1、BRITISH STANDARD BS5598-2: 1979 ISO3427:1976 Methods of sampling and test for halogenated hydrocarbons Part2:Sampling of liquefied gases UDC661.723:547.411:543.0514BS5598-2:1979 This BritishStandard, having been prepared under the directionof the Chemicals Standards Committee, was published under th
2、e authority ofthe Executive Board and cameinto effect on 28February1979 BSI12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/4 Draft for comment74/52954 ISBN 0 580 10707 8 Cooperating organizations The Chemicals Standards Committee, under whose directi
3、on this BritishStandard was prepared, 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 Depart
4、ment of Health and Social Security 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 G
5、reat Britain Ltd. Royal Institute 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 thefollowing, were directly represented on the committee entrusted with th
6、e preparation of this BritishStandard: Fabric Care Research Association Fire Extinguishing Trades Association Institute of Metal Finishing Institute of Refrigeration Individual company Amendments issued since publication Amd. No. Date of issue CommentsBS5598-2:1979 BSI 12-1999 i Contents Page Cooper
7、ating organizations Inside front cover National foreword ii 1 Scope and field of application 1 2 Principle 1 3 Apparatus 1 4 Procedure 1 Annex Other ISO publications relating to halogenated hydrocarbonsforindustrial use 4 Figure 1 Sample cylinder 2 Figure 2 Assembly using type (a) sample cylinder 3
8、Publications referred to Inside back coverBS5598-2:1979 ii BSI 12-1999 National foreword This BritishStandard has been prepared under the direction of the Chemicals Standards Committee in order to provide methods of sampling and test for halogenated hydrocarbons. For some years the United Kingdom ha
9、s 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 amines” of Technical Committee47 “Chemistry” of the International Organization for Standardization (ISO). As inte
10、rnational agreement is reached on the methods, it is proposed to publish them as Parts of this BritishStandard as follows: Part1: Sampling of liquid products, identical with ISO2209; Part2: Sampling of liquefied gases, identical with ISO3427; Part3: Determination of residue on evaporation, identical
11、 with ISO2210; Part4: Determination of acidity Titrimetric method, identical withISO1393; Part5: Determination of cloud point, identical with ISO1394; Part6: Determination of acidity of fluorochlorinated hydrocarbons, identical with ISO3363; Part7: Methods of test for methyl chloride and ethyl chlor
12、ide, identical withISO5781 1) ; Part8: Determination of non-volatile residue in fluorinated hydrocarbons, identical with ISO5789 1) . This Part is identical with ISO3427 “Gaseous halogenated hydrocarbons (liquefied gases) Taking of a sample”. Terminology and conventions. The text of the Internationa
13、l Standard hasbeen approved as suitable for publication, without deviation, as a BritishStandard. Some terminology and certain conventions are not identical with those used in BritishStandards; attention is especially drawn to the following. Where the words “International Standard” appear, referring
14、 to this standard, they should be interpreted as “BritishStandard”. Cross-references. The following International Standards are referred to in the Annex and for each there is a corresponding BritishStandard; these are listed below. 1) In course of preparation. International Standard Corresponding Br
15、itishStandard a ISO/R1393 a ISO/R1394 ISO2209:1973 BS5598 Methods of sampling and test for halogenated hydrocarbons Part4:1979 Determination of acidity (Identical) BS5598 Methods of sampling and test for halogenated hydrocarbons Part5:1979 Determination of cloud point (Identical) BS5598 Methods of s
16、ampling and test for halogenated hydrocarbons Part1:1978 Sampling of liquid products (Identical) ISO2210:1972 BS5598 Methods of sampling and test for halogenated hydrocarbons Part3 Determination of residue on evaporation (Identical) a ISO/R1393 and ISO/R1394 have been superseded by ISO1393:1977 and
17、ISO1394:1977 respectively.BS5598-2:1979 BSI 12-1999 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 adequa
18、te exhaust. This standard specifies methods of sampling only and should not be referred to asa specification defining limits 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 BS5598-2. A British Standard does
19、 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 immunity from legal obligations. Summary of pages This document comprises a front cover, an insid
20、e front cover, pagesi 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 blankBS5598-2:1979 BSI 12-1999 1 1 Scope and field o
21、f 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 (cylinder, drum, tank, etc.). 2 Principle Taking of a sample of halogenated hydrocarbon in a stai
22、nless 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 International Standards for the products concerned. This sample shall be taken only from the liquefied
23、phase. 3 Apparatus 3.1 Sampling assembly (seeFigure 2). 3.1.1 Sample cylinder, constructed of stainless steel, capable of withstanding an internal pressure of at least3MPa 2)or as prescribed for a particular product 3) , and of one of the two types shown in Figure 1: a) sample cylinder fitted with t
24、wo needle valves, connected respectively to an internal dip-tube extending to near the bottom of the cylinder and to a short internal tube (length30mm); b) sample cylinder with only one valve and without internal tubes. The sample cylinder shall be designed so as to be easily cleaned and dried and i
25、ts valve outlet(s) shallbe 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 shall be small in relation to the total quantity contained in the cylinder in order to avoid any varia
26、tion 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 anappropriate solvent, for example ethanol or acetone. Check its pressure-tightness periodically, for example by immersing it in wa
27、ter and filling it with nitrogen to a pressure ofabout3MPa 2) . 3.1.2 Connecting tube, preferably made of stainless steel, of suitable length and having threaded connectors (unions) fitting respectively the valve ofthe liquefied halogenated hydrocarbon container and the valve of the sample cylinder(
28、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 at105 to110 C. 3.3 Balance, accurate to1g. 3.4 Vacuum pump, capable of reducing the pressure in the cylinder(3.1.1) rapidly to ab
29、out100Pa 4) . 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 to the product to be sampled. 4 Procedure 4.1 Preparation of the cylinder(3.1.1) and connecting tube(3.1.2) 4.1
30、.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 temperature; continue this purging in the oven(3.2), controlled at105 to110 C, for at least30min bymeans of a thic
31、k-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 still hot, to about100Pa or lower, and maintain at this pressure for at least30min. 4.1.2 In the case of a cylinder of ty
32、pe (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) and pass a stream of the nitrogen(3.6) through these and then, by means of a further length of flexible tube, into the cylind
33、er emerging inside near the bottom; continue this purging with the nitrogen(3.6) in the oven(3.2), controlled at105 to110 C, for at least30min by means of a thick-walled flexible tube passing through an opening in the side of the oven; cool the valve, the cylinder and the connecting tube in the desi
34、ccator(3.5); reassemble the valve and cylinder, and fit the connecting tube; 2) 3MPa=30bar 3) If there exists a national or international regulation on this subject, it should be respected. 4) 100Pa=1mbarBS5598-2:1979 2 BSI 12-1999 reduce the pressure in the connecting tube/valve/cylinder assembly t
35、o about100Pa orlower, and maintain at this pressure for at least30min. 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 connec
36、ting tube (3.1.2), evacuate to a pressure of about100Pa 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 at105 to110 C, for at least1h
37、. Reduce the pressure in the still-hot cylinder and connecting tube to about100Pa or lower, and maintain it at this pressure for at least30min. 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
38、 each other and weigh the cylinder, 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) for10 to15min, taking care to keep the valve(s) free from condensation. Clean the mouth of the liquid-phase valve on the container from which the sam
39、ple is to be taken, using a jet 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. Fi
40、t the other end of the tube(3.1.2) to the valve of the sample cylinder(3.1.1) valve A for cylinder type (a), but without tightening the connection (seeFigure 2). Cautiously open the valve of the container and allowthe liquid to flow so that the air present in theconnecting tube is forced out through
41、 the non-tightened connection. 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
42、 sample. NOTEIt is recommended 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 t
43、otal capacity of the 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 wh
44、en the discharge consists 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 reweighin
45、g later. Figure 1 Sample cylinder(3.1.1)BS5598-2:1979 BSI 12-1999 3 Figure 2 Assembly using a type (a) sample cylinderBS5598-2:1979 4 BSI 12-1999 Annex Other ISO publications relating to halogenated hydrocarbons forindustrial use ISO/R1393, Determination of the acidity liquids. ISO/R1394, Determinat
46、ion of the cloud point liquids. ISO2209, Sampling liquids. ISO2210, Determination of residue on evaporation liquids.BS5598-2:1979 BSI 12-1999 Publications referred to Seenational forewordBS5598-2: 1979 ISO3427:1976 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the in
47、dependent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions BritishStandards are updated by amendment or revision. Users of BritishStandards should make sure that the
48、y 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 BritishStandard would inform the Secretary of the technical committee responsible, the id
49、entity of which can be found on the inside front cover. Tel:02089969000. Fax:02089967400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services. Tel:02089969001. Fax:02089967001. In response to orders for international standards, it is BSI policy to supply the BSI implementation of those
