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1、INTERNATIONAL STANDARD ISO 9030 First edi tion 1990-12-15 - - -_-_- Crude petroleum - Determination of water and Sediment - Centrifuge method Petrole brut - Determination de la tenecrr en eau et en Sediments - Methode par centrifugation Reference number ISO 9030: 199O(E) Copyright International Orga
2、nization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 22:05:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 90303 990(E) Foreword ISO (the International Organization for Standardi
3、zation) is a worldwide federation of national Standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Esch member body interested in a subject for which a technical committee has been established has the right to b
4、e represented on that committee. International organizations, govern- mental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matter-s of electrotechnical standardization. Draft Internation
5、al Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Interna- tional Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard ISO 9030 was prepared by Technical Committee ISO/TC 28, Petroleum
6、 products and lubricanfs. Annexes A and 6 form an integral part of this International Standard. 0 ISO 1990 All rights reserved. No part of this publication may be reproduced or utilized in any form or by any means, electronie or mechanical, including photocopying and microfilm, without Permission in
7、 writing from the publisher. International Organization for Standardization Case Postale 56 l CH-121 1 Geneve 20 l Switzerland Printed in Switzerland - ii Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 No
8、t for Resale, 04/23/2007 22:05:10 MDTNo reproduction or networking permitted without license from IHS -,-,- - _-.- INTERNATIONAL STANDARD ISO 9030:1990(E) Crude Petroleum - Determination of vvater and Sediment - Centrifuge method WARMING - The use of this International Standard may involve hatardous
9、 materials, operations and eqwipment. Chis Standard does nst purpsrt to address all of the safety prablems associated with its use. it is the responsibility sf the user od this standard to establish apprspriate safety and health practices and determine the applicability sf regwlatsry Bimitatisns Pri
10、or to use. 1 Scope This International Standard specifies a method for the Iaboratory determination of water and Sediment in crude oils by means of a centrifuge procedure. The precision data have only been determined for water contents up to 1 % (V/v). NOTE 1 lt has been obset-ved that centrifugal me
11、thods of determination of watet- and Sediment may, in many cases, give erroneous results. This is especially so when use of a high-speed mixer has been employed to obtain a representative Sample. The method is therefore not en- tirely satisfactory and the amount of water determined is almost always
12、lower than the actual water content. 2 Normative references The foilowing Standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publi- cation, the editions indicated were valid. All stan- dards are subject to revision
13、, and Parties to agreements based on this International Standard at-e encouraged to investigate the possibility of ap- plying the most recent editions of the Standards in- dicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 3170:1988, Petroleum li
14、quids - Manual sampling. ISO 3171:1988, Petroleum liquids - Automatic pipe- line sampling. ISO 4787:1984, Laboratory glassware - Volumetric glassware - Methods for use and testing of capacity. ISO 5272:1979, Toluene for industrial use - Specifi- cafions. ISO 9029:1990, Crude petroleum - Determinatio
15、n of Water - Distillafion method. 3 Significance A knowledge of the water content of crude oil is im- portant in the refining, purchase, sale and transfer of products. The amount of watet- as determined by this method is used to correct the volume involved in the custody transfer of Oil. 4 Principle
16、 Equal volumes of crude oil and water-saturated toluene are placed in a cone-shaped centrifuge tube- After centrifugation, the volume of the higher-density water and Sediment layer at the bottom of the tube is read. 5 Apparatus Usual laboratory apparatus, together with the fol- lowing: 5.1 Centrifug
17、e. 5.1.1 The centrifuge shall be capable of spinning two or more filled, cone-shaped 203 mm centrifuge tubes at a Speed that tan be controlled to give a relative centrifugal forte (rcf) of a least 600 at the tip of the tubes (see 5.1.5). 1 Copyright International Organization for Standardization Pro
18、vided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 22:05:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 9030: 199O(E) 5.1.2 The revolving head, trunnion rings and trunnion cups, including the cushions, shall
19、 be soundly constructed to withstand the maximum centrifugal forte capable of being delivered by the power Source. The trunnion cups and cushions shall firmly support the tubes when the centrifuge is in motion. The centrifuge shall be enclosed in a metal shield or case strong enough to eliminate dan
20、ger if any breakage occurs. 51.3 The centrifuge shall be heated so that the Sample temperature tan be maintained at 60 “C + 3 “C during the entire run (see 8.7). If a thermoitatic control is provided, it shall be capable of maintaining the temperature within these limits and operate safely if there
21、is a flammable atmos- phere. 5.1.4 Electric-powered and heated centrifuges shall meet all safety requirements for use in hazardous areas. 5.1.5 The necessary minimum Speed of the rotating head in revolutions per minute (rpm) is caiculated as foiiows: rpm = 1335 J 5 where rcf is the relative centrifu
22、gai forte; d is the diameter of Swing, in millimetres, measured between the tips of opposite tubes when in the rotating Position. 5.2 Centrifuge tubes. 5.2.1 Esch centrifugai tube shail be a 203 mm cone-shaped tube, conforming to the dimensions given in figure 1 and made of thoroughly annealed glass
23、. The graduations, numbered as shown in fig- ure 1, shall be clear and distinct, and the mouth shall be constricted in shape for closure with a cork. Scale-error tolerantes and the smallest graduations between various calibration marks are given in tabie 1 and apply to calibration made with air-free
24、 water at 20 OC, when reading the bottom of the meniscus. 5.3 Bath. The bath shall be either a solid-metai-block bath or a liquid bath of sufficient depth for immersing the centrifuge tube in the vertical Position to the 100 ml mark. Means shali be provided for maintaining the temperature at 60 “C +
25、 3 “C. - NOTE 2 By agreement between Parties, a temperature of 49 OC + 3 C may be used, but the precision achieved may not be the precision indicated in this International Standard. 6 Reagents 6.1 Toluene, conforming with the requirements for grade 1 toiuene as specified in ISO 5272. The solvent sha
26、ll be water-saturated at 60 “C + 3 “C (see note) but shali be free of sus- pended-water (see annex B for the solvent/water Saturation procedure). NOTE 3 By agreement between Parties, a temperature of 49 OC 0,03 0,05 0,05 + + 0,lO T T 0,lO T 0,20 T 0,50 7 l,oo - l,oo Table 2 - Expression of results V
27、olume of water and Sediment in tube 1 Volume of water and Sediment in tube 2 Total percentage of water and Sediment ml ml Yxl ( v/ v) No visible water and Sediment No visible water and sedimeot 0 No visible water and Sediment 0,025 0,025 0,025 0,025 0,025 0,05 0,05 0,05 0,075 0,05 0,05 0,lO 0,075 0,
28、075 0,125 0,075 0,075 0,15 0,lO 0,lO 0,175 OJO 0,lO 0,20 0,15 0,25 10 Precision The precision of this method as obtained by statis- tical examination of inter-laboratory test results is as follows: 10.1 Repeatability The differente between successive test results ob- tained by the Same Operator with
29、 the Same appara- tus under constant operating conditions on identical test material would, in the long run, in the normal and correct Operation of the test method, exceed the following values in only one case in twenty: from 0,O % (V/v) to 0,3 % (V/V) water and Sediment: see figure 3; from 0,3 % (V
30、/v) to 1,0 % (V/V) watet- and Sediment: OJ2 % (V/v). would, in the long run, in the normal and correct Operation of the test method, exceed the following values in only one case in twenty: from 0,O % (V/v) to 0,3 % (V/ r/) water and Sediment: see figure 3; from 0,3 % (V/V) to 1,O % (V/P) water and S
31、ediment: 0,28 % (V/ 13. 11 Test report The test report shall contain at least the following information: a) all details necessary for the identification of the product tested; b) a reference to this International Standard; c) the result of the test (see clause 9); 10.2 Reproducibility The differente
32、 between two Single and independent results obtained by different Operators working in different Iaboratories on identical test material d) any deviation, by agreement or otherwise, from the procedure specified; e) the date of the test- Copyright International Organization for Standardization Provid
33、ed by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 22:05:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 9030:1990(E) OC bC I 50 37,75 36 Dimensions in millimetres Internal diameter + Extemal diameter Level of i
34、nside bottom LA Inside-taper shape Figure ? - 203 mm centrifuge tube Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 22:05:10 MDTNo reproduction or networking permitted without l
35、icense from IHS -,-,- ISO 9030:1990(E) - - 4 l - - - - - - - - .- - _- - - -_ - - - i/ - -_ - -4 - 4 mL J - -_ _. -j-.-j- 45 ,nL Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 2
36、2:05:10 MDTNo reproduction or networking permitted without license from IHS -,-,- g On3 c 0 s L. z !i 2 02 * 2 t!i Ei 6 z Cl 01 , 0 ISO 9030:199O(E) I 1 1 1 1 1 0,05 01 , 0,15 02 , 0,25 03 I Average water content, % (V/ V) Figure 3 - Precision of Che method for water and Sediment contents within the
37、 range 0,O % (V/Vj to 0,3 % (V/v) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/23/2007 22:05:10 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 9030:199O
38、(E) Annex A (normative) Sample kandling NOTE 7 This annex reproduces the instructions on Sample handling from ISO 3170:1988 and ISO 3171: 1988 and is essentially identical with the corresponding clauses therein. A.l General A.1.1 The method of handling sampies between the Point at which they are ext
39、racted or drawn, and the Iaboratory test bench or Sample storage are de- vised to ensure that the nature and integrity of the Sample are maintained. A.1.2 The method of handling a Sample will de- pend on the purpose for which it has been taken. The laboratory analytical procedure to be used will oft
40、en require a special handling procedure to be associated with it. For this reason, consult the ap- propriate methods of test so that any nccessary in- structions as to Sample handling tan be given to the person drawing the Sample. If the analytical proce- dures to be applied have conflicting require
41、ments, then draw separate samples and apply the appro- priate procedure to each Sample. A.1.3 Take particular care in respect of the follow- ing: a) liquids containing volatile material, since loss by evaporation tan occur; b) liquids containing water and/or Sediment, since Separation tends to occur
42、 in the Sample con- tainer; c) liquids with potential wax deposition, since de- Position tan occur if a sufficient temperature is not maintained. A-l.4 When making up composite samples, take great care not to lose light ends from volatile liquids and not to alter water and Sediment content. This is
43、a very difficult Operation and should be avoided if at all possible. A.1.5 DO not transfer samples of volatile liquids to other Containers at the sampling location but trans- port them to the laboratory in the original Sample Container, cooled and inverted, if necessary. Great care is necessary if a
44、 Sample contains both volatile components and free water. 8 A.2 Homogenization of samples A.2.1 Introduction Procedures are specified for the homogenization sf samples that may contain water and Sediment, or are in any other way non-uniform, before transfet from the Sample Container to smaller Conta
45、iners or into laboratory test apparatus Procedures for veri- fying that the Sample is satisfactorily mixed before transfer are given in clause A.3. lt is not possible to agitate manually small samples of Iiquids containing water and Sediment sufficiently to disperse the water and Sediment within the
46、 sam- ple. Vigorous mechanical or hydraulic mixing is necessary in Order to homogenize the Sample Prior to transfer or sub-sampling. Homogenization may be by various methods. Whichever method is used, it is recommended that the homogenizing System produces water dr-oplets below 50 iln-l, but not les
47、s %han i Ilrn. Water droplets sf below 1 p-l will give a stable emulsion and the water content cannot then be detet-mined by centrifuge methods. A.2.2 Homogenization lby high-shear mechanical mixer Insert a high-shear mechanical mixer into the sam- ple Container so that the rotating element reaches
48、to within 30 mm of the bottom. A mixer with counter-rotating blades operating at about 3 000 min-1 is usually suitable. Other designs may be used if the Performance is satisfactory. In Order to minimize loss of light ends from crude oils or other samples containing volatile com- pounds, operate the stirrer through a gland in the closure of the Sample Container. Mix until the sam- ple is completely homogenized. A mixing time of 5 min is sometimes sufficient, but the size of the Container and the nature of the Sample affect the homogenization time. Verify tha