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1、 Reference number ISO 10981:2004(E) ISO 2004 INTERNATIONAL STANDARD ISO 10981 Second edition 2004-06-15 Nuclear fuel technology Determination of uranium in reprocessing-plant dissolver solution Liquid chromatography method Technologie du combustible nuclaire Dosage de luranium dans les solutions de
2、dissolution des usines de retraitement Mthode par chromatographie en phase liquide Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without lice
3、nse from IHS -,-,- ISO 10981:2004(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing th
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6、at at the address given below. ISO 2004 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
7、 below or ISOs member 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.org Web www.iso.org Published in Switzerland ii ISO 2004 All rights reserved Copyright International Organization for St
8、andardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E) ISO 2004 All rights reserved iii Contents Page Forewordiv 1 Scope1 2 Normative references
9、 .1 3 Principle.1 4 Reagents2 5 Apparatus.2 6 Procedure.3 7 Expression of results3 8 Precision and accuracy4 9 Interferences4 Annex A (informative) Example of computer output from chromatography package 7 Copyright International Organization for Standardization Provided by IHS under license with ISO
10、 Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E) iv ISO 2004 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national stand
11、ards bodies (ISO member bodies). 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 orga
12、nizations, governmental and non-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
13、in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. 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
14、% of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 10981 was prepared by Technical Committee ISO/TC 85, Nucle
15、ar energy, Subcommittee SC 5, Nuclear fuel technology. This second edition cancels and replaces the first edition (ISO 10981:1993), which has been technically revised. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not fo
16、r Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 10981:2004(E) ISO 2004 All rights reserved 1 Nuclear fuel technology Determination of uranium in reprocessing-plant dissolver solution Liquid chromatography method 1 Sco
17、pe This International Standard specifies an analytical method for determining the uranium concentration between 0,1 g/l and 400 g/l in nitric acid solutions of irradiated fuel from light-water reactors, gas-cooled reactors and fast-breeder reactors. It specifies how interference by nitrite and pluto
18、nium ions is prevented. The other constituents of fuel solutions do not interfere. This method is suitable for process control, but not for accountancy purposes. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, on
19、ly the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 8299:1), Nuclear fuel technology Determination of isotopic content and elemental uranium and plutonium concentrations of nuclear materials in nitric acid soluti
20、ons Thermal-ionization mass spectrometry 3 Principle 3.1 The sample is diluted in aqueous ascorbic acid solution until the amount of free acid of the nitric solution injected onto the reversed-phase column is lower than 0,1 mol/l in HNO3 (1 99 %, spectrophotometric grade. 4.7 Mobile phase: solution
21、containing 5 103 mol/l cetyltrimethylammonium bromide (4.2) with 2 102 mol/l sodium hydrogen sulfate (4.3) and 0,18 mol/l ammonium sulfate (4.4) in an acetonitrile (4.1) water mixture (25 % to 75 % in volume); degassed and with 0,1 % in volume of the trifluoroacetic acid solution (4.6) added before
22、use. 4.8 Uranium reference solutions, at concentrations as close as possible to the concentration of the test sample, containing typically 0,1 g/l to 400 g/l of uranium prepared from certified reference materials. 5 Apparatus 5.1 Usual laboratory equipment, found in a high-activity laboratory analys
23、ing solutions containing uranium, plutonium and fission products. 5.2 Polytetrafluoroethylene (PTFE) filters, with a porosity of 0,22 m. 5.3 Chromatographic unit, comprising (see Figure 1): a high pressure chromatographic pump; a four-port injection valve with an internal loop of 1 l; a chromatograp
24、hic precolumn with a 3 cm length and a 4,6 mm inside diameter; a chromatographic column with a 10 cm length and a 4,6 mm inside diameter; Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56
25、MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E) ISO 2004 All rights reserved 3 NOTE A precolumn avoids changing the whole analytical column in the case of clogging. a spectrophotometric detector, capable of operation at a wavelength, , of 254 nm; an automa
26、tic calculator/integrator; a system for transferring the prepared sample to the chromatographic valve. 6 Procedure 6.1 Calibration 6.1.1 Use at least two uranium reference solutions (4.8) at concentrations bracketing those of the samples to be analysed. 6.1.2 Aliquot 2 ml of the first uranium refere
27、nce solution into a 100 ml calibrated flask. NOTE With an automatic diluter, the volume of the sample and thus the volume of the wastes can be reduced (for example, 0,5 ml in 25 ml). 6.1.3 Dilute to 100 ml with ascorbic acid solution (4.5) and homogenize. 6.1.4 Inject 1 l of the diluted reference so
28、lution into the sampling loop. 6.1.5 Elute with the mobile phase reagent (4.7) at a 1 ml/min flow rate. The retention time of uranium is approximately 5 min. It is completely eluted after about 8 min. 6.1.6 Measure the peak areas by means of the integrator. 6.1.7 After each analysis, rinse the sampl
29、ing line with a dilute nitric acid solution (0,1 mol/l for example) to avoid cross contamination or crystallisation by evaporation of the remaining sample. 6.1.8 Repeat operations 6.1.2 to 6.1.7 with the other reference solution(s). 6.2 Analysis of the sample 6.2.1 Treatment of the sample Filter the
30、 test sample by means of a PTFE filter (5.2); then aliquot 2 ml of this solution into a 100 ml calibrated flask. Dilute to 100 ml with the ascorbic acid solution (4.5) and homogenize. 6.2.2 Chromatographic measurement Inject 1 l of the diluted sample into the sampling loop and then proceed with step
31、s 6.1.5 to 6.1.7. 7 Expression of results Calculate the uranium concentration from the measured peak area using a linear interpolation. The low concentration standard should be not less than 95 % of the high concentration standard. Copyright International Organization for Standardization Provided by
32、 IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E) 4 ISO 2004 All rights reserved 8 Precision and accuracy 8.1 General The following estimates of the performance of
33、the procedure are based on the statistical evaluation of duplicate analyses performed on about 200 batches of dissolver solutions from light-water reactor fuel irradiated from 20 000 to 35 000 MWd/t and 45 batches of dissolver solutions of gas-cooled reactor fuel irradiated at 5 500 MWd/t. 8.2 Repea
34、tability The coefficient of variation (including all steps of Clause 6) is of the order of 0,4 % to 0,6 % at concentrations of 200 g/l of uranium and using the appropriate integration range. The use of an automatic diluter improves this coefficient of variation to 0,2 %. 8.3 Systematic errors The me
35、an of duplicate results obtained by this method differed by 0,1 % to + 0,4 % from the mean of duplicate results obtained by isotopic dilution mass spectrometry in accordance with ISO 8299. The coefficient of variation of the systematic error is of the order of 0,4 % or less. It is recommended that e
36、valuation of errors has to be done by users for each specific situation. 9 Interferences 9.1 Plutonium Plutonium (III) does not interfere. Plutonium (IV) and (VI) may adversely affect the uranium peak when the U/Pu ratio is less than 100. However, the ascorbic acid solution (4.5) used for the diluti
37、on steps 6.1.3 and 6.2.1, reduces plutonium to its trivalent state at room temperature. This species does not interfere. This procedure is suitable for use on one-month-aged PUREX solutions. On longer aged solutions, the amount of ascorbic acid added should be increased. 9.2 Fission Products (FP) an
38、d other elements The elements given in Table 1, which are present in an actual FP concentrate solution, do not affect the base line in the region of interest of the spectrum when present in concentrations less than those specified. 9.3 Nitrite anions Nitrite anions interfere if they are present. How
39、ever, the ascorbic acid solution (4.5) used for the dilution in steps 6.1.3 and 6.2.1 reduces the nitrite ions and prevents any interferences. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:4
40、7:56 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E) ISO 2004 All rights reserved 5 Table 1 Elements Concentration g/l Elements Concentration g/l B P Na Mg Ca Fe Cr Ni Mn Cu Al 0,1 0,1 22,0 5,0 0,1 10,2 0,1 2,2 10,5 0,2 40,0 Ba Mo Ce Rh Zr La Sr Pr Nd Ru G
41、d 0,7 1,9 0,2 0,3 4,0 1,0 0,1 1,1 1,7 0,3 0,1 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E)
42、6 ISO 2004 All rights reserved Key 1 mobile phase 9 pressurized water 2 sample 10 3 cm precolumn 3 chromatographic pump 11 10 cm long column 4 injection valve with 1 l sampling loop 12 UV detector 5 separator 13 integrator 6 venturi 14 waste 7 waste 15 mobile phase pipes 8 waste 16 sample pipes Figu
43、re 1 Chromatographic unit flow-sheet Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E) ISO 2004
44、All rights reserved 7 Annex A (informative) Example of computer output from chromatography package Figure A.1 Example of a uranium concentration determination using a computer-based chromatograhy package Copyright International Organization for Standardization Provided by IHS under license with ISO
45、Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10981:2004(E) ICS 27.120.30 Price based on 7 pages ISO 2004 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 02:47:56 MDTNo reproduction or networking permitted without license from IHS -,-,-