BS 4835-1973 Methods of test for plasticizer esters《增塑剂酯类试验方法》.pdf

1、BRITISH STANDARD BS 4835:1973 Methods of test for Plasticizer esters UDC 66.063.726:543BS4835:1973 This British Standard, having been approved by the ChemicalsIndustry Standards Committee, was published underthe authority of the Executive Board on 30April1973 BSI 12-1999 The following BSI references

2、 relate to the work on this standard: Committee references CIC/4 andCIC/4/4 Draft for comment 70/3331 ISBN 0 580 07392 0 Co-operating organizations The Chemicals Industry Standards Committee, under whose supervision this British Standard was prepared, consists of representatives of the following Gov

3、ernment departments and scientific and industrial organizations: British Steel Industry Chemical Industries Association* Department of Health and Social Security Department of Trade and Industry Department of Trade and Industry Laboratory of the Government Chemist* Fertiliser Manufacturers Associati

4、on Limited Ministry of Agriculture, Fisheries and Food National Sulphuric Acid Association Royal Institute of Public Health and Hygiene Soap and Detergent Industry Association The Government department and industries organization marked with an asterisk in the list, together with the following, were

5、 directly represented on the committees entrusted with the preparation of this British Standard: British Plastics Federation Ministry of Defence, Army Department Ministry of Defence, Navy Department Oil and Colour Chemists Association Paintmakers Association of Great Britain Pharmaceutical Society o

6、f Great Britain Research Association of British Paint, Colour and Varnish Manufacturers Royal Institute of Chemistry Society of Chemical Industry Society of Motor Manufacturers and Traders Limited Amendments issued since publication Amd. No. Date of issue CommentsBS4835:1973 BSI 12-1999 i Contents P

7、age Co-operating organizations Inside front cover Foreword ii 1 Scope 1 2 Measurement of colour 1 3 Measurement of colour after heat treatment 1 4 Determination of water content 2 5 Determination of ash 2 6 Determination of acidity to phenolphthalein 2 7 Determination of ester content and saponifica

8、tion and ester values 3 8 Determination of viscosity 4 9 Determination of matter oxidizable by potassium dichromate 4 10 Determination of density at 20 C 5 11 Determination of crystallizing point 5 12 Determination of refractive index 6 13 Determination of flash point 6 Publications referred to Insi

9、de back coverBS4835:1973 ii BSI 12-1999 Foreword This standard forms one of a series of British Standards for solvents and allied products; its preparation was authorized by the Chemicals Industry Standards Committee in order to provide methods of test for plasticizer esters. In the drafting of thes

10、e methods account has been taken of methods adopted by the International Organization for Standardization (ISO), in the preparation of which the United Kingdom has been an active participant. This British Standard prescribes methods of test only and should not be used or quoted as a specification de

11、fining limits of purity. Reference to the standard should be made in a form of words indicating that the methods of test used conform to BS4835. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct app

12、lication. 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, pages i and ii, pages1 to 6, an inside back cover and a back cover. This standard has been updated (see copyright dat

13、e) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS4835:1973 BSI 12-1999 1 1 Scope This British Standard describes general methods of test applicable to organic ester type plasticizers containing only carbon, hydrogen and oxygen but

14、 excluding esters of phenols and esters of hydroxy-acids. NOTEThe titles of the British Standards referred to in this Standard are listed on the inside back cover. 2 Measurement of colour 2.1 Introduction This clause is technically identical with the draft of International Standard ISO2211, modified

15、 in accordance with the comments made by the United Kingdom during its development. 2.2 Apparatus. The following apparatus is required: 1) Two matched Nessler cylinders, 100ml capacity, complying with BS612. 2) One-mark volumetric flask, 500ml capacity, complying with BS1792. 3) One-mark volumetric

16、flasks, 250ml capacity, complying with BS1792. 2.3 Reagents. The reagents used shall be of a recognized analytical reagent quality, Water complying with BS3978 shall be used throughout. 1) Cobaltous chloride, hexahydrate. 2) Hydrochloric acid, concentrated36% (m/m) (11N). either 3) Chloroplatinic ac

17、id reagent. Dissolve250mg of platinum in a small quantity 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. or

18、4) Potassium chloroplatinate. 2.4 Preparation of 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 c

19、lear solution and, after cooling, pour into the500ml one-mark volumetric flask. Dilute with water to the mark. From this solution prepare a series of colour standards ranging from0 Hazen colour units upwards at intervals of10units. For each 10units pipette5.0ml of the solution into a250ml one-mark v

20、olumetric flask and dilute with water to the mark. These diluted solutions should always be freshly prepared 1) . 2.5 Procedure. Fill one of the Nessler cylinders to the mark with the sample, and the other with the selected colour standard. If the sample is a solid, make the measurement at a tempera

21、ture10 C above its melting point. Using a white background compare the colours viewing vertically. Repeat with other colour standards, if necessary, until the closest match is obtained. If the colour of the sample does not match that of any of the colour standards, report, if possible, an approximat

22、e value or give a description of the colour with an appropriate note. 3 Measurement of colour after heat treatment 3.1 Introduction. This clause is technically identical with the draft of International Standard ISO2524, modified in accordance with the comments made by the United Kingdom during its d

23、evelopment. 3.2 Apparatus. The following apparatus is required: 1) Boiling tube, 200mm 38mm, complying with BS3218. 2) Two thermometers, No. B210C/100 complying with BS593. 3) Oil bath with stirrer. A volume of about2 litres of oil in the oil bath is suitable for testing together three samples. 1) P

24、ermanent glass Hazen colour standards for use in the BDH Lovibond Nesslerizer are available from The Tintometer Ltd., Salisbury, Wilts.BS4835:1973 2 BSI 12-1999 3.3 Procedure. Transfer70ml of the sample (or, if the material is a solid, sufficient to form70ml when melted) to the boiling tube and clos

25、e this with a vented cork, covered with aluminium foil, carrying one of the thermometers. Adjust the position of the thermometer so that the top of the bulb is55mm below the surface of the sample. Support the tube in the oil bath, fitted with the other thermometer and already heated to180 2 C, at su

26、ch a depth that the surface of the sample is25mm below the surface of the oil. Note the time at the moment of immersion of the sample. Maintain the temperature of the bath thereafter at180 2 C. At the end of120 2min withdraw the tube containing the sample and allow it to cool in air to room temperat

27、ure. If the sample is normally solid at room temperature, cool it to a temperature10 C above its melting point. Measure the colour of the treated sample by the method described in Clause2, using equal volumes of the sample and colour standard in, for example,50ml Nessler cylinders. 4 Determination o

28、f water content Determine the water content by one of the general methods described in BS2511, using20g of the sample. 5 Determination of ash 5.1 Introduction. This clause is technically identical with the draft of International Standard ISO2526, modified in accordance with the comments made by the

29、United Kingdom during its development. 5.2 Apparatus. Ordinary laboratory apparatus and a furnace, capable of control at600 30 C, is required. 5.3 Procedure. Weigh, to the nearest 1g, about50g of the sample and then slowly burn it, a little at a time, in a weighed platinum or silica basin, previousl

30、y heated to600 30 C, cooled in a desiccator and weighed to the nearest0.1mg. Gently heat in a furnace at600 30 C until all carbonaceous matter has disappeared. Cool in a desiccator and weigh to the nearest0.1mg. 5.4 Calculation. Ash, expressed as a percentage by mass = where M 1= mass, in grams, of

31、the residue; andM 2= mass, in grams, of the test portion. 6 Determination of acidity to phenolphthalein 6.1 Introduction. This clause is technically identical with the draft of International Standard ISO2525, modified in accordance with the comments made by the United Kingdom during its development.

32、 6.2 Reagents. The reagents used shall be of a recognized analytical reagent quality. Water complying with BS3978 shall be used throughout. 1) Sodium hydroxide, 0.1N standard volumetric solution. 2) Ethanol 2) ,95% (v/v). 3) Phenolphthalein indicator solution, 10g/l, prepared as described in BS4123.

33、 6.3 Procedure. Weigh, to the nearest 0.5g, about50g of the sample and mix with50ml of the ethanol previously neutralized to phenolphthalein. Titrate the mixture with the sodium hydroxide solution, using0.5ml of the phenolphthalein indicator solution until the pink colour remains for5s. 6.4 Calculat

34、ion. Acidity, calculated as a percentage by mass of the acid of relative molar mass 3)m Aand basicity n A 2) Ethanol may be replaced by industrial methylated spirits, 66 degrees OP, complying with BS3591. It should be noted that the use of industrial methylated spirits is governed by The Methylated

35、Spirits Regulations (S.I. 1952, No. 2230). 3) Hitherto known as molecular weight. 100 M 1 M 2 -BS4835:1973 BSI 12-1999 3 or calculated as milliequivalents per kilogram 7 Determination of ester content and saponification and ester values 7.1 Introduction. This clause is technically identical with the

36、 draft of International Standard ISO2527, modified in accordance with the comments made by the United Kingdom during its development. 7.2 Reagents. The reagents used shall be of a recognized analytical reagent quality. Water complying with BS3978 shall be used throughout. 1) Potassium hydroxide, app

37、roximately N reagent solution in95% (v/v) ethanol 4) . 2) Hydrochloric acid, N standard volumetric solution. 3) Phenolphthalein indicator solution, 10g/l, prepared as described in BS4123. 7.3 Procedure. Using the same pipette, introduce50.0ml of the potassium hydroxide solution into each of two dry2

38、50ml conical flasks with ground glass joints. Immediately add5ml of water to each flask. Close the flasks with their glass stoppers. Transfer into one of the flasks the mass of sample given by the following formula, weighing to the nearest milligram; and using a weighing pipette if the sample is liq

39、uid: The table below gives the mass of sample to be taken of a number of esters. Attach the flasks to water-cooled reflux condensers fitted with ground glass joints and heat for1h in a boiling water bath. Withdraw the flasks, still carrying their condensers, and immerse them in cold running water. W

40、hen cool, wash down the inside of each condenser with two20ml portions of water. Disconnect the flasks and wash each joint with a further20ml of water. Add0.5ml of the phenolphthalein indicator solution and titrate the mixture immediately with the hydrochloric acid solution until the pink colour is

41、just discharged. where V 1 = volume, in millilitres, of 0.1N sodium hydroxide solution used; M 3 = mass, in grams, of the test portion. 4) Ethanol may be replaced by industrial methylated spirits, 66degreesOP, complying with BS3591. It should be noted that the use of industrial methylated spirits is

42、 governed by The Methylated Spirits Regulations (S.I. 1952, No. 2230). 0.2 g where m E = relative molar mass of the sample and n E = number of ester groups in the molecule. Relative molar mass Mass of sample Relative molar mass Mass of sample g g Dimethyl phthalate 194 2.4 0.2 Ditridecyl phthalates

43、531 6.6 0.2 Diethyl phthalate 222 2.8 0.2 Dibutyl adipates 254 3.2 0.2 Dibutyl phthalates 278 3.5 0.2 Dioctyl adipates 371 4.6 0.2 Dimethoxyethyl phthalate 280 3.5 0.2 Diononyl adipates 399 5.0 0.2 Benzyl Butyl phthalates 312 3.9 0.2 Didecyl adipates 427 5.3 0.2 Diheptyl phthalates 362 4.5 0.2 Diund

44、ecyl adipates 455 5.7 0.2 Dibutoxyethyl phthalates 366 4.6 0.2 Didodecyl adipates 483 6.0 0.2 Dioctyl phthalates 390 4.9 0.2 Ditridecyl adipates 511 6.4 0.2 Dinonyl phthalates 418 5.2 0.2 Dibutyl sebacates 314 3.9 0.2 Didecyl phthalates 447 5.6 0.2 Dioctyl sebacates 426 5.4 0.2 Dioctyl azelates 412

45、5.3 0.2 100V 1 M 3 - = B = 0.025m E n -BS4835:1973 4 BSI 12-1999 7.4 Calculation 7.4.1 Ester content. The ester content, expressed as a percentage by mass of the ester concerned 7.4.2 Saponification and ester values. Especially in the case of mixed alcohol esters, for which the relative molecular ma

46、ss can only, at best, be estimated, saponification or ester values are used to express the result. 7.4.2.1 Saponification value. Saponification value, expressed as milligrams of potassium hydroxide per gram NOTE56.10 is the relative molar mass of potassium hydroxide. 7.4.2.2 Ester value. Ester value

47、 expressed as milligrams of potassium hydroxide per gram NOTEThe ester content, as a percentage by mass of the ester concerned, may be estimated from the ester value by multiplication by the factor: 8 Determination of viscosity Determine the viscosity at a temperature of20 0.1 C by one of the metho

48、ds described in BS188. 9 Determination of matter oxidizable by potassium dichromate 9.1 Reagents. The reagents used shall be of recognized analytical reagent quality. Water complying with BS3978 shall be used throughout. 9.1.1 Oxidizing solution. Dissolve approximately1g of potassium dichromate in10

49、0ml of water. Then cautiously add150ml of concentrated nitric acid,70% (m/m) (16N). Cool the flask during the addition of the nitric acid. Store the solution in a dark-coloured bottle. 9.1.2 Potassium iodide, 50g/l solution. Dissolve50g of potassium iodide in1litre of water. 9.1.3 Sodium thiosulphate, 0.1N standard volumetric solution. 9.1.4 Cyclohexane. Wash1 litre of cyclohexane with three100ml portions of water. 9.1.5 Starch indicator soluti