this British Standard was prepared, consists of representatives from the following Government departments and industrial organizations: Board of Trade British Steel Industry Chemical Industries Association* Department of Health and Social Security Fertilizer Manufacturers Associ
4、ation Gas Council Institution of Gas Engineers Ministry of Agriculture, Fisheries and Food Ministry of Technology Laboratory of the Government Chemist* National Sulphuric Acid Association Royal Institute of Public Health & Hygiene The Government department and industrial organization marked with an
5、asterisk in the above list, together with the following, were directly represented on the committee entrusted with the preparation of this British Standard. British Plastics Federation Ministry of Defence, Navy Department Oil and Colour Chemists Association Paintmakers Association of Great Britain P
6、harmaceutical Society of Great Britain Research Association of British Paint, Colour & Varnish Manufacturers Royal Institute of Chemistry Society of Chemical Industry Society of Motor Manufacturers and Traders Ltd. Toilet Preparations Federation Amendments issued since publication Amd. No. Date Comm
7、entsBS549:1970 BSI 12-1999 i Contents Page Co-operating organizations Inside front cover Foreword ii 1 Scope 1 2 Description 1 3 Colour 1 4 Relative density 1 5 Refractive index 1 6 Flash point 1 7 Water 1 8 Residue on evaporation 1 9 Acidity 1 10 Sampling and size of sample 1 Appendix A Limit test
8、for colour 2 Appendix B Method for the determination of residue on evaporation 2 Appendix C Method for the determination of acidity 2BS549:1970 ii BSI 12-1999 Foreword This standard makes reference to the following British Standards: BS 612, Nessler cylinders. BS 1792, One-mark volumetric flasks. BS
9、 2511, Methods for the determination of water (Karl Fischer method). BS 2839, Method for the determination of closed flash-point of petroleum products by means of the Pensky-Martens apparatus. BS 3591, Industrial methylated spirits. BS 3978, Water for laboratory use. This standard forms one of a ser
10、ies of British Standards for solvents and allied products, the preparation of which was authorized originally by the Fine Chemicals Industry Standards Committee (now merged in the Chemicals Industry Standards Committee). This British Standard was first issued in1934, and was last revised in1964. In
11、the present revision the limits for relative density, water content and acidity have been made more stringent. The requirement in respect of miscibility with water has been deleted but a limit for colour has been introduced. A British Standard does not purport to include all the necessary provisions
12、 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. Summary of pages This document comprises a front cover, an inside front cover, pagesiandii, pages1to4, an inside bac
13、k 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 amendment table on the inside front cover.BS549:1970 BSI 12-1999 1 1 Scope This British Standard specifies requirements for diacetone alcohol suitable
14、 for industrial purposes. 2 Description British Standard diacetone alcohol shall be clear and free from matter in suspension, and shall consist essentially of4-hydroxy-4-methylpentan-2- one, CH 3 COCH 2 C(OH)(CH 3 ) 2 . 3 Colour The colour of the material shall not exceed25Hazen units when measured
15、by the method described in Appendix A or by a suitable instrumental method. 4 Relative density The relative density 1)of the material at any one of the following temperatures shall be within the appropriate values as shown: 5 Refractive index The refractive index of the material at20 C for the sodiu
16、m D line shall be not lower than1.4230 and not higher than1.4245. 6 Flash point The flash point of the material, determined by the method described in BS2839 2)shall be not lower than52.0 C. 7 Water The material shall not contain more than0.25% by mass of water, determined by the method described in
17、 BS2511 3) , Part 4 and using20ml of the material. 8 Residue on evaporation The material shall not leave more than0.02% by mass of residue when tested by the method described in Appendix B. 9 Acidity The material shall not contain more than0.010% by mass of acid, calculated as acetic acid, CH 3 COOH
18、, and determined by the method described in Appendix C. 10 Sampling and size of sample A representative sample of the material measuring not less than one litre shall be taken from the bulk for the purpose of examination in accordance with this specification. The sample shall be placed in a clean, d
19、ry and airtight glass-stoppered bottle of such a size that it is nearly filled by the sample. When it is necessary to seal the container, care shall be taken to avoid the risk of contaminating the contents in any way. 1) Ratio of the density of a liquid at a specified temperature to the density of w
20、ater at a specified temperature. Temperature Relative density C min. max. 20/4 0.936 0.939 20/20 0.938 0.941 25/25 0.934 0.937 2) BS2839, “Method for the determination of closed flash-point of petroleum products by means of the Pensky-Martens apparatus”. 3) BS2511, “Methods for the determination of
21、water (Karl Fischer method)”.BS549:1970 2 BSI 12-1999 Appendix A Limit test for colour A.1 Apparatus The following apparatus is required: 1) Two matched Nessler cylinders 4) , 100ml. capacity. 2) One-mark volumetric flask 5) , 500ml capacity. 3) One-mark volumetric flask 5) , 250ml capacity. A.2 Rea
22、gents The reagents used shall be of a recognized analytical reagent quality. Water complying with BS3978 6)shall be used throughout. 1) Cobaltous chloride, hexahydrate. 2) Hydrochloric acid, concentrated36% (m/m) (11N). either 3) Chloroplatinic acid reagent. Dissolve250mg of platinum in a small quan
23、tity of aqua regia contained in a glass or porcelain basin by heating on a water bath. When the metal has dissolved evaporate the solution to dryness. Add1ml of the hydrochloric acid and again evaporate to dryness. Repeat this operation twice more. or 4) Potassium chloroplatinate A.3 Preparation of
24、colour standard Dissolve0.50g of the cobaltous chloride hexahydrate and either the whole of the chloroplatinic acid (prepared as described above) or0.623g of potassium chloroplatinate in50ml of the hydrochloric acid. Warm, if necessary, to obtain a clear solution and after cooling, pour into the500m
25、l volumetric flask. Dilute with water to the mark and mix well. This solution has a colour of500Hazen units. Pipette12.5ml of this solution into the250ml volumetric flask. Dilute with water to the mark. This diluted solution has a colour of25Hazen units and should always be freshly prepared. A.4 Pro
26、cedure Fill one of the Nessler cylinders to the mark with the sample, and the other with the colour standard. Using a white background compare the colours. Appendix B Method for the determination of residue on evaporation B.1 Procedure Pipette100ml of the sample into a weighed glass evaporating dish
27、 on a boiling water bath. Blow a stream of filtered air onto the surface of the liquid from a jet1mm in diameter, with the tip of the jet10mm above the edge of the dish and under a pressure of50mm of water. Evaporate the sample to dryness and dry the residue for one hour in an oven at a temperature
28、of105 5 C. Cool in a desiccator and weigh. Dry the residue in the oven again for30minutes, cool in the desiccator and weigh again. Repeat, if necessary, until two successive weighings do not differ by more than1mg. B.2 Calculation Residue on evaporation, per cent by mass, Appendix C Method for the d
29、etermination of acidity C.1 Reagents The reagents used shall be of a recognized analytical reagent quality. Water, complying with BS3978 6) , shall be used throughout. 1) Sodium hydroxide, 0.1N standard volumetric solution. 2) Phenolphthalein indicator solution, 10g/l. Dissolve2.5g of phenolphthalei
30、n in250ml of ethanol 7) , 95% (v/v) and make faintly pink by the addition of dilute sodium hydroxide solution. 4) BS612, “Nessler cylinders”. 5) BS1792, “One-mark volumetric flasks”. 6) BS3978, “Water for laboratory use”. = where M = mass, in grammes, of residue and d = relative density of the sampl
31、e. 7) Ethanol may be replaced by industrial methylated spirits, 66degrees O.P., complying with BS3591. It should be noted that the use of industrial methylated spirits is governed by The Methylated Spirits Regulations1952 (S.I. 1952, No. 2230). M d -BS549:1970 BSI 12-1999 3 C.2 Procedure Place100ml
32、of water and a few pieces of clean porous pot in a500ml conical flask of borosilicate glass and boil gently for five minutes to eliminate carbon dioxide. Cool slightly and add50ml of the sample. Boil gently for a further5minutes. At the end of this period close the neck of the flask with a stopper c
33、arrying a soda-lime tube and allow to cool. When cold remove the stopper, add0.5ml of the plenolphthalein indicator and titrate with the sodium hydroxide solution using a microburette. C.3 Calculation Acidity, calculated as acetic acid, CH 3 COOH, percent by mass = where V = volume, in millilitres,
34、of 0.1N sodium hydroxide solution used and d = relative density of the sample. 0.012V d -4 blankBS549:1970 BSI 12-1999 British Standards Institution The following are available on application: YEARBOOK Including subject index and numerical list of British Standards SECTIONAL LISTS. Gratis. Acoustics
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