1、BRITISH STANDARD BS 5598-6: 1979 ISO 3363:1976 Methods of sampling and test for halogenated hydrocarbons Part 6: Determination of acidity of fluorochlorinated hydrocarbons ISO title: Fluorochlorinated hydrocarbons for industrial use Determination of acidityTitrimetric method UDC 661.723:547.411:543.
2、062:543.241.5BS5598-6:1979 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Executive Board and cameinto effect on 31January1979 BSI 11-1999 The following BSI references relate to the work on this standard: C
3、ommittee reference CIC/4 Draft for comment 74/53096 ISBN 0 580 10711 6 Cooperating organizations The Chemicals Standards Committee, under whose direction this BritishStandard was prepared, consists of representatives from the following Government departments and scientific and industrial organizatio
4、ns: Association of Fatty Acid Distillers British Tar Industry Association Chemical Industries Association* Chemical Society, Analytical Division Department of Health and Social Security Department of Industry: Laboratory of the Government Chemist Fertiliser Manufacturers Association Ltd. Hydrocarbon
5、 Solvents Association Ministry of Agriculture, Fisheries and Food Ministry of Defence* National Sulphuric Acid Association Paintmakers Association of Great Britain Ltd. Royal Institute of Public Health and Hygiene Soap and Detergent Industry Association Standardization of Tar Products Tests Committe
6、e The organizations marked with an 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 Fabric Car Research Association Fire Extinguishing Trades Association Institute
7、of Metal Finishing Institute of Refrigeration Oil and Colour Chemists Association Pharmaceutical Society of Great Britain Royal Institute of Chemistry Society of Chemical Industry Individual companies Amendments issued since publication Amd. No. Date of issue CommentsBS5598-6:1979 BSI 11-1999 i Cont
8、ents Page Cooperating organizations Inside front cover National foreword ii 1 Scope and field of application 1 2 References 1 3 Principle 1 4 Sampling 1 5 Reagents 1 6 Apparatus 1 7 Procedure 1 8 Expression of results 2 9 Test report 2 Annex Other ISO publications relating to halogenated hydrocarbon
9、s for industrial use 4 Figure Apparatus for absorption of acidity for products gaseous at ordinary temperatures 3 Publications referred to Inside back coverBS5598-6:1979 ii BSI 11-1999 National foreword This British Standard has been prepared under the direction of the Chemicals Standards Committee
10、in order to provide methods of sampling and test for halogenated hydrocarbons. For some years the UnitedKingdom has participated in the work of preparing methods of sampling and test applicable to halogenated hydrocarbons for industrial use, organized by Sub-committee12, Halogenated hydrocarbons and
11、 amines, of Technical Committee47, Chemistry, of the International Organization for Standardization (ISO). As international agreement is reached on the methods, it is proposed to publish them as Parts of this British Standard as follows: Part 1: Sampling liquid products, identical with ISO2209; Part
12、 2: Sampling of liquefied gases, identical with ISO3427; Part 3: Determination of residue on evaporation, identical with ISO2210; Part 4: Determination of acidityTitrimetric method, identical with ISO1393; Part 5: Determination of cloud point, identical with ISO1394; Part 6: Determination of acidity
13、 of fluorochlorinated hydrocarbons, identical with ISO3363; Part 7: Methods of test for methyl chloride and ethyl chloride, identical with ISO5781 1) ; Part 8: Determination of non-volatile residue in fluorinated hydrocarbons, identical with ISO5789 1) . This Part is identical with ISO3363 “Fluoroch
14、lorinated hydrocarbons for industrial useDetermination of acidityTitrimetric method”. Terminology and conventions. The text of the International Standard has been approved as suitable for publication, without deviation, as a British Standard. Some terminology and certain conventions are not identica
15、l with those used in British Standards; attention is especially drawn to the following. The comma has been used throughout as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. Where the words “International Standard” appear, refe
16、rring to this standard, they should be interpreted as “British Standard”. 1) In course of preparation. Cross references International Standard Corresponding British Standard ISO/R 1393 a BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 4:1979 Determination of acidity (Identical
17、) ISO 2209:1973 BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 1:1978 Sampling of liquid products (Identical) ISO 3427:1976 BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 2:1979 Sampling of liquefied gases (Identical) a ISO/R1393 has been superseded by
18、 ISO1393:1977.BS5598-6:1979 BSI 11-1999 iii Additional information WARNING NOTE. Care should be taken to avoid breathing the vapour of halogenated hydrocarbons. All operations likely to produce an appreciable concentration in the atmosphere should be conducted under a hood with an adequate exhaust.
19、This standard specifies a method of test only and should not be referred to as a specification defining limits of purity. Reference to the standard should be in the form of words indicating that the method of test used conforms to the requirements of BS5598-6. A British Standard does not purport to
20、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 immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, p
21、ages i to iv, 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 amendment table on the inside front cover.iv blankBS5598-6:1979 BSI 11-1999 1 1 Scope and field of application T
22、his International Standard specifies a titrimetric method for the determination of the acidity of fluorochlorinated hydrocarbons for industrial use. The method is applicable to products of which the acidity is in the range2 to2004mol of univalent acid per kilogram. Two procedures are given; one appl
23、icable to products that are liquid at ordinary temperatures (R11, R113, etc.), and the other to products that are gaseous at ordinary temperatures (R12, R22, R114etc.). 2 References ISO/R 1393, Liquid halogenated hydrocarbons for industrial useDetermination of acidity. ISO 2209, Liquid halogenated h
24、ydrocarbons for industrial useSampling. ISO 3427, Gaseous halogenated hydrocarbons (liquefied gases)Taking of sample. 3 Principle Extraction of the acidity in the fluorochlorinated hydrocarbon by water. Titration of the acidity of the aqueous phase with a standard volumetric sodium hydroxide solutio
25、n in the presence of bromocresol green as indicator. 4 Sampling The laboratory sample of liquid products shall be collected by the method specified in ISO2209. The laboratory sample of products which are gaseous at ordinary temperatures shall be collected as a liquefied gas in a stainless steel samp
26、le cylinder by the method specified in ISO3427. 5 Reagents During the analysis use only reagents of recognized analytical grade. 5.1 Distilled water, neutral to bromocresol green. Add to distilled water, or water of equivalent purity, contained in a conical flask with a ground glass stopper,1% (V/V)
27、 of the bromocresol green solution(5.3) and neutralize with the sodium hydroxide solution (5.2) until the colour changes to clear blue. 5.2 Sodium hydroxide, 0,01N standard volumetric solution. Standardize this solution with0,01N standard volumetric hydrochloric acid solution under the conditions of
28、 the determination. 5.3 Bromocresol green, 1g/l solution in95% (V/V) ethanol. 6 Apparatus Ordinary laboratory apparatus and 6.1 For products gaseous at ordinary temperatures See the Figure for the arrangement of apparatus. 6.1.1 Needle valve, of any convenient type, with screw-thread union for conne
29、ction to the sample cylinder. 6.1.2 Bubble indicator, of glass, capacity about15ml. NOTEThe bubble indicator is used empty to check complete vaporization of the test portion. 6.1.3 Three tail-form Drechsel-type gas washing bottles, of capacity100ml, fitted with sintered glass disks. 6.2 For both liq
30、uid and gaseous products 6.2.1 Microburette, of capacity2ml, graduated in0,01ml. 7 Procedure 7.1 Liquid products Use the method specified in ISO/R1393 with the following modifications appropriate for the products concerned: 7.1.1 Test portion Weigh, to the nearest0,1g, about100g of the laboratory sa
31、mple. 7.1.2 Determination In the case of R11 (boiling point24 C), carry out the extraction with the water (5.1) previously cooled to15 C. For all products, transfer the whole of the aqueous phase to a250ml conical flask and titrate. 7.2 Gaseous products Weigh, to the nearest1g, the capped sample cyl
32、inder containing the laboratory sample, remove the cap and connect the needle valve (6.1.1) to the valve of inverted cylinder type (b) (ISO3427), or to valve A of cylinder type (a) (ISO3427) (seetheFigure). Add50ml of the water (5.1) to each of the three gas washing bottles (6.1.3). Connect the outl
33、et of the needle valve to the bubble indicator(6.1.2), connected in turn to the gas washing bottles connected in series as shown in theFigure. Open the sample cylinder valve fully and open the needle valve to the extent required to give a steady vaporization rate of about100g of sample per hour. NOT
34、E 1The required setting is judged by experience and observation of the bubble rate through the gas washing bottles.BS5598-6:1979 2 BSI 11-1999 NOTE 2It may be necessary to warm the bubble indicator and cylinder valves by means of a warm air blower when analysing higher boiling products such as R114.
35、 After about1h, close first the cylinder valve and then the needle valve. Disconnect the needle valve and replace the cylinder cap. Allow the cylinder to warm up to room temperature, dry it if necessary, and reweigh it, to the nearest1g, under the same conditions as previously. Mix the contents of t
36、he first two gas washing bottles; if the sample is acid, the solution will be coloured yellow. Titrate the acidity (if any) with the standard volumetric sodium hydroxide solution(5.2), using the microburette (6.2.1), until the appearance of a clear blue colour. The water in the third gas washing bot
37、tle should remain blue. If this is not the case, repeat the test. 8 Expression of results 8.1 The acidity, expressed in micromoles of univalent acid per kilogram, is given by the formula: where 8.2 The acidity, expressed in milligrams of hydrogen chloride (HCl) per kilogram, is given by the formula:
38、 where V and m have the same meaning as in8.1. 8.3 The acid number, expressed in milligrams of potassium hydroxide (KOH) per gram, is given by the formula: where V and m have the same meaning as in8.1. 8.4 Express the result with a precision corresponding to the accuracy of weighing and titration. N
39、OTEIf the concentration of the standard volumetric solution used is not exactly as specified in the list of reagents, an appropriate correction should be made. 9 Test report The test report shall include the following particulars: a) the reference of the method used; b) the results and the method of
40、 expression used; c) any unusual features noted during the determination; d) any operation not included in this International Standard or in the InternationalStandards to which reference is made, or regarded as optional. V is the volume, in millilitres, of the standard volumetric sodium hydroxide so
41、lution (5.2) used for the titration; m is the mass, in grams, of the test portion (equal to the change in mass of the sample cylinder in the case of gaseous products). V 0,01 1 000 1 000 m - 10 000V m - = V 365 m - 56,1V 0,01 m - 0561 , V m - =BS5598-6:1979 BSI 11-1999 3 Figure Apparatus for absorpt
42、ion of acidity for products gaseous at ordinary temperaturesBS5598-6:1979 4 BSI 11-1999 Annex Other ISO publications relating to halogenated hydrocarbons for industrial use ISO/R 1393, Determination of acidity liquids. ISO/R 1394, Determination of cloud point liquids. ISO 2209, Sampling liquids. ISO
43、 2210, Determination of residue on evaporation liquids. ISO 3427, Taking of a sample liquefied gases.BS5598-6:1979 BSI 11-1999 Publications referred to See national forewordBS 5598-6: 1979 ISO 3363:1976 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent na
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