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1、BRITISH STANDARD BS 5598-2: 1979 ISO 3427:1976 Methods of sampling and test for halogenated hydrocarbons Part 2: Sampling of liquefied gases UDC 661.723:547.411:543.05 14 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 This Br
2、itish Standard, having been prepared under the direction of the Chemicals Standards Committee, was published under the authority of the Executive Board and came into effect on 28 February 1979 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/4 Dra
3、ft for comment 74/52954 ISBN 0 580 10707 8 Cooperating organizations The Chemicals Standards Committee, under whose direction this British Standard was prepared, consists of representatives from the following Government departments and scientific and industrial organizations: Association of Fatty Ac
4、id 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 Solvents Association Minis
5、try 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 Committee The organizations marked
6、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: Fabric Care Research Association Fire Extinguishing Trades Association Institute of Metal Finishing Institute of Refrigeration Individu
7、al company Amendments issued since publication Amd. No.Date of issueComments Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 BSI 12-1999i Contents Page Cooperating organizationsInside front cover National forewordii 1Scope and
8、 field of application1 2Principle1 3Apparatus1 4Procedure1 Annex Other ISO publications relating to halogenated hydrocarbons for industrial use4 Figure 1 Sample cylinder2 Figure 2 Assembly using type (a) sample cylinder3 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldu
9、n, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 ii BSI 12-1999 National foreword This British Standard has been prepared under the direction of the Chemicals Standards Committee in order to provide methods of sampling and test for halogenated hydrocarbons. For so
10、me 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 hydrocarbons and amines” of Technical Committee 47 “Chemistry” of the International Organization fo
11、r 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 of liquid products, identical with ISO 2209; Part 2: Sampling of liquefied gases, identical with ISO 3427; Part 3: Determinatio
12、n 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: Determination of acidity of fluorochlorinated hydrocarbons, identical with ISO 3363; Part 7: Meth
13、ods 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 ISO 3427 “Gaseous halogenated hydrocarbons (liquefied gases) Taking of a sample”. Terminolo
14、gy 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 identical with those used in British Standards; attention is especially drawn to the following. Where t
15、he words “International Standard” appear, referring to this standard, they should be interpreted as “British Standard”. Cross-references. The following International Standards are referred to in the Annex and for each there is a corresponding British Standard; these are listed below. 1) In course of
16、 preparation. International StandardCorresponding British Standard aISO/R 1393 aISO/R 1394 ISO 2209:1973 BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 4:1979 Determination of acidity (Identical) BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 5:1979 De
17、termination of cloud point (Identical) BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 1:1978 Sampling of liquid products (Identical) ISO 2210:1972BS 5598 Methods of sampling and test for halogenated hydrocarbons Part 3 Determination of residue on evaporation (Identical) a ISO
18、/R 1393 and ISO/R 1394 have been superseded by ISO 1393:1977 and ISO 1394:1977 respectively. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 BSI 12-1999iii Additional information WARNING NOTE. Care should be taken to avoid bre
19、athing 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. This standard specifies methods of sampling only and should not be referred to as a specification defining limits
20、of purity. Reference to the standard should be in a form of words indicating that the method of sampling used conforms to the requirements of BS 5598-2. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their cor
21、rect 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, pages i to iv, pages 1 to 4, an inside back cover and a back cover. This standard has been updated (see copyr
22、ight date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:
23、23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 BSI 12-19991 1 Scope and field of application This International Standard specifies the apparatus and the procedures to be used when taking a laboratory sample of a gaseous halogenated hydrocarbon (as a liquefied gas) from a container (
24、cylinder, drum, tank, etc.). 2 Principle Taking of a sample of halogenated hydrocarbon in a stainless steel cylinder, previously cleaned, dried and evacuated. The sample cylinder is filled to the filling ratio allowed by safety considerations: relevant details will be given in the individual Interna
25、tional Standards for the products concerned. This sample shall be taken only from the liquefied phase. 3 Apparatus 3.1 Sampling assembly (see Figure 2). 3.1.1 Sample cylinder, constructed of stainless steel, capable of withstanding an internal pressure of at least 3 MPa2) or as prescribed for a part
26、icular product3), and of one of the two types shown in Figure 1: a) sample cylinder fitted with two needle valves, connected respectively to an internal dip-tube extending to near the bottom of the cylinder and to a short internal tube (length 30 mm); b) sample cylinder with only one valve and witho
27、ut internal tubes. The sample cylinder shall be designed so as to be easily cleaned and dried and its valve outlet(s) shall be fitted with sealing cap(s) for use during transport. Its capacity depends on the quantity of the product required to carry out all of the intended analyses. This quantity sh
28、all be small in relation to the total quantity contained in the cylinder in order to avoid any variation in the composition of the liquid phase. NOTEThe interior of the sample cylinder shall be examined periodically. If the surface is not clean, wash it with water and an appropriate solvent, for exa
29、mple ethanol or acetone. Check its pressure-tightness periodically, for example by immersing it in water and filling it with nitrogen to a pressure of about 3 MPa2). 3.1.2 Connecting tube, preferably made of stainless steel, of suitable length and having threaded connectors (unions) fitting respecti
30、vely the valve of the liquefied halogenated hydrocarbon container and the valve of the sample cylinder (3.1.1). All connectors shall be fitted with washers made of a material which is not attacked by the product to be analysed. 3.2 Electric oven, capable of being controlled at 105 to 110 C. 3.3 Bala
31、nce, accurate to 1 g. 3.4 Vacuum pump, capable of reducing the pressure in the cylinder (3.1.1) rapidly to about 100 Pa4). 3.5 Desiccator, capable of containing the cylinder (3.1.1), with an efficient desiccant. 3.6 Compressed nitrogen, clean and dry. 3.7 Cooling bath, at a temperature appropriate t
32、o the product to be sampled. 4 Procedure 4.1 Preparation of the cylinder (3.1.1) and connecting tube (3.1.2) 4.1.1 In the case of a cylinder of type (a) with two valves carry out the three following operations in succession: purge the cylinder and connecting tube with the nitrogen (3.6) at ambient t
33、emperature; continue this purging in the oven (3.2), controlled at 105 to 110 C, for at least 30 min by means of a thick-walled flexible tube passing through an opening in the side of the oven; reduce the pressure in the connecting tube/cylinder assembly, after its removal from the oven and while st
34、ill hot, to about 100 Pa or lower, and maintain at this pressure for at least 30 min. 4.1.2 In the case of a cylinder of type (b) with only one valve carry out the five following operations in sucession: remove the valve of the cylinder, join a suitable flexible tube to the connecting tube (3.1.2) a
35、nd pass a stream of the nitrogen (3.6) through these and then, by means of a further length of flexible tube, into the cylinder emerging inside near the bottom; continue this purging with the nitrogen (3.6) in the oven (3.2), controlled at 105 to 110 C, for at least 30 min by means of a thick-walled
36、 flexible tube passing through an opening in the side of the oven; cool the valve, the cylinder and the connecting tube in the desiccator (3.5); reassemble the valve and cylinder, and fit the connecting tube; 2) 3 MPa = 30 bar 3) If there exists a national or international regulation on this subject
37、, it should be respected. 4) 100 Pa = 1 mbar Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 2 BSI 12-1999 reduce the pressure in the connecting tube/valve/cylinder assembly to about 100 Pa or lower, and maintain at this press
38、ure for at least 30 min. NOTEWhen the sample cylinder is used only for one product of practically constant composition, the procedure specified above may be simplified as follows. Empty the cylinder of the remainder of the previous sample. Fit the connecting tube (3.1.2), evacuate to a pressure of a
39、bout 100 Pa and then allow to refill with the nitrogen (3.6) at atmospheric pressure. Repeat the evacuation and refilling twice and place the cylinder and connecting tube, with the valve fully open, in the oven 3.2, controlled at 105 to 110 C, for at least 1 h. Reduce the pressure in the still-hot c
40、ylinder and connecting tube to about 100 Pa or lower, and maintain it at this pressure for at least 30 min. 4.1.3 In both cases, close the valve(s) of the cylinder to retain the vacuum. Disconnect the cylinder and connecting tube from the vacuum pump (3.4) and from each other and weigh the cylinder,
41、 using the balance (3.3). 4.2 Taking of the sample Cool the cylinder (3.1.1) by immersing it in the cooling bath (3.7) for 10 to 15 min, taking care to keep the valve(s) free from condensation. Clean the mouth of the liquid-phase valve on the container from which the sample is to be taken, using a j
42、et of the nitrogen (3.6). When the sample is to be taken from a container fitted with only one valve, position the container so that the sample will be taken from the liquid phase. Join the connecting tube (3.1.2) hermetically to the liquid phase valve of the container. Fit the other end of the tube
43、 (3.1.2) to the valve of the sample cylinder (3.1.1) valve A for cylinder type (a), but without tightening the connection (see Figure 2). Cautiously open the valve of the container and allow the liquid to flow so that the air present in the connecting tube is forced out through the non-tightened con
44、nection. Then tighten the connection on the valve of the sample cylinder to make a hermetic seal. Open the valve of the cylinder (3.1.1) and allow it to fill with liquid. Close the valves and disconnect the cylinder. Check the filling of the cylinder immediately after taking the sample. NOTEIt is re
45、commended that, if suitable apparatus (spring balance and flexible connecting tube) is available, the cylinder be weighed during filling. 4.3 Checking of filling Using the balance (3.3), reweigh the full cylinder (3.1.1) to check on the filling operation, taking into account the total capacity of th
46、e cylinder and the density of the liquid phase halogenated hydrocarbon concerned. If the recommended filling ratio of the sample cylinder has been exceeded, discharge the excess as follows. For a cylinder of type (a), hold it with the valves uppermost, open valve B and close it when the discharge co
47、nsists of vapour only. For a cylinder of type (b), hold it with the valve underneath, open the valve carefully and allow the necessary amount of liquid to escape. Fit the valve outlet caps. Weigh the cylinder again to check the filling and check its pressure-tightness by reweighing later. Figure 1 S
48、ample cylinder (3.1.1) Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 BSI 12-19993 Figure 2 Assembly using a type (a) sample cylinder Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolle
49、d Copy, (c) BSI BS 5598-2:1979 4 BSI 12-1999 Annex Other ISO publications relating to halogenated hydrocarbons for industrial use ISO/R 1393, Determination of the acidity liquids. ISO/R 1394, Determination of the cloud point liquids. ISO 2209, Sampling liquids. ISO 2210, Determination of residue on evaporation liquids. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:23:55 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5598-2:1979 BSI 12-1999 Publications referred to See national foreword Licens