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Analysis of Zirconium and Nickel Based Alloys and Zirconium Oxides

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Analysis of Zirconium and Nickel Based Alloys and Zirconium Oxides NET318_proof ■ 22 February 2017 ■ 1/7 Nuclear Engineering and Technology xxx (2017) 1e7 Available online at ScienceDirect 65 66 1 67 2 Nuclear Engineering and Technology 68 3 69 4 70 5 journal homepage: www.elsevier.com/locate/net 71 6 72 7 73 8 74 9 Original Article 75 10 76 11 Analysis of Zirconium and Nickel Based Alloys and 77 12 78 13 Zirconium Oxides by Relative and Internal 79 14 80 15 81 16 Monostandard Neutron Activation Analysis 82 17 83 18 Q1 Methods 84 19 85 20 * 86 21 a b, a,1 Q15 Q2Amol D. Shinde , R. Acharya , and A.V.R. Reddy 87 22 88 Q3 a Analytical Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085, India 23 89 b Radiochemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400 085, India 24 90 25 91 26 92 article info abstract 27 93 28 94 29 Article history: Background: The chemical characterization of metallic alloys and oxides is conventionally 95 30 Received 9 March 2016 carried out by wet chemical analytical methods and/or instrumental methods. Instru- 96 31 Received in revised form mental neutron activation analysis (INAA) is capable of analyzing samples nondestruc- 97 32 1 August 2016 tively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and 98 33 99 34 Accepted 19 September 2016 zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and Available online xxx oxides were also analyzed by inductively coupled plasma optical emission spectroscopy 100 35 101 (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance pur- 36 102 Keywords: poses. The samples are important in various fields including nuclear technology. 37 103 Methods: 38 AES Samples were neutron irradiated using nuclear reactors, and the radioactive assay 104 39 Chemical Quality Control was carried out using high-resolution gamma-ray spectrometry. Major to trace mass 105 40 IM-NAA fractions were determined using both relative and internal monostandard (IM) NAA 106 41 INAA methods as well as OES methods. 107 42 Nimonic alloy Results: In the case of alloys, compositional analyses as well as concentrations of some 108 43 Zircaloys trace elements were determined, whereas in the case of zirconium oxides, six trace ele- 109 44 Q4 Zirconium oxide ments were determined. For method validation, BCS-certified reference material 310/1 (a 110 45 nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. 111 46 112 Conclusion: The results showed that IM-NAA and relative INAA methods can be used for 47 113 nondestructive chemical quality control of alloys and oxide samples. 48 114 Copyright © 2017, Published by Elsevier Korea LLC on behalf of Korean Nuclear Society. This 49 115 50 is an open access article under the CC BY-NC-ND license (http://creativecommons.org/ 116 51 licenses/by-nc-nd/4.0/). 117 52 118 53 119 54 120 55 121 56 122 57 123 58 124 59 125 60 * Corresponding author. 126 61 E-mail addresses: [email protected], [email protected] (R. Acharya). 127 62 1 Present address: Department of Chemistry, Vikrama Shimhapuri University, Nellore, AP, India. 128 63 http://dx.doi.org/10.1016/j.net.2016.09.009 129 64 1738-5733/Copyright © 2017, Published by Elsevier Korea LLC on behalf of Korean Nuclear Society. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/). Please cite this article in press as: A.D. Shinde et al., Analysis of Zirconium and Nickel Based Alloys and Zirconium Oxides by Relative and Internal Monostandard Neutron Activation Analysis Methods, Nuclear Engineering and Technology (2017), http:// dx.doi.org/10.1016/j.net.2016.09.009 NET318_proof ■ 22 February 2017 ■ 2/7 2 Nuclear Engineering and Technology xxx (2017) 1e7 1 1. Introduction The IM-NAA method was successfully applied for the 66 2 standard-less analysis of nuclear reactor structural materials 67 3 68 The chemical characterization of materials is an important step such as zircaloys [7, 11] and stainless steels [7, 8, 12]. For 4 69 validation of the IM-NAA method, BCS certified reference Q5 5 in chemical quality control (CQC) exercises. It involves the 70 materials (CRMs) 225/1 (low alloy steel) and 466 (austenitic 6 determination of major, minor, and trace concentrations of 71 7 elements with good accuracy and precision. CQC helps in stainless steel) [8, 12, 13] were analyzed. Various analytical 72 8 ensuring the quality of the material as per the required speci- techniques have been used for the analysis of alloys and ox- 73 9 fications. In the case of nuclear reactor materials, the finished ides including NAA [14], prompt gamma-ray NAA [15, 16], XRF 74 10 products should meet the stringent chemical specifications for [17], spectroscopic methods such as ICP-OES [18e21], atomic 75 11 major to trace constituents for better performance of a nuclear absorption spectroscopy [22e26], and ICP-MS [27e29]. 76 12 reactor during its operation. The materials of interest are This research paper deals with the chemical character- 77 13 mainly nuclear reactor structural materials of alloy and oxide ization of zirconium and nickel based alloys by IM-NAA and 78 14 79 matrices. It is important to use suitable analytical techniques to compares results with conventional INAA and ICP-OES. 15 80 analyze these complex matrix samples to obtain good quality Samples in triplicate analyzed by INAA, IM-NAA, and ICP- 16 81 OES are nimonic alloys, Zircaloy 2, and Zircaloy 4. Zirconium 17 results. The routinely used analytical methods are mostly wet 82 18 chemical and spectroscopic techniques, such as atomic ab- oxide samples (four replicates) were analyzed by INAA and 83 19 sorption spectroscopy, inductively coupled plasma optical direct current Arc OES (DC Arc OES). This sample (zirconium 84 20 emission spectroscopy (ICP-OES), and ICP-mass spectrometry oxide) could not be analyzed by IM-NAA as the neutron flux 85 21 (ICP-MS), as well as chromatographic techniques. Although parameters (f and a) of irradiation position at Dhruva reactor 86 22 these techniques give high quality results, they are destructive are not available. In addition to the comparison of results with 87 23 methods and are associated with a cumbersome dissolution relative INAA and ICP-OES, a nimonic alloy CRMdBCS CRM 88 24 process that uses various acids. In some cases, radioanalytical 310/1dwas analyzed using IM-NAA as well as relative INAA 89 25 90 techniques such as X-ray fluorescence (XRF), instrumental methods. 26 91 neutron activation analysis (INAA), prompt gamma-ray NAA 27 92 (PGNAA), and ion beam analysis are used. Nuclear analytical 28 93 29 techniques, such as INAA and PGNAA, have several advantages. 2. Materials and methods 94 30 They are able to perform simultaneous multielement determi- 95 31 nation, are nondestructive in nature, have a negligible matrix 2.1. About the samples 96 32 effect, are highly sensitive and selective, and have achievable 97 33 high precision and accuracy. Different alloys are important in almost all fields of modern 98 34 Routine work using conventional INAA is mainly carried out science and technology. The elements Fe, Ni, Cr, Zr, Pb, and Ti 99 35 using the relative method, in which aprioriknowledge of the are the base materials for most of the alloys. High nickel alloys 100 36 101 constituents in a sample needs to be known. By contrast, k0- are used in the chemical, petrochemical, turbine, and aero- 37 102 based NAA uses a single comparator such as gold (197Au) or any space industries. High Ni alloys (having 50e80% Ni), such as 38 103 other suitable element that is coirradiated with the same 39 nimonic alloys, are used in the pressure lining of steam gen- 104 e 40 neutron flux along with the sample [1 3]. As the single erators and are also preferred over stainless steels as struc- 105 41 comparator is different to the element of interest, this method tural materials in fast nuclear reactors. Swelling under the 106 42 requires neutron spectrum parameters, namely, the epithermal prevailing irradiation conditions of high temperature is low 107 43 neutron flux shape factor (a) and the subcadmium to epi- for these alloys, and they are less prone to stress corrosion 108 44 thermal neutron flux ratio (f), absolute detection efficiency, and cracking. 109 45 the k0 factor [4, 5] for concentration calculations. In the case of Zirconium occurs in nature, mostly in the form of a silicate 110 46 111 k0-based internal monostandard NAA (IM-NAA), an element mineral known as zircon, which is extensively used in the 47 112 present in the sample, which is expected to be reasonably ho- glass and ceramic industries. Zirconium oxide (ZrO2, zirconia), 48 113 mogeneous, is used as the monostandard [6e8].IM-NAAusing prepared from zircon, is used as traditional and advanced 49 114 in situ relative detection efficiency [7, 8] is useful for the analysis ceramics and as a refractory material. It is used as a material 50 115 e 51 of small- as well as large-size (g kg scale) and nonstandard for machinery wear parts, insulations and coatings, and solid 116 52 geometry samples. The k0-NAA method was adapted in 1995 in electrolytes for fuel cells. It is also used as a raw material for 117 53 our laboratory. Later, in 2003, the IM-NAA in conjunction with in the preparation of various zirconium-based alloys. Zirconium 118 54 situ relative efficiency method was developed. The irradiation forms alloys with a variety of metals, such as Nb, Ni, Fe, Sn, 119 55 positions of APSARA [9] and KAMINI [10] reactors were char- and Cr.
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