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1、Reference number ISO 15597:2001(E) ISO 2001 INTERNATIONAL STANDARD ISO 15597 First edition 2001-02-15 Petroleum and related products Determination of chlorine and bromine content Wavelength-dispersive X-ray fluorescence spectrometry Produits ptroliers et produits connexes Dosage du chlore et du brom
2、e Spectromtrie par fluorescence X dispersive en longueur donde Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:48:21 MDTNo reproduction or networking permitted without license from IHS -,-,- I
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6、ven below. ISO 2001 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs membe
7、r body in the country of the requester. ISO copyright office Case postale 56 ? CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2001 All rights reserved Copyright International Organization for Standardization Provided
8、 by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:48:21 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15597:2001(E) ISO 2001 All rights reservediii ContentsPage Foreword.iv 1Scope 1 2Normative references1 3Principle1 4Reagents
9、and materials 2 5Apparatus.2 6Samples and sampling3 7Calibration solutions.3 8Calibration4 9Procedure.6 10Calculation6 11Expression of results 6 12Precision.6 13Test report7 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100
10、Not for Resale, 04/23/2007 08:48:21 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15597:2001(E) iv ISO 2001 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies)
11、. The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non
12、-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part
13、 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of th
14、is International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 15597 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants. Copyright International Organization for
15、Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:48:21 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 15597:2001(E) ISO 2001 All rights reserved1 Petroleum and related products Dete
16、rmination of chlorine and bromine content Wavelength-dispersive X-ray fluorescence spectrometry WARNING The use of this International Standard may involve hazardous materials, operations and equipment. This International Standard does not purport to address all of the safety problems associated with
17、 its use. It is the responsibility of the user of this International Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1Scope This International Standard specifies a method for the determination of the chlorine and b
18、romine content of liquid petroleum products, synthetic oils and fluids, and additives for petroleum products (including used oils) that are soluble in organic solvents of negligible or accurately known chlorine/bromine content. The method is applicable to products or additives having chlorine conten
19、ts in the range 0,0005 % (m/m) to 0,1000 % (m/m), and bromine contents in the range 0,0010 % (m/m) to 0,1000 % (m/m). Other elements do not generally interfere, although lead may interfere at contents above 0,1500 % (m/m) (see note 2). NOTE 1For the purposes of this International Standard, the term
20、“% (m/m)” is used to represent the mass fraction of a material. NOTE 2Used lubricants may pose particular problems due to the range of potentially interfering elements at relatively high concentrations. For used lubricants generally, the lower limit of sensitivity may be 0,0050 % (m/m) even when the
21、 provisions of the last paragraph of 9.3 are applied. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
22、publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred
23、to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3170:1988, Petroleum liquids Manual sampling. ISO 3171:1988, Petroleum liquids Automatic pipeline sampling. ISO 4259:1992, Petroleum products Determination and application of precision data in relat
24、ion to methods of test. 3Principle The test portion and a bismuth solution as internal standard are mixed in a given mass ratio and exposed, in a sample cell, to the primary radiation of an X-ray tube. Copyright International Organization for Standardization Provided by IHS under license with ISO Li
25、censee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:48:21 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15597:2001(E) 2 ISO 2001 All rights reserved The count rates of the chlorine K? at 0,4729 nm and bismuth M? at 0,4909 nm, or bromine K? at 0,104 1 nm and bism
26、uth L? at 0,114 4 nm fluorescence thus excited, and the count rate of the background radiation at 0,480 7 nm or 0,108 5 nm, are measured, and the ratio of these net count rates is calculated. The chlorine and/or bromine content of the sample is determined from calibration curves prepared on the basi
27、s of chlorine and/or bromine calibration standards. 4Reagents and materials 4.1White oil (light paraffin oil), high purity grade, sulfur content 1 mg/kg maximum. 4.2Chlorine compound, 1-chlorooctane or another oil-soluble chlorine compound of accurately known chlorine content, used for the preparati
28、on of the primary standards. The chlorine content shall be accurately known to the nearest 0,01 % (m/m). 4.3Bromine compound, 1,1,2,2-tetrabromoethane or another oil-soluble bromine compound of accurately known bromine content, used for the preparation of the primary standards. The bromine content s
29、hall be accurately known to the nearest 0,01 % (m/m). CAUTION 1,1,2,2-tetrabromoethane is extremely toxic by inhalation and ingestion. Appropriate precautions for the handling operations of opening the container and weighing shall be followed. 4.4Certified reference materials, obtained from a nation
30、al standards body or accredited supplier with a range of certified chlorine and/or bromine contents for the production of calibration curves for routine analysis. 4.5Bismuth compound, triphenylbismuth, of minimum purity 98 %. 4.62-ethylhexanoic acid, of minimum purity 98 %. 5Apparatus 5.1Wavelength-
31、dispersive X-ray fluorescence spectrometer, any suitable spectrometer that allows the count rates of the Cl-K?, Br-K?, Bi-M? and Bi-L? X-ray fluorescence to be measured, provided that the design incorporates the general features given in Table 1. It shall be set up according to the manufacturers ins
32、tructions. Table 1 General requirements of the spectrometer ComponentRequirement AnodeRhodium, scandium, chromium, or any other tube anode that allows the counting times to be adjusted to achieve the required precision Collimator (if used)Coarse for chlorine, narrow for bromine Analysing crystalGerm
33、anium for chlorine, lithium fluoride (LiF) for bromine, or any other crystal suitable for the required dispersion of the wavelengths in Table 2 within the angular range of the spectrometer Optical pathHelium Cell windowPolyester or polypropylene film, chlorine- and bromine-free, thickness 2 ?m to 6
34、?m DetectorProportional counter with pulse-height analyser. For bromine, a scintillation counter with pulse- height analyser is preferred 5.2Analytical balance, capable of weighing accurately to the nearest 0,1 mg. 5.3Homogenizer, of the non-aerating, high-speed shear type, or heatable magnetic or u
35、ltrasonic stirrer. 5.4Filters, of sintered glass, with a pore size of 10 ?m to 60 ?m. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:48:21 MDTNo reproduction or networking permitted without l
36、icense from IHS -,-,- ISO 15597:2001(E) ISO 2001 All rights reserved3 5.5Flasks, of 25 ml to 100 ml capacity, narrow-necked, conical, made of borosilicate glass, and fitted with ground-glass stoppers. 6Samples and sampling 6.1Unless otherwise specified, samples shall be taken in accordance with the
37、procedures specified in ISO 3170 or ISO 3171. 6.2Test portions from the samples shall be drawn after thorough mixing and subdivision. Heat viscous samples to a temperature which renders the sample fluid, and homogenize, using the homogenizer or stirrer (5.3) as necessary. NOTEFor the purpose of this
38、 procedure, the term “sample” includes solutions prepared from additives, semi-solid or solid petroleum products that have been appropriately pre-treated and/or diluted. 7Calibration solutions 7.1General Use either certified reference materials (4.4) or primary standards prepared from chlorine compo
39、unds (4.2) and/or bromine compounds (4.3) dissolved in white oil (4.1) as a basis for the preparation of the appropriate range of stock solutions. 7.2Preparation of stock solutions 7.2.1Chlorine and bromine stock solutions Weigh, to the nearest 0,1 mg, a quantity of chlorine compound (4.2) or bromin
40、e compound (4.3) to prepare stock solutions of approximately 0,10 % by mass of chlorine or bromine, calculated to the nearest 0,001 % (m/m), and dissolve in white oil (4.1) at room temperature. Mix the contents thoroughly using a homogenizer (5.3), and store in a glass-stoppered flask (5.5). It is r
41、ecommended that a polytetrafluorethylene (PTFE) or glass-coated magnetic stirrer and stirring device be used to mix the contents of the flask. Calculate the exact chlorine and/or bromine content, w2, in percent by mass, to three decimal places, in each case from the amounts of white oil and compound
42、 used as follows: c1 2 c0 mw w mm ? ? ? (1) where mcis the mass of the chlorine or bromine compound, expressed in grams; w1is the chlorine or bromine content of the compound, expressed in percent by mass; m0is the mass of white oil, expressed in grams. 7.2.2Bismuth solution Weigh, to the nearest 0,1
43、 mg, a quantity of triphenylbismuth (4.5) sufficient to make a 1 % by mass solution in white oil. Dissolve the triphenylbismuth in white oil by stirring and warming to a temperature not exceeding 80 ?C. Add 5 % (m/m) 2-ethylhexanoic acid (4.6) to the solution. Remove any residual turbidity by filter
44、ing the gently heated mixture through the filter (5.4). Store in a tightly stoppered flask or bottle. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 08:48:21 MDTNo reproduction or networking per
45、mitted without license from IHS -,-,- ISO 15597:2001(E) 4 ISO 2001 All rights reserved When protected against moisture, the bismuth solution can be kept for several months. Any turbidity should be taken as an indication that the solution is no longer suitable for use. 7.3Preparation of standard solu
46、tions Preparestandardsolutionsofchlorineand/orbrominecontentsof0,000 5 % (m/m),0,001 0 % (m/m), 0,002 0 % (m/m), 0,005 0 % (m/m), 0,010 0 % (m/m), 0,025 0 % (m/m) and 0,050 0 % (m/m) from the stock solutions (7.2.1), by weighing, to the nearest 0,1 mg, a quantity of the stock solution to produce app
47、roximately 25 g of standard solution, into a flask (5.5), and diluting this with white oil (4.1). Reweigh to the nearest 0,1 mg and mix thoroughly at room temperature. Calculate the content of chlorine or bromine, w3, in percent by mass, in each solution to the nearest 0,000 01 % (m/m) by means of e
48、quation (2) below. Transfer the solutions to tightly stoppered dark glass bottles with the content recorded on each bottle. ? 221 3 31 wmm w mm ? ? ? (2) where m1is the mass of the flask, expressed in grams; m2is the mass of the flask plus stock solution, expressed in grams; m3is the mass of the flask plus stock solution plus white oil, expressed in grams. 7.4Preparation of calibration solutions Weigh a series of flasks (5.5) and add a quantity of each standard solution (7.3) to separate flasks. Also add a quantity of each stoc