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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 acidity Titrimetric method UDC 661.723:547.411:543
2、.062:543.241.5 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 This British Standard, having been prepared under the direction of the Chemicals Standards Committee, was published under the authority of the Executive Board and
3、came into effect on 31 January 1979 BSI 11-1999 The following BSI references relate to the work on this standard: Committee reference CIC/4 Draft for comment 74/53096 ISBN 0 580 10711 6 Cooperating organizations The Chemicals Standards Committee, under whose direction this British Standard was prepa
4、red, consists of representatives from the following Government departments and scientific and industrial organizations: Association of Fatty Acid Distillers British Tar Industry Association Chemical Industries Association* Chemical Society, Analytical Division Department of Health and Social Securit
5、y Department of Industry: Laboratory of the Government Chemist Fertiliser Manufacturers Association Ltd. Hydrocarbon Solvents Association Ministry of Agriculture, Fisheries and Food Ministry of Defence* National Sulphuric Acid Association Paintmakers Association of Great Britain Ltd. Royal Institute
6、 of Public Health and Hygiene Soap and Detergent Industry Association Standardization of Tar Products Tests Committee 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 St
7、andard: British Plastics Federation Fabric Car Research Association Fire Extinguishing Trades Association Institute of Metal Finishing Institute of Refrigeration Oil and Colour Chemists Association Pharmaceutical Society of Great Britain Royal Institute of Chemistry Society of Chemical Industry Indi
8、vidual companies Amendments issued since publication Amd. No.Date of issueComments Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 BSI 11-1999i Contents Page Cooperating organizationsInside front cover National forewordii 1Sco
9、pe and field of application1 2References1 3Principle1 4Sampling1 5Reagents1 6Apparatus1 7Procedure1 8Expression of results2 9Test report2 Annex Other ISO publications relating to halogenated hydrocarbons for industrial use4 Figure Apparatus for absorption of acidity for products gaseous at ordinary
10、temperatures3 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 ii BSI 11-1999 National foreword This British Standard has been prepared under the direction of the Chemicals Standards Co
11、mmittee in order to provide methods of sampling and test for halogenated hydrocarbons. For some years the United Kingdom has participated in the work of preparing methods of sampling and test applicable to halogenated hydrocarbons for industrial use, organized by Sub-committee 12, Halogenated hydroc
12、arbons and amines, of Technical Committee 47, 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 IS
13、O 2209; Part 2: Sampling of liquefied gases, identical with ISO 3427; Part 3: Determination of residue on evaporation, identical with ISO 2210; Part 4: Determination of acidity Titrimetric method, identical with ISO 1393; Part 5: Determination of cloud point, identical with ISO 1394; Part 6: Determi
14、nation of acidity of fluorochlorinated hydrocarbons, identical with ISO 3363; Part 7: Methods of test for methyl chloride and ethyl chloride, identical with ISO 57811); Part 8: Determination of non-volatile residue in fluorinated hydrocarbons, identical with ISO 57891). This Part is identical with I
15、SO 3363 “Fluorochlorinated hydrocarbons for industrial use Determination of acidity Titrimetric 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 conventio
16、ns are not identical 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 Sta
17、ndard” appear, referring to this standard, they should be interpreted as “British Standard”. 1) In course of preparation. Cross references International StandardCorresponding British Standard ISO/R 1393aBS 5598 Methods of sampling and test for halogenated hydrocarbons Part 4:1979 Determination of ac
18、idity (Identical) ISO 2209:1973BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 1:1978 Sampling of liquid products (Identical) ISO 3427:1976BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 2:1979 Sampling of liquefied gases (Identical) a ISO/R 1393 has bee
19、n superseded by ISO 1393:1977. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 BSI 11-1999iii Additional information WARNING NOTE. Care should be taken to avoid breathing the vapour of halogenated hydrocarbons. All operations
20、likely to produce an appreciable concentration in the atmosphere should be conducted under a hood with an adequate exhaust. 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 wor
21、ds indicating that the method of test used conforms to the requirements of BS 5598-6. 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 it
22、self confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, 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 be i
23、ndicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 BSI
24、 11-19991 1 Scope and field of application This 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 range 2 to 200 4mol of univalent acid p
25、er kilogram. Two procedures are given; one applicable to products that are liquid at ordinary temperatures (R 11, R 113, etc.), and the other to products that are gaseous at ordinary temperatures (R 12, R 22, R 114 etc.). 2 References ISO/R 1393, Liquid halogenated hydrocarbons for industrial use De
26、termination of acidity. ISO 2209, Liquid halogenated hydrocarbons for industrial use Sampling. 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 p
27、hase with a standard volumetric sodium hydroxide solution in the presence of bromocresol green as indicator. 4 Sampling The laboratory sample of liquid products shall be collected by the method specified in ISO 2209. The laboratory sample of products which are gaseous at ordinary temperatures shall
28、be collected as a liquefied gas in a stainless steel sample cylinder by the method specified in ISO 3427. 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, contain
29、ed in a conical flask with a ground glass stopper, 1 % (V/V) 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, 0,01 N standard volumetric solution. Standardize this solution with 0,01 N standa
30、rd volumetric hydrochloric acid solution under the conditions of the determination. 5.3 Bromocresol green, 1 g/l solution in 95 % (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 Need
31、le valve, of any convenient type, with screw-thread union for connection to the sample cylinder. 6.1.2 Bubble indicator, of glass, capacity about 15 ml. 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,
32、 of capacity 100 ml, fitted with sintered glass disks. 6.2 For both liquid and gaseous products 6.2.1 Microburette, of capacity 2 ml, graduated in 0,01 ml. 7 Procedure 7.1 Liquid products Use the method specified in ISO/R 1393 with the following modifications appropriate for the products concerned:
33、7.1.1 Test portion Weigh, to the nearest 0,1 g, about 100 g of the laboratory sample. 7.1.2 Determination In the case of R 11 (boiling point 24 C), carry out the extraction with the water (5.1) previously cooled to 15 C. For all products, transfer the whole of the aqueous phase to a 250 ml conical f
34、lask and titrate. 7.2 Gaseous products Weigh, to the nearest 1 g, the capped sample cylinder containing the laboratory sample, remove the cap and connect the needle valve (6.1.1) to the valve of inverted cylinder type (b) (ISO 3427), or to valve A of cylinder type (a) (ISO 3427) (see the Figure). Ad
35、d 50 ml of the water (5.1) to each of the three gas washing bottles (6.1.3). Connect the outlet 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 the Figure. Open the sample cylinder valve fully and open the needle valve
36、 to the extent required to give a steady vaporization rate of about 100 g of sample per hour. NOTE 1The required setting is judged by experience and observation of the bubble rate through the gas washing bottles. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontr
37、olled Copy, (c) BSI BS 5598-6:1979 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 R 114. After about 1 h, close first the cylinder valve and then the needle valve. Disconnect the ne
38、edle valve and replace the cylinder cap. Allow the cylinder to warm up to room temperature, dry it if necessary, and reweigh it, to the nearest 1 g, under the same conditions as previously. Mix the contents of the first two gas washing bottles; if the sample is acid, the solution will be coloured ye
39、llow. 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 bottle should remain blue. If this is not the case, repeat the test. 8 Expression of result
40、s 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: where V and m have the same meaning as in 8.1. 8.3 The acid number, expressed in millig
41、rams of potassium hydroxide (KOH) per gram, is given by the formula: where V and m have the same meaning as in 8.1. 8.4 Express the result with a precision corresponding to the accuracy of weighing and titration. NOTEIf the concentration of the standard volumetric solution used is not exactly as spe
42、cified 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 expression used; c) any unusual features noted during the determination; d) any opera
43、tion not included in this International Standard or in the International Standards to which reference is made, or regarded as optional. V is the volume, in millilitres, of the standard volumetric sodium hydroxide solution (5.2) used for the titration; m is the mass, in grams, of the test portion (eq
44、ual to the change in mass of the sample cylinder in the case of gaseous products). V0,011 000 1 000 m - - 10 000V m -= V 365 m - - 56,1V0,01 m - - 0 561,V m - -= Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 BSI 11-19993 Fig
45、ure Apparatus for absorption of acidity for products gaseous at ordinary temperatures Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 4 BSI 11-1999 Annex Other ISO publications relating to halogenated hydrocarbons for industri
46、al use ISO/R 1393, Determination of acidity liquids. ISO/R 1394, Determination of cloud point liquids. ISO 2209, Sampling liquids. ISO 2210, Determination of residue on evaporation liquids. ISO 3427, Taking of a sample liquefied gases. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47
47、GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6:1979 BSI 11-1999 Publications referred to See national foreword Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:24:47 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-6: 1979 ISO 3363:1976 BSI 389 Chiswick High Road London W4 4AL BSI B
48、ritish Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users o
49、f British Standards 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 British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: