ISO-13464-1998.pdf
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1、A Reference number ISO 13464:1998(E) INTERNATIONAL STANDARD ISO 13464 First edition 1998-04-01 Simultaneous determination of uranium and plutonium in dissolver solutions from reprocessing plants Combined method using K-absorption edge and X-ray fluorescence spectrometry Dosage simultan de luranium e
2、t du plutonium dans les solutions de dissolution des usines de retraitement Mthode combine de spectromtrie dabsorptiomtrie K et de fluorescence X Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Res
3、ale, 04/20/2007 06:26:25 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 13464:1998(E) ISO 1998 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 ph
4、otocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case postale 56 CH-1211 Genve 20 Switzerland Internetcentraliso.ch X.400c=ch; a=400net; p=iso; o=isocs; s=central Printed in Switzerland ii Contents 1 Scope1 2 Principle1 3 Appa
5、ratus.1 4 Operating procedure .5 5 Method of calculation6 6 Calibration8 7 Bias correction factors10 8 Measurement uncertainty .11 Annex A (informative) Bibliography 13 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1
6、/9972545001 Not for Resale, 04/20/2007 06:26:25 MDTNo reproduction or networking permitted without license from IHS -,-,- ISOISO 13464:1998(E) iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of
7、 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-governmental
8、, 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. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. P
9、ublication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard ISO 13464 was prepared by Technical Committee ISO/TC 85, Nuclear energy, Subcommittee 5, Nuclear fuel technology. Annex A of this International Standard is for infor
10、mation only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/20/2007 06:26:25 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organizati
11、on for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/20/2007 06:26:25 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISOISO 13464:1998(E) 1 Simultaneous determination of urani
12、um and plutonium in dissolver solutions from reprocessing plants Combined method using K-absorption edge and X-ray fluorescence spectrometry 1 Scope This International Standard specifies a nondestructive method for the simultaneous determination of volumetric uranium and plutonium concentrations in
13、nitric acid feed solutions from reprocessing plants. The method is directly applicable, without interference, to the original feed solution, which typically contains about 150 gl-1 to 300 gl-1 uranium and 1 gl-1 to 2,5 gl-1 plutonium in the presence of fission products with a total ,-activity of up
14、to 10 TBql-1. 2 Principle A sample vial containing about 3 ml to 5 ml of the feed solution is irradiated with a suitably filtered X-ray continuum from an X-ray tube. The X-ray continuum must include X-ray energies up to about 150 keV, and the maximum of its intensity distribution should occur at an
15、energy above 100 keV. The attenuation of a highly collimated X-ray beam, crossing a well-defined pathlength of solution in the vial, is measured with a HPGe detector below and above the K-absorption edge energy of uranium (EK = 115,6 keV). The underlying K-edge densitometry (KED) method determines t
16、he uranium concentration from the abrupt change of the photon attenuation across the K-absorption edge. At the same time a second HPGe detector, viewing a larger portion of the sample, measures the intensity ratio of fluoresced K1 X-rays from uranium and plutonium. This X-ray fluorescence (XRF) meas
17、urement determines the U/Pu element ratio. The plutonium concentration is calculated from the measured values for the uranium concentration and the U/Pu ratio. The advantage of this XRF method arises from the fact that it is totally based on intensity ratio measurements. Further details on the measu
18、rement principle can be found in 1. 3 Apparatus 3.1 Components 3.1.1 Advanced standard spectroscopy equipment for high-resolution gamma spectroscopy including two HPGe detectors, electronics for fast pulse processing, and a computer-based multichannel analyzer for spectrum acquisition and evaluation
19、. 3.1.2 X-ray equipment with X-ray tube, high voltage power supply, operating console and a circuit for water cooling. 3.1.3 Mechanics including beam collimators, shielding materials, adjustment device for the X-ray tube, and a system for transferring the sample into a defined position in the spectr
20、ometer. A block diagram of the instrument components is shown in figure 1. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/20/2007 06:26:25 MDTNo reproduction or networking permitted wit
21、hout license from IHS -,-,- ISO 13464:1998(E) ISO 2 Key: 1X-ray tube7Main amplifier 2H.V. generator8ADC 3Water cooling9Ratemeter 4HPGe detecto XRF10Stabilizer 5HPGe detector K-edge11MCA and PC system 6H.V. Figure 1 Block diagram of the instrument components 3.2 Geometric arrangement The geometric ar
22、rangement (see figure 2) shall satisfy three basic requirements: a) The distance D between X-ray tube and sample shall be kept as short as technically feasible (D 6,5 cm) in order to achieve the highest possible flux of X-rays from the tube at the sample position (integrated flux of X-rays with ener
23、gies from 115 keV to 150 keV 5 1010 photonscm-2s-1). b) The angle between primary X-ray beam and collimator axis directed towards the XRF detector shall take values 150 in order to shift inelastically scattered radiation out of the energy region of analysis in the XRF spectrum. c) The solid angle su
24、btended by the collimator between sample and K-edge detector shall be limited to values 10 4Filter (Cd), d ; 0,111Containment of sample transfer system 5Collimator (W)12Sample conveyor 6Filter (Fe), d ; 213Shielding 7Collimator (W) L 1014Window of containment of sample transfer system; for XRF measu
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