1、UDC 665.6/.7: 662.753 : 621.892:620.113 DEUTSCHE NORM December 1990 Sampling of petroleum products General information DIN - 51 750 Part 1 Prfung von Minerallen; Probenahme; Allgemeines Supersedes August 1983 edition. In keeping with current practice in standards published by the International Organ
2、ization for Standardization (ISO), a comma has been used throughout as the decimal marker. See Explanatory notes for connection with IS0 3170 : 1988 published by the International Organization for Standardization (ISO) and ASTM D 4057-88 published by the American Society for Testing and Materials (A
3、STM). 1 Field of application 1.1 a) crude oils, liquid petroleum products (e.9. engine fuels, special boiling point spirits and white spirits, fuel oils, kerosene and liquid lubricants (cf. DIN 51 750 Part 2 for sampling procedure), as well as b) pasty and solid petroleum products (e.g. lubricating
4、greases, petroleum jelly and paraffins (cf. DIN 51 750 Pari 3 for Bampling procedure). Where the petroleum product can be liquefied by heating without that chang- ing its composition, sampling may also be carried out as specified in DIN 51 750 Part 2. The DIN 51 750 series of standards covers 1.2 Th
5、is standard applies to petroleum products forming the content of one or more containers, which may vary in type and size and be completely or partly filled, or contained in a pipeline. The petroleum product may thus be flowing or non-flowing. For the purposes of this standard, a product is defined a
6、s non-flowing when inflow and ouiilow from a container are prevented and as flowing if it is conveyed in a pipeline or discharged via a container outlet. 1.3 This standard does not cover a) bituminous binders (cf. EN 58); b) lubricating oils in internal combustion engines (cf. DIN 51 574); c) liquef
7、ied natural gases (cf. DIN 51 610); d) solid fuels (cf. DIN 51 701 Part 2 to Part 4); e) gaseous fuels, inert and combustion gases (cf. DIN 51 853). 2 Scope This standard specifies methods of manual sampling of petroleum products, either by taking bulk samples or tap samples. 2.1 Bulk sampling The a
8、im of bulk sampling is to obtain a representative sample, .e. the characteristics as determined by testing may be assumed to represent the characteristics of the bulk. 2.2 lap sampling The aim of tap sampling is to obtain a sample which may be used to assess the quality of a product at its point of
9、delivery (e.g. petrol pump). 3 Concepts 3.1 Spot sample A spot sample is a sample collected at a discrete location in the container. 3.1.1 Skim sample A skim sample is a spot sample collected at a point located not more than 5 cm below the surface. 3.1.2 Top sample A top sample is a spot sample coll
10、ected 15 cm below the surface of the product. 3.1.3 Upper sample An upper sample is aspot sample collected at the mid-point of the upper third of the container contents. 3.1.4 Middle sample A middle sample is a spot sample collected at a point approximately halfway between upper and lower sampling p
11、oint. 3.1.5 Lower sampie A lower sample is a spot sample collected at the mid-point of the lower third of the container contents. 3.1.6 Boaom sample A bottom sample is a spot sample collected at the bottom surface of a container. 3.1.7 Draln sample A drain sample is a spot sample collected from the
12、draw-off point of a container or from a dispensing device at a point of delivery. Continued on pages 2 to 6 DIN 51 750 Part 7 Engl. Price group 6 uth Verlag GmbH, Berlin. has the exclusive right of sale for German Standards (DIN-Normen). 06.92 Sales No. O106 Page 2 DIN 51 750 Part 1 Table 1. Minimum
13、 number o1 packages from which one spot sample each Is to be collected Total number of packages (per batch) 1 to 3 4tO 64 65to 125 126to 216 217 to 343 344to 512 513 to 729 730 to 1000 1001 to 1331 Minimum number of packages from which one spot sample each is to be collected al I 4 5 6 7 8 9 10 11 3
14、.2 Ail-levels sample An all-levels sample is a sample collected by passing the sampler (e.g. sampling tube or bottle, or bomb-type sampler) through the total depth of a container so that all levels are represented proportionately. 3.2.1 Runnlng sample A running sample is an all-levels sample collect
15、ed by passing a sampling bottle or a bomb-type sampler through the total depth of a container. 3.3 Mainstream sample A mainstream sample is a combined sample collected with a scoop from a stream of liquid leaving a container. 3.4 Sidestream sample A sidestream sample is a sample collected from a sid
16、e- stream drawn off from the main pipeline. 3.5 Combined sample A combined sample is a blend of spot samples. 3.6 Composite sample A composite sample is obtained by combining a number of spot samples taken according to a sampling plan in given proportions so as to obtain a sample representative of t
17、he bulk of a product. 3.7 Laboratory sample A laboratory sample is the sample submitted to the laboratory for examination. For individual examinations (e.9. for analyses), specimens are taken from that sample, which may have undergone special treatment. If the vapour pressure of a product is to be d
18、etermined, decantation of the sample is not permitted. 3.8 Representative sample A representative sample is a sample which reproduces as closely as possible the average characteristics of the bulk. 4 General conditions for collecting 4.1 Sampling from containers of capacity not exceeding 5 ms 4.1.1
19、Sample type If the contents of a container can be assumed to be homogeneous, a spot sample shall be considered repre- sentative, otherwise an all-levels sample is to be collected. representalive samples Total number of packages (per batch) 1332 to 1728 1729 to 2197 2198 to 2744 2745 to 3375 3376 to
20、4096 4097 to 4913 4914 to 5832 5833 to 6859 6860 or more Minimum number of packages from which one spot sample each is to be collected 12 13 14 15 16 17 18 19 20 4.1.2 Sample size If the bulk, whatever its volume, of a homogeneous product takes up more than one barrel, drum or other small container
21、with a capacity not exceeding 5 m3, the number of containers from which one spot sample each is to be taken is specified for liquid petroleum products in table 1, and for pasty and solid petroleum products in table 2. The mini- mum numbers stated are generally large enough to obtain representative s
22、amples. If the total batch of a product has been transferred to containers of different sizes, all containers of one size shall be considered a separate batch. 4.1.3 Combination of spot samples Spot samples may be blended to form a combined sample il the product in a number of containers seems to be
23、 homogeneous. Otherwise, .e. if the barrels bear different markings, if they have a different temperature, or if there are differences in sample appearance or in the weather conditions they have been exposed to, only the spot samples that appear homogeneous shall be combined. When combining samples,
24、 due attention shall be paid to the specifications of subclause 3.7, second paragraph, and clause 6. 4.2 Sampling from containers of capacity exceeding 5 ms 4.2.1 Spot samples A spot sample collected from a container of capacity exceeding 5 m3 may be regarded as representative if the product is know
25、n to be completely homogeneous or has been vigorously mixed immediately prior to sampling. Homogeneity of the material cannot be assumed if a) it consists of components which cannot be mixed in any given ratio; b) there are differences in temperature within the product; c) it is composed of two or m
26、ore petroleum products with different characteristics (e.g. density or viscosity). 4.2.2 Composite samples A composite sample is deemed to be representative if it has been collected from a) a product in a vertical cylindrical tank and consists of a mixture of equal parts by volume of upper, middle a
27、nd lower samples, or b) a product in a horizontal cylindrical tank and consists of a mixture of spot samples as specified in table 3. DIN 51 750 Part 1 Page 3 Capacity o package, in kg Minimum sample size andior minimum number o packages for a laboratory sample Total size of batch I Below 0.5) I Any
28、 I Sufficient for a combined sample of 1 kg I Above 5 I 0,5 to 23 I Any I Three packages I Below 5 t Sufficient for a combined sample of 1 to 1,5 kg derived from one or more packages Sufficient for a combined sample of 1 to 2.5 kg derived from two or more packages Sufficient for a combined sample of
29、 1 to 2,5 kg derived from three or more packages 5 to 25 t Above 25 t Any I One package I I Above2,5upto5 I 50 50 50 50 50 40 - - - - 20 20 20 20 20 20 20 15 10 5 Table 3. Collection of spot samples from horizontal cylindrical containers Liquid depth, as a percentage of container diameter 1 O0 90 80
30、 70 60 50 40 30 20 10 I Constituents of composite sample, as percentages by volume I Sampling level, as a percentage of diameter above bottom Middle I Lower -I- Lower 30 30 30 40 50 60 1 O0 1 O0 1 O0 1 O0 By agreement, a running sample may be taken instead of a composite sample, but this shall be cl
31、early identified as such. The running sample shall not be considered a composite sample if the material at the sampling levels is not homogeneous or there are doubts as to whether the sampler has been drawn at a uniform rate through the different levels. If a composite sample is collected immediatel
32、y after the container has been filled, then it is sufflcientfor ittoconsist of equal parts by volume of middle and bottom samples only. A drain sample may be taken instead of a bottom sample provided that a sufficient quantity has been pre- viously drawn off to ensure that the sample is free from se
33、diments that may have been in the tank. Spot samples that do not appear to be homogeneous shall not be used to prepare composite samples. If the total quantity of a given product occupies more than one container (e.g. units in a tank farm or container area, compartments of an oil tanker) and if each
34、 container has a capacity of more than 5 m3, separate composite samples shall be prepared from the contents o each container. Preparation of a combined sample from the composite samples thus obtained shall be subject to agreement. 4.3 Sampling a flowing produd Mainstream samples and sidestream sampl
35、es shall be regarded as representative. 4.4 Tap sampling Drain samples collected from dispensers shall be regarded as representative of the product discharged. 5 Sampling personnel 5.1 The way in which a sample is taken significantly affects the result o the test. The sampling procedure shall be sel
36、ected to suit the particular case and the person delegated to collect samples shall be experienced in the sampling of the material concerned. A sampling report shall be be prepared which contains all relevant details (e.g. time of sampling, sampling site, designation of container and quantity of sam
37、ple taken, type o sampler used (cf. Appendix A and DIN 51 750 Parts 2 and 3) and type of sample prepared (cf. subclauses 3.1 to 3.8). Note. The relevant safety regulations shall be observed when sampling toxic liquids. Sampling personnel shall avoid breathing vapours from toxic substances and shall
38、not wear shoes with nails or shoes with a high electrical resistance. 5.2 For arbitration analyses, the delegation of the person who collects samples shall be by agreement. Page 4 DIN 51 750 Part 1 6 Preparation of laboratory sample and treat- ment prior to testing 6.1 Spot samples shall not be mixe
39、d to form a combined or a composite sample at the point of collection but in a closed room, preferably in a laboratory. In the case of lubricating greases, where determination of cone penetration as described in DIN 51 804 Part 2 or IS0 2137 is not required, the sample shall be thoroughly mixed if t
40、he worked penetration in accordance with the above-mentioned standards exceeds 175 units. A representative sample shall be divided into approxi- mately equal portions and transferred to four vessels, which shall be filled to 70 to 90% of their capacity. Every test portion (laboratory sample) shall b
41、e of adequate size for the intended analysis. For determining the vapour pressure, four samples col- lected under identical conditions shall be regarded as representative. 6.2 Thoroughly cleaned and dried vessels with tight closures may be used as containers (e.g. steel cans and type-approved plasti
42、cs spare fuel cans bearing an official test number). In the case of saponifiable greases, wide mouth glass bottles or containers made of porcelain, earthenware or suitable plastics shall be used, due account also being taken in their selection of any sensitivity of the sample to light, moisture, etc
43、. Samples intended for the determination of vapour pressure shall be transported and stored only in dark glass bottles or steel cans with gas-tight closure. The containers shall be closed immediately after filling and the closures provided with lead seals or sealing tags which also serve to secure t
44、he tie-on label as illustrated in Appendix A (size as in DIN 476) by way of example. 6.3 One each of four samples obtained as described in subclause 6.2 shall be distributed to: a) the client; b) the laboratory commissioned to carry out the analysis; c) the person delegated to take the sample for ar
45、bitration d) the manufacturer and/or supplier (.e. party responsible analysis purposes; for the quality of the product). 6.4 Samples of hazard categories A I and A II l) shall not be exposed to temperatures above 28 OC (maximum ambient temperature specified in DIN 50014) between sampling and testing
46、. I) See subclause 2.1 of DIN 51 755, March 1974 edition, for hazard categories. DIN 51 750 Part 1 Page 5 Appendix A Specimen tie-on label Sampling as specified in DIN 51 750 Part 2 or 3 Address of sample collector: Sample No. of product originating from rail tanker no. road tanker no. tank no. Samp
47、ling method: Productype: Quantity: Sampling equipment: Sampling site: Description of sampling point: Date of sampling: Time of sampling: Signature of sample collector: Page 6 DIN 51 750 Part 1 Standards referred to DIN 476 DIN 50 014 DIN 51 574 DIN 51 610 DIN 51 701 Part 2 DIN 51 701 Part 3 DIN 51 7
48、04 Part 4 DIN 51 750 Part 2 DIN 51 750 Part 3 DIN 51 755 DIN 51 804 Part 2 DIN 51 853 EN 58 IS0 2137 : 1985 IS0 31 70 : 1988*) ASTM D 4057-88) Trimmed sizes of paper Artificial climates in technical applications; standard atmospheres Sampling of lubricating oils taken from internal combustion engine
49、s Sampling of liquefied petroleum gases Sampling of solid fuels; procedure Sampling of solid fuels; sample preparation Sampling of solid fuels; apparatus Sampling of liquid petroleum products Sampling of pasty and solid petroleum products Determination of flashpoint of mineral oils and other combustible liquids by the Abel-Pensky closed cup method Determination of cone penetration of lubricating greases using a one-quarter cone Sampling of fuel gases, protective gases and exhaust gases Sampling of bituminous binders Petroleum products; lubricating grease; determination of cone
