1、BRITISH STANDARD BS 1940:1987 Specification for Butanone (ethyl methyl ketone) for industrial use UDC 661.727.6BS1940:1987 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authorityofthe Board of BSIandcomes into effect on 2
2、8 August 1987 BSI 12-1999 First published February 1953 First revision February 1968 Second revision August 1987 The following BSI references relate to the work on this standard: Committee reference CIC/51 Draft for comment 85/55847 DC ISBN 0 580 15820 9 Committees responsible for this British Stand
3、ard The preparation of this British Standard was entrusted by the Chemicals Standards Committee (CIC/-) to Technical Committee CIC/51, upon which the following bodies were represented: British Pharmacopoeia Commission British Society of Perfumers Chemical Industries Association Department of Trade a
4、nd Industry (Laboratory of the Government Chemist) Royal Society of Chemistry Amendments issued since publication Amd. No. Date of issue CommentsBS1940:1987 BSI 12-1999 i Contents Page Committees responsible Inside front cover Foreword ii 1 Scope 1 2 Description 1 3 Sampling and size of sample 1 4 C
5、olour 1 5 Density 1 6 Distillation range 1 7 Residue on evaporation 1 8 Water content 1 9 Acidity 1 10 Alcoholic impurities 1 Appendix A Determination of distillation range 2 Appendix B Determination of acidity 2 Appendix C Determination of alcoholic impurities 2 Publications referred to Inside back
6、 coverBS1940:1987 ii BSI 12-1999 Foreword This British Standard, which has been prepared under the direction of the Chemicals Standards Committee, comprises a specification for butanone to meet the requirements of a wide range of industrial users. This British Standard supersedes BS1940:1968 which i
7、s withdrawn. In this revision of BS1940 the requirement for water content has been made more stringent and the requirement for relative density has been replaced by one for density at20 C. This British Standard is related to ISO2497:1973 but is not equivalent in technical content. ISO2497 is publish
8、ed by the International Organization for Standardization (ISO). ISO2497 lists various general test methods and test methods specifically for butanone, and many of these methods correspond to those which are referred to in this British Standard; ISO2497 does not specify limits for any of the properti
9、es of butanone. Appendix B of this British Standard is related to ISO2887:1973 but is not equivalent in technical content. ISO2887 is published by ISO. The main differences are that in the method described in ISO2887 the test portion is diluted with either ethanol or propan-2-ol and carbon dioxide i
10、s removed by passing a stream of nitrogen through the solution. Appendix C of this British Standard is related to ISO2501:1974 but is not equivalent in technical content. ISO2501 is published by ISO. The main differences are that in the method described in ISO2501 phenolphthalein is used as the indi
11、cator and the calculation of results includes a correction for the acidity of the sample. 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 does not o
12、f itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 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
13、 be indicated in the amendment table on the inside front cover.BS1940:1987 BSI 12-1999 1 1 Scope This British Standard specifies requirements for butanone suitable for industrial purposes. NOTEThe titles of the publications referred to in this standard are listed on the inside back cover. 2 Descript
14、ion The material shall be clear and free from matter in suspension, as assessed by visual inspection, and shall consist essentially of butanone, CH 3 COC 2 H 5 . 3 Sampling and size of sample 1) A representative sample of the material measuring not less than1L shall be taken from the bulk for the pu
15、rpose of examination in accordance with this standard. The sample shall be placed in a clean, dry and air-tight, ground glass-stoppered bottle, or screw-capped bottle fitted with a polyethylene cone insert, of such capacity that it is almost filled by the sample. NOTE 1When it is necessary to seal t
16、he container, care should be taken to avoid the risk of contaminating the contents in any way. NOTE 2Sufficient ullage should be left in the bottle to avoid excessive pressure changes that could arise from temperature variations during storage and handling. About10% ullage is recommended. 4 Colour T
17、he colour of the material shall not exceed10Hazen units when measured by the method described inBS5339. 5 Density The density of the material at20 C, determined by the method described in BS4522, shall be not lower than0.803g/mL and not higher than0.805g/mL. 6 Distillation range When the material is
18、 distilled by the method described in BS4591, modified as described inAppendix A, the initial boiling point at1013mbar 2)pressure shall be not lower than79.0 C and the dry point at1013mbar pressure shall be not higher than81.0 C. 7 Residue on evaporation The residue on evaporation of the material sh
19、all not exceed0.002% (m/m) when determined by the method described in BS4524. 8 Water content The material shall contain not more than0.15% (m/m) of water when determined by one of the methods described in clause5 of BS2511:1970 using20mL of the material. 9 Acidity The acidity of the material, calcu
20、lated as acetic acid (CH 3 COOH), shall not exceed0.004% (m/m) when determined by the method described inAppendix B. 10 Alcoholic impurities The material shall contain not more than0.7% (m/m) of alcoholic impurities, calculated as butanol (C 4 H 9 OH), when determined by the method described inAppen
21、dix C. 1) Detailed information on the sampling of liquid chemical products is given in BS5309-1 and BS5309-3. 2) 1 mbar = 100N/m 2= 100Pa.BS1940:1987 2 BSI 12-1999 Appendix A Determination of distillation range Determine the distillation range, in terms of the initial boiling point and the dry point
22、, by the method described in BS4591, using the following thermometer, distillation conditions and temperature corrections. a) Thermometer (3.2 of BS4591:1971). Use a thermometer designatedF100C/100 complying with BS593. b) Distillation (6.1 of BS4591:1971). Regulate the rate of heating so that the f
23、irst drop of distillate falls from the end of the condenser after10min to15min. c) Corrections to be applied to observed temperatures (7.2 of BS4591:1971). If the corrected barometric pressure deviates from1013mbar apply corrections to the observed temperatures by subtracting0.028 C for every millib
24、ar above1013mbar, or adding0.028 C for every millibar below1013mbar. NOTEThese corrections are valid only for pressures above933mbar. Appendix B Determination of acidity B.1 Principle A test portion is diluted with carbon dioxide-free water and titrated with standard volumetric sodium hydroxide solu
25、tion, using phenolphthalein as indicator. B.2 Reagents B.2.1 General. During the analysis, use only reagents of recognized analytical grade, only methylated spirits complying with BS3591, and only water complying with BS3978. B.2.2 Sodium hydroxide, standard volumetric solution, c(NaOH) = 0.100mol/L
26、. B.2.3 Phenolphthalein, 5g/L ethanolic solution. Dissolve0.5g of phenolphthalein in100mL of95% (V/V) ethanol, or95% (V/V) industrial methylated spirits, and add the sodium hydroxide solution(B.2.2) until a pale pink coloration is obtained. NOTEIt should be noted that the use of industrial methylate
27、d spirits is governed by The Methylated Spirits Regulations,1983 (S.I.1983No.252). It is not permissible to use duty-free ethanol, received under the provisions of The Alcoholic Liquor Duties Act1979, Section10, for purposes for which industrial methylated spirits is an acceptable alternative to eth
28、anol. B.3 Apparatus B.3.1 Ordinary laboratory apparatus B.3.2 Conical flask, of500mL capacity, of borosilicate glass, fitted with a ground glass stopper carrying a guard tube containing sodium hydroxide on an inert support (soda lime). B.3.3 Burette, of10mL capacity, graduated in0.02mL divisions, co
29、mplying with class A ofBS846. B.4 Procedure B.4.1 Test portion Take 1001mL of the sample, measured at20 C. B.4.2 Determination Place100mL of water and a few clean anti-bumping granules in the conical flask (B.3.2) and boil gently for5min to remove any carbon dioxide. Cool slightly and then add the t
30、est portion(B.4.1). Boil the mixture gently for a further5min. At the end of this period, insert the stopper and allow to cool to ambient temperature. Remove the stopper, add0.5mL of the phenolphthalein solution (B.2.3) and titrate with the sodium hydroxide solution(B.2.2), using the burette (B.3.3)
31、, until a pink coloration, persisting for about15s, is obtained. Stopper the flask and swirl its contents after each addition of sodium hydroxide solution. B.5 Expression of results The acidity A, expressed as a percentage by mass of acetic acid (CH 3 COOH), is given by the equation: where Appendix
32、C Determination of alcoholic impurities C.1 Principle Any alcoholic impurities are acetylated by reaction with acetyl chloride. The amount of acetyl chloride that has reacted is determined by titration with standard volumetric sodium hydroxide solution, using 3,3-bis (4-hydroxy-1-naphthyl) phthalide
33、 (1-naphtholphthalein) as indicator, and the alcohol equivalent is calculated. V 1 is the volume of the sodium hydroxide solution used for the determination (inmL); is the density of the sample at 20 C (determined by the method described in BS 4522) (in g/mL); 0.006 is the mass of acetic acid corres
34、ponding to1.00mL of sodium hydroxide solution, c(NaOH) = 0.100 mol/L (in g). A 0.006 V 1 - =BS1940:1987 BSI 12-1999 3 C.2 Reagents C.2.1 General. During the analysis, use only reagents of recognized analytical grade, only methylated spirits complying with BS3591, and only water complying with BS3978
35、. C.2.2 Pyridine, dry. C.2.3 Acetylating reagent. To118mL of acetyl chloride, add sufficient dry toluene to give a total volume of1000mL. C.2.4 Sodium hydroxide, standard volumetric solution, c(NaOH) = 1.00mol/L. C.2.5 3,3-bis(4-hydroxy-1-naphthyl)phthalide indicator solution, 5g/L ethanolic solutio
36、n. Dissolve0.5g of 3,3-bis(4-hydroxy-1-naphthyl) phthalide in100mL of95% (V/V) ethanol or95%(V/V) industrial methylated spirits. NOTEIt should be noted that the use of industrial methylated spirits is governed by The Methylated Spirits Regulations,1983 (S.I.1983No.252). It is not permissible to use
37、duty-free ethanol, received under the provisions of The Alcoholic Liquor Duties Act1979, Section10, for purposes for which industrial methylated spirits is an acceptable alternative to ethanol. C.3 Apparatus C.3.1 Ordinary laboratory apparatus C.3.2 Two conical flasks, of250mL capacity, fitted with
38、ground glass stoppers. C.3.3 Pipette, of10mL capacity, complying with class B of BS1583, fitted with an automatic suction device. C.3.4 Water bath, capable of being maintained at60 1 C. C.4 Procedure C.4.1 Test portion Take25 0.1mL of the sample, measured at20 C. C.4.2 Determination Dry the two coni
39、cal flasks (C.3.2) and place10.0mL of the acetylating reagent (C.2.3) into each flask using the pipette (C.3.3). Add2mL of the pyridine(C.2.2) to each flask, immediately insert the stoppers tightly and mix the contents thoroughly without wetting the stoppers. To one flask add the test portion (C.4.1
40、), ensuring that all of it comes into contact with the acetylating reagent. Replace the stopper and mix the contents thoroughly without wetting the stopper. Place both flasks in the water bath (C.3.4), maintained at60 1 C, loosening the stoppers momentarily to release any pressure and then replacing
41、 them tightly. Keep the flasks in the water bath for20min, shaking them occasionally, then remove the flasks and cool them to ambient temperature. Add25mL of water and0.5mL of the indicator solution (C.2.5) to each flask and then titrate the contents of each flask in turn with the sodium hydroxide s
42、olution (C.2.4) until the appearance of a faint blue colour. C.5 Expression of results The alcohol content B, expressed as a percentage by mass of butanol (C 4 H 9 OH), is given by the equation: where V 1 is the volume of the sodium hydroxide solution used for the titration of the blank (in mL); V 2
43、 is the volume of the sodium hydroxide solution used for the titration of the test solution (in mL); is the density of the sample at 20 C (determined by the method described in BS4522) (in g/mL). B 0.296 V 1 V 2 () - =4 blankBS1940:1987 BSI 12-1999 Publications referred to BS 593, Laboratory thermom
44、eters. BS 846, Specification for burettes. BS 1583, One-mark pipettes. BS 2511, Methods for the determination of water (Karl Fischer method). BS 3591, Specification for industrial methylated spirits. BS 3978, Water for laboratory use. BS 4522, Method for the determination of density of liquids at20
45、C. BS 4524, Method for the determination of residue on evaporation on a water bath. BS 4591, Method for the determination of distillation characteristics. BS 5309, Methods for sampling chemical products. BS 5309-1, Introduction and general principles. BS 5309-3, Sampling of liquids. BS 5339, Method
46、of measurement of colour in Hazen units (platinum-cobalt scale) of liquid chemical products. ISO 2497, Methyl ethyl ketone for industrial use List of methods of test 3) . ISO 2501, Methyl ethyl ketone, isobutyl methyl ketone, and isoamyl ethyl ketone for industrial use Determination of alcoholic imp
47、urities Volumetric method 3) . ISO 2887, sec Butyl alcohol, methyl ethyl ketone, isobutyl methyl ketone, isoamyl ethyl ketone, diacetone alcohol, and hexylene glycol for industrial use Determination of acidity to phenolphthalein Volumetric method 3) . 3) Referred to in the foreword only.BS 1940:1987
48、 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions BritishStandards are
49、 updated by amendment or revision. Users of BritishStandards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this BritishStandard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel:02089969000. Fax:02089967400.
