1、BRITISH STANDARD BS 5598-1: 1978 ISO 2209:1973 Methods of sampling and test for halogenated hydrocarbons Part 1: Sampling of liquid products UDC 661.723:547.411:543.05 14BS5598-1:1978 This British Standard, having been prepared under the directionof the Chemical Standards Committee, waspublished und
2、er theauthorityofthe ExecutiveBoard on 30 June 1978 BSI 11-1999 The following BSI references relate to the work on this standard: Committee reference CIC/4 Draft for comment 74/50328 DC ISBN 0 580 10237 8 Cooperating organizations The Chemicals Standards Committee, under whose direction this British
3、 Standard 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 Department of Health
4、 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 Great Britain L
5、td. 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 the following, were directly represented on the committee entrusted with the preparation
6、 of this British Standard: British Plastics Federation Fabric Care Research Association Fire Extinguishing Trades Association Imperial Chemical Industries Limited Imperial Smelting Corporation Institute of Metal Finishing Institute of Refrigeration Oil and Colour Chemists Association Pharmaceutical
7、Society of Great Britain Royal Institute of Chemistry Society of Chemical Industry Amendments issued since publication Amd. No. Date of issue CommentsBS5598-1:1978 BSI 11-1999 i Contents Page Cooperating organizations Inside front cover National foreword ii 1 Scope and field of application 1 2 Princ
8、iple 1 3 Apparatus 1 4 Procedure 1 5 Sampling report 4 Figure 1 Pipette 5 Figure 2 Steel sampler 5 Figure 3 Bottle 5 Figure 4 Continuous sampler 5 Table 1 2 Publications referred to Inside back coverBS5598-1:1978 ii BSI 11-1999 National foreword This Part of this British Standard is identical with I
9、SO2209 “Liquid halogenated hydrocarbons for industrial use Sampling”. It 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 has participated in the work of prepari
10、ng 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 international agreement is reached on the
11、 methods, it is proposed to publish them as Parts of this British Standard. 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 identical with tho
12、se used in British Standards; attention is especially drawn to the following. Wherever the 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 text and for
13、each there is a corresponding British Standard; these are as listed below: This standard specifies methods of sampling only and should not be used as a specification defining limits of purity. Reference to this standard should indicate that the methods of sampling used comply with the requirements o
14、f BS5598-1. 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 itself confer immunity from legal obligations. International Standard Corres
15、ponding British Standard ISO 842 BS 4726 Methods for sampling raw materials for paints and varnishes (technically equivalent) ISO 3165 a BS 5309 Methods for sampling chemical products Part 1 Introduction and general principles (related) a ISO 3165 is no longer at the stage of draft, as indicated in
16、the text; it was published in1976. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, pages1 to6, 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 t
17、he amendment table on the inside front cover.BS5598-1:1978 BSI 11-1999 1 1 Scope and field of application This International Standard specifies sampling procedures for liquid halogenated hydrocarbons for industrial use, with the exception of liquefied gases. NOTEFor the sampling of liquid halogenate
18、d hydrocarbons intended to be used as raw materials for paints and varnishes, see ISO842, Raw materials for paints and varnishes Sampling. The methods are applicable to products not contaminated by an extraneous phase (water, solid deposits, etc). However, accidental pollution is also considered and
19、 an initial examination is provided for checking phase homogeneity. Three cases are considered, namely: small containers (cans, drums); large containers (cylinders, tanks); continuous sampling. 2 Principle Formation of a blended bulk sample, representing the whole of the batch, by mixing several ele
20、mentary samples. The number and the method of taking of the elementary samples will depend on the number and capacity of vessels containing the product. 3 Apparatus Three main types of apparatus can be used for sampling, as appropriate: 3.1 Usual apparatus, of steel or glass, with a capacity of250 t
21、o500ml (for example, a pipette, as inFigure 1) for sampling from a small vessel. 3.2 Closeable device, with a capacity of500to1000ml (for example, a steel sampler with a ground closure, as inFigure 2) used mainly for sampling from large containers. A ballast bottle with a cork stopper can also be us
22、ed, but not for bottom sampling (for example, a bottle as inFigure 3). 3.3 Continuous samplers (for example as in Figure 4), connected to the flowline of the product, such as when delivering the batch to the tank. 4 Procedure WARNING A number of hazards may arise in the sampling of volatile solvents
23、. They include flammability and toxicity. 1) Flammability The lower-boiling solvents are flammable and the following precautions are advised: 1) Care must be taken to see that all sampling equipment used for these substances is made of low-energy spark generating material such as beryllium-copper al
24、loys or glass. If an earth connection can be made to large containers, this should be done. 2) All regulations regarding “controlled” or “flammable” areas in which the samples are being drawn must be strictly adhered to. Toxicity Vapour from lower-boiling solvents is toxic and precautions should be
25、taken to avoid its inhalation. It is recommended that two persons should be present when samples are drawn from large containers such as storage tanks, road tanks or rail tanks. Before sampling from rail tanks it should be ensured that no shunting operations are likely. In order to allow for the hig
26、h coefficient of expansion of certain products and to allow for the need ultimately to mix the samples thoroughly to obtain representative test samples the containers should be filled to between about80 and90% of their total capacity. Contacts with the skin, spillage on clothing, etc. should be avoi
27、ded as far as possible during sampling. The correct treatment for any harmful material should be known beforehand and the appropriate treatment antidote should be at hand. 4.1 General All sampling operations shall be carried out carefully and with a due regard for cleanliness. It is essential in the
28、 case of some products to work away from moisture, dust, smoke, etc. For a given level of sampling, the number of sampling vessels depends on the degree of homogeneity of the product, and not on the tonnage. However, the larger the batch to be sampled, the greater is the need to increase the probabi
29、lity that the blended bulk sample is representative, resulting in a larger number of samples being taken. 4.2 Small containers Cans, drums and, in general, containers with a capacity less than or equal to300litres. 1) With regard to safety precautions, see also ISO3165, Sampling of chemical products
30、 Safety (at present at the stage of draft).BS5598-1:1978 2 BSI 11-1999 4.2.1 Number and selection of containers for sampling In the absence of any agreement to the contrary between the parties, useTable 1 to give reasonable values for the number of vessels to be sampled for various numbers of contai
31、ners making up the batch. Table 1 The containers to be sampled shall be chosen at random. 4.2.2 Taking of elementary samples Carry out the sampling using the usual apparatus(3.1). Always take the same quantity ofliquid. In order to take a sample, introduce the sampler vertically into the container,
32、down to the bottom. Immersion shall be carried out sufficiently slowly for the level of the liquid inside the sampler to be near the level in the container. Close the sampler with a finger, then withdraw it from the container, and allow the quantity thus sampled to run into a completely clean and dr
33、y flask. NOTEIf sampling has to be carried out at a certain level, for example for checking homogeneity (see4.2.3), introduce the sampler, closed at the top, down to the level to be examined, open and then, after the liquid has been introduced, re-close and withdraw from the container. 4.2.3 Initial
34、 examination for assessing phase homogeneity in the container If confirmation is required that the contents of the vessels are homogeneous, or can be made homogeneous readily by stirring, an initial visual examination is recommended on a number of elementary samples. These samples shall be taken fro
35、m a certain number of containers for sampling. (SeeTable 1.) Take three samples from each of the containers selected: one at the top, another at the middle, and a third as near as possible to the bottom, in accordance with the instructions in4.2.2. First examine the appearance of the three samples (
36、homogeneous phase, suspended particles, etc.), then mix them and stir vigorously. Leave to stand and examine the appearance of the mixture. Three cases are possible according to the observations: a) the product appears homogeneous in each container examined; continue as indicated in4.2.5; b) the pro
37、duct appears slightly heterogeneous but can be made homogeneous by stirring (fine suspended particles, for example); continue as indicated in4.2.4; c) the product cannot be made homogeneous by stirring (layer of water or solid deposit which cannot be dispersed, for example); continue the initial exa
38、mination on other containers, in order to reach a closer assessment of the phase homogeneity in the container. In each of the containers taken for the initial examination, separate the two phases present as well as possible, in order to determine approximately the percentage of extraneous phase. Car
39、ry out sampling as indicated in4.2.5, but take care to sample only the halogenated hydrocarbon. 4.2.4 Homogenisation If it is first necessary to make the contents of the containers to be sampled homogeneous 4.2.3 b), stir the contents of each of the containers mechanically for several minutes, using
40、 a stirrer. Stirring shall be more vigorous the less homogeneous is the product. 4.2.5 Sampling proper Blended bulk sample and laboratory sample Take the elementary samples as described in4.2.2, taking samples from the container to be sampled. NOTEIf the product is homogeneous, the samples taken in
41、the course of the initial examination can be used if less than one third of the total volume is taken. Pour all the elementary samples into a clean and dry container, and stir vigorously in order to make homogeneous. The blended bulk sample is thus obtained. If this sample is too large, take a suita
42、ble volume, after stirring if necessary. A laboratory sample is thus obtained. In all cases the sample shall be kept in a clean, dry, perfectly stoppered glass flask away from light. Number of containers in the batch Number of containers to be sampled 1 to4 all 5 to10 5 11 to20 6 21 to30 7 31 to50 8
43、 51 to75 9 76 to 100 10 101 to 125 11 126 to 150 12 151 to 200 13 201 to 250 14 etc.BS5598-1:1978 BSI 11-1999 3 NOTEIf a closer knowledge is required of the batch to be sampled, it may be advantageous to prepare several partial samples, obtained by blending several elementary samples, and not a sing
44、le blended bulk sample which will provide only one test result corresponding to the average of the batch. Each partial sample shall be the subject of a test, and several results will thus be obtained providing a knowledge not only of the mean value of the batch, but also of the deviations from this
45、mean value. 4.3 Large containers (capacity over 300 litres) Large drums, cylinders, tanks, fixed or transportable. 4.3.1 Number and choice of containers for sampling Follow exactly the instructions given in4.2.1. 4.3.2 Taking of elementary samples Use a closeable device (3.2) or preferably a samplin
46、g tube. Always take the same amount of liquid, between500 and1000ml. In order to take a sample, lower the closed device into the liquid down to the necessary depth (see4.3.4). Open the device to allow it to fill and then reclose, in the case of the sampling tube, and raise to the surface. Transfer t
47、he sample thus obtained into a clean, dry flask. Continuous sampling can also be carried out when transferring the liquid (see4.3.5). 4.3.3 Initial examination for assessing phase homogeneity in the container If confirmation is required that the contents of the containers are homogeneous, an initial
48、 visual examination of a number of elementary samples is recommended. These samples shall be taken from a certain number (seeTable 1) of containers for sampling. For containers with a capacity less than or equal to1000litres proceed as for small containers (see4.2.3). For larger containers, take one
49、 or, if possible, two series of samples along one or two vertical lines, selected as a function of the form and location of the openings (vertical lines located near the two ends of the tank for example). Take three samples, one at the top, another at the middle and a third as near as possible to the bottom. Take the samples as described in4.3.2 and place them in different containers. Examine the appearance of all the elementary samples taken from the same container (homogeneous phase, suspended particles, etc.). Two cases are possible according to the
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