BS 509-2-1984 Acetone for industrial use - Methods of test《工业用丙酮 第2部分 试验方法》.pdf

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1、BRITISH STANDARD BS 509-2:1984 Incorporating Amendment No.1 Acetone for industrial use Part 2: Methods of test UDC661.727.4:543.062BS509-2:1984 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Board of BSI an

2、d comes intoeffect on 31 May1984 BSI09-1999 The following BSI references relate to the work on this standard: Committee reference CIC/4 Draft for comment81/50138 DC ISBN 0 580 13882 8 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Chemi

3、cals Standards Committee (CIC/-) to Technical Committee CIC/4 upon which the following bodies were represented: Chemical Industries Association Ministry of Defence Oil and Colour Chemists Association Royal Society of Chemistry Society of Chemical Industry The following bodies were also represented i

4、n the drafting of the standard, through subcommittees and panels: British Pharmacopoeia Commission British Society of Perfumers Cosmetic, Toiletry and Perfumery Association Limited Department of Trade and Industry (Laboratory of the Government Chemist) Amendments issued since publication Amd. No. Da

5、te of issue Comments 5446 January1987 Indicated by a sideline in the marginBS509-2:1984 BSI 09-1999 i Contents Page Committees responsible Inside front cover Foreword ii 1 Scope 1 2 Sampling 1 3 Determination of distillation characteristics 1 4 Determination of water content 1 5 Determination of den

6、sity at20 C 1 6 Determination of dry residue after evaporation on a water bath 1 7 Determination of acidity to phenolphthalein 1 8 Test for miscibility with water 2 9 Determination of permanganate time 2 10 Control test with Agulhons reagent 3 11 Measurement of colour 3 12 Test reports 3 13 Detectio

7、n of alkalinity 3 Table 1 Methods of test for acetone: relationship between BritishStandardand international series 4 Publications referred to Inside back coverBS509-2:1984 ii BSI 09-1999 Foreword This Part of this British Standard has been prepared under the direction of the Chemicals Standards Com

8、mittee and provides a comprehensive series of test methods for acetone for industrial use. Although applicable to the material in general, it includes all the test methods required to assess compliance with BS509-1. In preparing this standard, the opportunity has been taken to implement, without tec

9、hnical alteration, the International Standards describing test methods for acetone. These have been prepared, with the active participation of the UK, by Technical Committee47, Chemistry, of the International Organization for Standardization (ISO), as separate Parts of ISO757 and constitute the revi

10、sion of ISO Recommendation R757. Table 1 gives the relationship between International Standards and this British Standard, together with the relationship between general test methods and corresponding International Standards. Subsequent International Standards in the ISO757 series, if approved by th

11、e UK, will be published as additions to this British Standard, without technical alteration. This Part of this standard specifies methods of test only and should not be used as a specification defining limits of purity. Reference to this Part of this standard should indicate that the methods of test

12、 used are in accordance with the appropriate clause(s) of BS509-2. 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 of itself confer immunit

13、y from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, pages1to4, 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 amendme

14、nt table on the inside front cover.BS509-2:1984 BSI 09-1999 1 1 Scope This Part of BS509 describes methods for testing acetone for industrial use. NOTEThe titles of the publications referred to in this standard are listed on the inside back cover. 2 Sampling 1) Store the laboratory sample in a clean

15、, dry and airtight, ground glass stoppered bottle, or a screw-capped bottle fitted with a polyethylene cone insert, of such capacity that it is almost filled by the sample. Sufficient ullage should be left in the bottle to avoid excessive pressure changes that could arise from temperature variations

16、 during storage and handling. About10%ullage is recommended. If it is necessary to seal the bottle, take care to avoid any risk of contamination of the contents. Store the sample in a cool place in the dark. 3 Determination of distillation characteristics Determine the distillation characteristics b

17、y the method described in BS4591:1971, except that the following thermometer and temperature corrections should be used. a) Thermometer (3.2 of BS4591:1971). Use a thermometer No. F75C/1000 complying with the requirements of BS593. b) Corrections to be applied to observed temperatures (7.2 of BS4591

18、:1971). If the corrected barometric pressure deviates from1013 mbar 2)apply a correction to the observed temperature by subtracting0.029 C for every millibar above, or adding0.029 C for every millibar below,1013mbar. 4 Determination of water content Determine the water content using the method descr

19、ibed in clause4 of BS2511:1970, using as test portions (see4.4.3 of BS2511:1970)20mL of the material mixed with100mL of dry pyridine. 5 Determination of density at20 C Determine the density at20 C by the method described in BS4522. 6 Determination of dry residue after evaporation on a water bath Det

20、ermine the dry residue after evaporation by the method described in BS4524. 7 Determination of acidity to phenolphthalein 7.1 Field of application. This method is applicable to products having acidities, expressed as acetic acid (CH 3COOH), equal to or greater than0.0006%(m/m). 7.2 Principle. Diluti

21、on of a test portion with carbon dioxide-free water. Titration of the test solution, if acid, with standard volumetric sodium hydroxide solution, using phenolphthalein as indicator. 7.3 Reagents 7.3.1 General. During the analysis, use only reagents of recognized analytical grade and only water compl

22、ying with BS3978. 7.3.2 Water, carbon dioxide-free. Boil distilled water and allow it to cool in a flask fitted with a stopper carrying a soda-lime guard tube. 7.3.3 Sodium hydroxide, standard volumetric solution, c (NaOH)=0.1mol/L. 7.3.4 Phenolphthalein, 5g/L ethanolic solution. Dissolve0.5g of phe

23、nolphthalein in100mL of95%(V/V) ethanol and add the sodium hydroxide solution(7.3.3) until a pale pink coloration is obtained. NOTEThe ethanol may be replaced for this purpose by industrial methylated spirits,95%(V/V) complying with BS3591. It should be noted that the use of industrial methylated sp

24、irits is governed by The Methylated Spirits Regulations,1983 (S.I.1983 No.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 ethano

25、l. 7.4 Apparatus 7.4.1 Ordinary laboratory apparatus 7.4.2 Conical flask, of capacity250mL, of borosilicate glass, fitted with a ground glass stopper carrying a soda-lime guard tube. 7.4.3 Burette, of capacity10mL, graduated in0.02mL divisions. 7.5 Procedure 7.5.1 Test portion. Take100 0.1mL of the

26、laboratory sample. 7.5.2 Determination. Place80mL of the water(7.3.2) in the conical flask(7.4.2), add0.5mL of the phenolphthalein solution(7.3.4) and make faintly pink by the addition of a few drops of the sodium hydroxide solution(7.3.3). 1) Additional guidance is given in BS5309-1 and BS5309-3. 2

27、) 1 mbar=100N/m 2 =100Pa.BS509-2:1984 2 BSI 09-1999 Add the test portion(7.5.1) and a further0.5mL of the phenolphthalein solution(7.3.4). If the solution is acid (colourless), titrate it with the sodium hydroxide solution(7.3.3), stoppering the flask and swirling its contents after each addition, u

28、ntil a pink coloration, persisting for about15s, is obtained. 7.6 Expression of results. The acidity, expressed as acetic acid (CH 3COOH), in%(m/m), is given by the formula NOTEIf the concentration of the standard volumetric solution used is not exactly as specified in the list of reagents, an appro

29、priate correction should be made. 8 Test for miscibility with water 8.1 Principle. Addition of water to a test portion, under specified conditions, and examination for opalescence or turbidity. 8.2 Reagents. During the test, use only water complying with BS3978. 8.3 Apparatus 8.3.1 Ordinary laborato

30、ry apparatus 8.3.2 Two matched Nessler cylinders, of capacity100mL, similar in every respect. 8.4 Procedure 8.4.1 Test portion. Take, by means of a safety pipette,5mL of the laboratory sample at a temperature of about20 C and transfer to one of the Nessler cylinders(8.3.2). 8.4.2 Test. Add slowly, w

31、ith thorough mixing,95mL of water to the test portion(8.4.1) in the Nessler cylinder. Examine for opalescence during the addition. Adjust the temperature of the mixture to20 C. Examine vertically for opalescence or turbidity against a black background with side illumination, using as a standard the

32、second cylinder containing100mL of water. 8.5 Expression of results. Report the formation of opalescence or turbidity or whether the solution remained clear. 9 Determination of permanganate time 9.1 Definition For the purposes of this clause of BS509-2, the following definition applies. 9.1.1 perman

33、ganate time the number of minutes required, after adding2mL of0.2g/L potassium permanganate solution to50mL of the sample, for the colour to match that of a colour standard 9.2 Principle. Addition to a test portion, under specified conditions, of potassium permanganate solution. Determination of the

34、 time taken for the colour of this test solution to match that of a cobalt(II) chloride and uranyl nitrate colour standard. 9.3 Reagents 9.3.1 General. During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only water complying with BS3978. 9.3.2 Potassium

35、 permanganate, 0.2g/L solution. Use water previously boiled for30min with sufficient dilute potassium permanganate solution to give a stable faint pink coloration. Cool the water to ambient temperature before preparation of the solution. Prepare this solution immediately before use and protect it fr

36、om light. 9.3.3 Cobalt(II) chloride and uranyl nitrate, colour standard. To5mL of a50g/L solution of cobalt(II) chloride hexahydrate (CoCl 2 .6H 2 O), add7mL of a40g/L solution of uranyl nitrate hexahydrate UO 2(NO 3 ) 2 .6H 2 O, and dilute with water to50mL. Prepare this solution on the day of use.

37、 9.4 Apparatus NOTEClean the glassware used so as to avoid any risk of contamination. 9.4.1 Ordinary laboratory apparatus 9.4.2 Water bath, capable of being controlled at25 0.2 C. 9.4.3 Two matched cylinders, of capacity100mL, of colourless transparent glass, graduated at50mL and fitted with ground

38、glass stoppers. 9.4.3 Pipette, of capacity2mL. where V 1 is the volume, in mL, of the sodium hydroxide solution(7.3.3) used for the determination; is the density, in g/mL, of the sample at20 C (determined by method described in BS4522); 0.006 is the mass, in g, of acetic acid corresponding to1.00mL

39、of sodium hydroxide solution, c (NaOH)=0.100mol/L. 0.006 V 1 -BS509-2:1984 BSI 09-1999 3 0.1 Procedure 0.1.1 Test portion. Carry out the test as soon as possible after receipt of the sample. Rinse one of the cylinders(9.4.3), first with15mL to20mL of hydrochloric acid, of density approximately1.19g/

40、mL, about38%(m/m) solution, then six times with tap water, twice with distilled water and finally with some of the laboratory sample. Immediately fill the cylinder to the mark with more of the laboratory sample at a temperature of about25 C. 0.1.2 Determination. Rinse the second cylinder(9.4.2) as s

41、pecified in0.1.1 but omitting the last rinse with the laboratory sample. Fill the cylinder to the mark with the colour standard solution(9.3.3). Place the cylinder containing the test portion(0.1.1) in the water bath(9.4.2), controlled at25 0.2 C, so that the water level in the bath is approximately

42、25mm below the neck of the cylinder. After15min, remove the cylinder from the water bath and, using the pipette(9.4.4), add2.0mL of the potassium permanganate solution(9.3.2). Note the time. Immediately stopper the cylinder, shake, and replace in the water bath. Remove the cylinder from the water ba

43、th, from time to time, and compare the colour, viewing vertically downwards against a white background, with the colour standard. Towards the end of the determination, compare the colour at intervals of1min. Avoid exposing the test solution to strong daylight. Note the time when the colour of the te

44、st solution matches that of the colour standard. 0.2 Expression of results. Report the time, in minutes, from the addition of the potassium permanganate solution, for the colour of the test solution to match that of the colour standard. 1 Control test with Agulhons reagent 1.1 Principle. Treatment o

45、f a test portion with Agulhons reagent under specified conditions. The presence of certain impurities, in particular alcoholic ones, is indicated by a blue or violet coloration. 1.2 Reagents 1.2.1 General. During the test, use only reagents of recognized analytical grade and water complying with BS3

46、978. 1.2.2 Agulhons reagent. Dissolve0.50g of potassium dichromate in30mL of water and add about65mL of nitric acid solution, of density approximately1.40g/mL. Cool the solution to about20 C and dilute to100mL with more of the nitric acid solution. 1.3 Apparatus 1.3.1 Ordinary laboratory apparatus 1

47、.4 Procedure 1.4.1 Test portion. Take by means of a safety pipette,1mL of the laboratory sample. 1.4.2 Test. Place the test portion(1.4.1) in a test tube and add3mL of the Agulhons reagent(1.2.2). Mix and allow the solution to stand at approximately15 C for5min. After this period, examine the colour

48、 of the solution. 1.5 Expression of results. If no blue or violet colour appears, report the absence of alcoholic impurities. 2 Measurement of colour Determine the colour by the method described in BS5339. 3 Test reports The test report, for each determination, should contain the following informati

49、on: a) an identification of the sample; b) the reference to the method used; c) the results, and the method of expression used; d) any unusual features noted during the determination; e) any operation not included in the appropriate clause of this standard or in the British Standards to which reference is made, or regarded as optional. 4 Detection of alkalinity 4.1 Principle. Neutralization of water using bromothymol blue as indicator and the transfer of equal volumes to each of two glass cylinders. Mixing of a test portion with