scispace - formally typeset
Search or ask a question
Journal Article•DOI•

A comparative study using liquid scintillation counting to determine 63Ni in low and intermediate level radioactive waste

Céline Gautier, Christèle Colin, Cécile Garcia
01 Apr 2016-Journal of Radioanalytical and Nuclear Chemistry (Springer Netherlands)-Vol. 308, Iss: 1, pp 261-270
TL;DR: In this paper, a comparative study using liquid scintillation counting was performed to measure 63Ni in low and intermediate level radioactive waste, three DMG-based radiochemical procedures (solvent extraction, precipitation, extraction chromatography) were investigated, the solvent extraction method being considered as the reference method.
Abstract: A comparative study using liquid scintillation counting was performed to measure 63Ni in low and intermediate level radioactive waste. Three dimethylglyoxime (DMG)-based radiochemical procedures (solvent extraction, precipitation, extraction chromatography) were investigated, the solvent extraction method being considered as the reference method. Theoretical speciation calculations enabled to better understand the chemical reactions involved in the three protocols and to optimize them. In comparison to the method based on DMG precipitation, the method based on extraction chromatography allowed to achieve the best results in one single step in term of recovery yield and accuracy for various samples.

Summary (3 min read)

Jump to: [Introduction] – [Reagents and equipments] – [Sample preparation and digestion] – [Method 1 based on the organic extraction of the Ni(DMG) 2 complex] – [Method 2 based on the precipitation of the Ni(DMG) 2 complex] – [Method 3 based on the precipitation of the Ni(DMG) 2 complex on Ni resin] – [Speciation studies] – [Applications of the three DMG-based radiochemical methods to real nuclear waste samples] and [Where]

Introduction

  • In France, the National Radioactive Waste Management Agency is in charge of the long-term management of all radioactive waste.
  • Several repository sites have been built in order to accommodate nuclear waste packages.
  • Elimination of the interfering elements is mainly achieved with ammonium citrate during the rinsing step.

Reagents and equipments

  • All chemicals (nitric acid, hydrochloric acid, hydrofluoric acid, hydroiodic acid, ammonium hydroxide, hydrogen peroxide, citrate ammonium, sodium citrate, tartaric acid, 2-nitroso-1-naphthol, dimethylglyoxime) were of analytical grade.
  • Ultra-pure water (resistivity 18.2 M cm) was obtained from a Milli-Q purification system (Millipore, France).
  • Anion-exchange resin AG1-X4 (50-100 mesh) was supplied by Bio-Rad Laboratories .
  • All measurements of gamma emitting radionuclides were completed using a high purity germanium detector (Canberra, ) which was calibrated with a multi gamma standard (9ML01ELME20) supplied by CERCA LEA .
  • The uncertainties of the 63 Ni activities concentrations were calculated according to the standard NF M60-317 [21] by combining the uncertainties associated with the quantities of digested samples, the standards, the recovery yields and the LSC measurements.

Sample preparation and digestion

  • The different radioactive samples were collected in several French nuclear facilities and laboratories.
  • They consisted of the following types of materials: evaporate concentrates, steels, muds embedded in concretes, effluents, ion exchange resins embedded or not in polymers and graphites (denoted from S1 to S8 in this work).
  • All samples were digested using a microwave acid digestion system (Speed Wave, Berghof, Germany), except graphites.
  • The resulting solutions were transferred to 100 mL volumetric flasks and diluted with ultra-pure water.
  • As examples, the chemical and radiochemical compositions of two studied samples (S1 and S2) are detailed in Table 1 .

Method 1 based on the organic extraction of the Ni(DMG) 2 complex

  • Aliquots of the digested samples were first weighed in a beaker.
  • As the reaction between Co and 2-nitroso-1-naphthol proceeds rather slowly [34] , the solutions were allowed to stand for about 30 min.
  • 3x10 mL of chloroform were then added to extract the Co-nitrosonaphtol complex in the organic phases whereas Ni remained in the aqueous phases.

Method 2 based on the precipitation of the Ni(DMG) 2 complex

  • As the total activity concentrations of the other radionuclides are not 10 times higher in comparison to 63 Ni in the studied samples, only one precipitation step was implemented from the specifications of this standard [21] .
  • Aliquots of the digested samples were first weighed in a beaker.
  • The precipitates were collected by filtration and washed with water.
  • Afterwards, the solutions were evaporated near to dryness (otherwise insoluble black residues were obtained as indicated in Ref. [26] ).
  • DMG was then decomposed with hydrogen peroxide.

Method 3 based on the precipitation of the Ni(DMG) 2 complex on Ni resin

  • Eichrom Technologies recommend to eliminate Given the Fe compositions of the studied samples, an additional purification step was introduced only for the steel sample.
  • From the works of Hou et al. and Rajkovich et al. [6, 23] , it was decided to implement a separation on the anion exchange AG1-X4 resin before the purification step on the Ni resin.
  • The AG1-X4 resin has indeed a higher loading capacity towards Fe (around 15 mg/g resin) in comparison to TRU resin (5 mg/g resin).
  • The resulting solutions were then evaporated to dryness and the residues were treated as described above in the protocol dedicated to the Ni columns.

Speciation studies

  • A previous work of their group demonstrated the importance of speciation studies in order to achieve a better understanding of the behaviours of the analytes during the different separation steps and to optimize the radiochemical procedures [25] .
  • This approach was also investigated by Rosskopfova et al.
  • Ni which was not complexed by 2-nitroso-1-naphthol remained in the aqueous phase.
  • From the speciation studies, it can be inferred that the behaviours of Ni, Co and Fe strongly depend on the considered purification methods.

Applications of the three DMG-based radiochemical methods to real nuclear waste samples

  • From the literature, it is not obvious to choose the best selective radiochemical procedure based on DMG (solvent extraction, precipitation and extraction chromatography) and to determine if a single separation step can be implemented for nuclear waste samples.
  • To answer this question, the three radiochemical methods based on the use of DMG complexing agent were applied to different types of radioactive waste samples (evaporate concentrates, steels, muds embedded in concretes, effluents, ion exchange resins embedded or not in polymers and graphites).
  • The Ni recovery yields were satisfactory whatever the analysed samples and the radiochemical methods.

Where

  • For method 2 based on DMG precipitation, the E n values were higher than 1 for the majority of the studied samples (up to 17), which indicated that the performances of method 2 were unsatisfactory.
  • The E n value related to the S2 steel was prescribes that one DMG-based precipitation step should be sufficient when the total activity concentrations of the other radionuclides are not 10 times higher in comparison in comparison to 63 Ni [21] , which is not in agreement with their experimental results.
  • This standard published in 2001 [21] might be no more adapted to the nuclear waste produced in the past decade from decommissioning operations of various radioactive facilities.
  • For method 3 based on Ni column, the E n values were lower than 1 whatever the studied samples, which demonstrated that the performances of method 3 were satisfactory.
  • To check this assumption, the S3 sample (corresponding to muds embedded in concrete) was analysed with and without performing the AG1-X4 separation before the purification of the Ni column.

Did you find this useful? Give us your feedback

Figures (5)

Content maybe subject to copyright    Report

Journal of Radioanalytical and Nuclear Chemistry
1
A comparative study using liquid scintillation counting 1
to determine
63
Ni in low and intermediate level 2
radioactive waste 3
Names of the authors: Céline Gautier
1
, Christèle Colin
1
, Cécile Garcia
1♯
4
Title: A comparative study using liquid scintillation counting to determine
63
Ni in low 5
and intermediate level radioactive waste 6
Affiliation(s) and address(es) of the author(s):
1
Operator Support Analyses Laboratory, 7
Atomic Energy Commission, CEA Saclay, DEN/DANS/DPC/SEARS/LASE, Building 8
459, PC 171, 91191 Gif-sur-Yvette Cedex, FRANCE 9
♯
on leave for
AREVA, Demantelement et Services/MSIS Assistance, 91196 Gif-sur-10
Yvette Cedex, FRANCE
11
E-mail address of the corresponding author: celine.gautier@cea.fr 12
13
Journal of Radioanalytical and Nuclear Chemistry
2
A comparative study using liquid scintillation counting 14
to determine
63
Ni in low and intermediate level 15
radioactive waste 16
Céline Gautier
1
, Christèle Colin
1
, Cécile Garcia
1♯
17
1
Operator Support Analyses Laboratory, Atomic Energy Commission, CEA Saclay, 18
DEN/DANS/DPC/SEARS/LASE, Building 459, PC 171, 91191 Gif-sur-Yvette Cedex, 19
FRANCE 20
♯
On
leave for AREVA, Demantelement et Services/MSIS Assistance, 91196 Gif-sur-Yvette 21
Cedex, FRANCE 22
Abstract 23
A comparative study using liquid scintillation counting was performed to measure
63
Ni in 24
low and intermediate level radioactive waste. Three dimethylglyoxime (DMG)-based 25
radiochemical procedures (solvent extraction, precipitation, extraction chromatography) 26
were investigated, the solvent extraction method being considered as the reference 27
method. Theoretical speciation calculations enabled to better understand the chemical 28
reactions involved in the three protocols and to optimize them. In comparison to the 29
method based on DMG precipitation, the method based on extraction chromatography 30
allowed to achieve the best results in one single step in term of recovery yield and 31
accuracy for various samples. 32
Keywords 33
63
Ni, radiochemical analysis, liquid scintillation counting, decommissioning, radioactive 34
waste, dimethylglyoxime 35
Journal of Radioanalytical and Nuclear Chemistry
3
Introduction 36
In France, the National Radioactive Waste Management Agency (ANDRA) is in 37
charge of the long-term management of all radioactive waste. Several repository sites 38
have been built in order to accommodate nuclear waste packages. One is dedicated to the 39
Low and Intermediate Level short-lived Waste. The specifications for 143 radionuclides 40
have been defined by ANDRA which guarantees the safety of the facility [1]. Among this 41
long list,
63
Ni has to be declared as soon as its activity concentration is over 1 Bq g
-1
and 42
its maximum acceptance limit has been fixed to 3 x 10
6
Bq g
-1
[1].
63
Ni is produced by 43
neutron activation reactions of stable Ni and Cu which are components of various 44
materials used in the nuclear fuel cycle [2]. Consequently,
63
Ni can be present in many 45
radioactive materials and waste samples [2-17], such as graphites [6, 7], metals 46
(aluminium, lead, steel) [6-11], concretes [6, 7, 10, 12], ion-exchange resins and 47
charcoals [13], effluents [8, 14-17], sludges [14] and environmental samples [10, 18]. 48
63
Ni is a long-lived radionuclide with a half-life of 98.70 years (±24) [19]. It is a pure 49
beta emitter with a maximum energy of 66.98 keV [19]. As liquid scintillation counting 50
(LSC) has a high counting efficiency for
63
Ni (around 70 %) [2], this detection technique 51
is widely used for
63
Ni determination [2-17]. As a pure beta emitting radionuclide,
63
Ni 52
must be isolated from the matrix and the interfering radionuclides (especially
60
Co a 53
major radionuclide which has a similar chemical behavior) through chemical separations 54
prior to any analysis by LSC [2-17]. Consequently, a selective radiochemical method is 55
needed to measure
63
Ni in low and intermediate level radioactive waste [2-18]. Most 56
procedures of
63
Ni purification rely on the complexing agent of dimethylglyoxime 57
(DMG) implemented in three different types of methods: solvent extraction, precipitation 58
and extraction chromatography [2-18]. In all cases, the Ni(DMG)
2
complex is favourably 59
formed at basic pH, around 8-9 [2-18]. The recovery yield of the overall radiochemical 60
procedure is generally determined from the measurement of stable Ni by atomic 61
absorption spectroscopy (AAS) [12] or inductively coupled plasma - atomic emission 62
spectroscopy (ICP-AES) [5, 13, 15, 17]. 63
Journal of Radioanalytical and Nuclear Chemistry
4
Two or three decades ago, the reference radiochemical method to analyse
63
Ni was 64
based on a liquid-liquid extraction procedure. The Ni(DMG)
2
complex is first extracted 65
in an organic solvent [20], commonly chloroform [8, 10, 11, 18, 20] which has a higher 66
Ni extraction capacity [20]. Ni is then back-extracted in aqueous solution, mostly with 67
hydrochloric acid [11, 16, 18]. In France, this extraction method has been standardized in 68
the standard NF M60-317 to determine
63
Ni in radioactive effluents and waste [21]. Ni 69
amount is generally less than 1 mg [8, 18, 20] whereas the DMG amount varies from 10 70
mg [20] to 250 mg [8]. By replicating several extractions, this type of separation 71
procedure enabled to achieve satisfactory decontamination factors of Co towards Ni (less 72
than 0.2% of Co was extracted) [8]. In spite of its efficiency, the implementation of this 73
solvent extraction procedure has tended to decrease in the last decades because of the 74
restrictions of chloroform use, notably through the European REACH regulation [22]. 75
An alternative method to solvent extraction is the precipitation of the Ni(DMG)
2
76
complex [4, 9, 12-14]. The French standard NF M60-317 also includes this alternative 77
option as a second
63
Ni purification method [21]. When the total activity concentrations 78
of the other radionuclides are 10 times higher in comparison to
63
Ni, this standard 79
indicates the necessity to perform a second precipitation step [21]. Higher Ni amount is 80
added (around 2 or 3 mg) [12-14] whereas the DMG amount varies from 50 mg [12, 13] 81
to 200 mg [21] to favour the precipitation of the Ni(DMG)
2
complex, in comparison to 82
the solvent extraction method. Prior to LSC, the precipitate is destroyed to recover
63
Ni in 83
solution by using concentrated nitric acid [4, 9, 12, 13] or hydrogen peroxide [14]. The 84
procedure based on Ni(DMG)
2
precipitation has been applied for the measurement of 85
63
Ni in various radioactive matrices [4], such as metals [9], concretes [12], ion exchange 86
resins [13] and sludges [14]. However, the destruction of Ni(DMG)
2
precipitate appears 87
to be a delicate and fastidious step before LSC analysis [21]. 88
To overcome these above problems, the technique of extraction chromatography 89
based on the Eichrom Ni
®
resin has been developed to isolate Ni from the interfering 90
elements [23]. Some authors also prepared in-house Ni resins which relies on the same 91
principle [15, 27]. Indeed, over the past 20 decades, extraction chromatography has 92
become a leading technique for separation and preconcentration of radionuclides in the 93
Journal of Radioanalytical and Nuclear Chemistry
5
environmental, biological and nuclear fields [24, 25]. The combination of an organic 94
extractant coated on an inert support delivers the selectivity of solvent extraction with the 95
ease of use of resin based methods. In the case of Ni resin, the DMG extractant is coated 96
on an inert support of acrylic ester based-resin [23]. As relatively high amounts of DMG 97
and Ni are involved (respectively 50 mg and 2 to 3 mg for a 2 mL pre-packed column 98
[23]), on-column precipitation of Ni with DMG occurs on Ni resin [23]. Elimination of 99
the interfering elements is mainly achieved with ammonium citrate during the rinsing 100
step. Then, Ni is generally stripped from the column using nitric acid [23, 26]. In recent 101
years, many radiochemical procedures based on Ni resin have been applied on many 102
nuclear materials [5, 6, 12, 13, 15, 17, 27]. 103
DMG is an effective and selective complexing agent of Ni but also of other metal 104
elements, such as Co, Cu, Cd and Pd [28], which can induce interferences for
63
Ni 105
purification. Indeed, the
60
Co activation product is often present in substantial amounts in 106
radioactive materials in comparison to
63
Ni. Correlation factors between
63
Ni and
60
Co 107
highly depend on the types of nuclear plants and samples [29]. In CEA France, the third 108
quartile of
63
Ni/
60
Co ratio has been determined at 0.4 in solid radioactive waste. 109
Consequently, from the literature, it is frequently necessary to complete the purification 110
step based on DMG with other separation procedures so as to eliminate Co efficiently. In 111
the French standard NF M60-317, the elimination of Co is achieved with a preliminary 112
liquid-liquid extraction step based on the use of 2-nitroso-1-naphthol [21]. In this 113
standard, it is recommended to implement this Co solvent extraction when the total 114
activity concentrations of the other radionuclides are 10 times higher in comparison to 115
63
Ni [21]. Furthermore, the presence of
55
Fe, another significant activation product, can 116
also hinder the formation of Ni(DMG)
2
complex/precipitate because of its precipitation at 117
basic pH [23, 26]. Organic complexing agents, such as citric acid [6, 12, 21], tartaric acid 118
[9, 21] or oxalic acid [5] are generally introduced to prevent the precipitation of Fe and 119
the other metal elements at basic pH. However, their chelating properties may not be 120
sufficient in case of high Fe amounts, such as in steels [6, 28]. Consequently, it is also 121
highly recommended to remove Fe to achieve accurate
63
Ni measurements. Precipitation 122
with ammonia [12-16, 18] or hydroxide [6, 14] and anion exchange chromatography [4, 123
5, 9, 10, 11, 14, 15, 17] have been mainly applied in order to eliminate the interfering 124
Citations
More filters
Journal Article•DOI•
Liquid scintillation counting for determination of radionuclides in environmental and nuclear application

[...]

Xiaolin Hou1, Xiaolin Hou2•
Lanzhou University1, Technical University of Denmark2
01 Dec 2018-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: A review and discussion on the LSC based analytical methods for the determination of major radionuclides in environmental researches, decommissioning of nuclear faculties and nuclear application are presented, in both measurement techniques and sample preparation using radiochemical separation as discussed by the authors.
Abstract: Liquid scintillation counting (LSC) is a major technique not only for measurement of pure beta emitting radionuclides, but also radionuclides decay by electron capture and alpha emission. Although it is a conventional radiometric technique, but still a competitive techniques for the measurement of many radionuclides. This paper summaries the major development of this measurement technique in instrumentation, methodology and applications in the past decades. The progresses in the instrumentation and methodology mainly focus on the commercialization of triple-to-double coincidence ratio based LSC techniques and its application in the determination of different radionuclides. An overall review and discussion on the LSC based analytical methods for the determination of major radionuclides in environmental researches, decommissioning of nuclear faculties and nuclear application are presented, in both measurement techniques and sample preparation using radiochemical separation. Meanwhile the problems and challenges in the development and application of the LSC are also discussed.

42 citations

Book Chapter•DOI•
Environmental liquid scintillation analysis

[...]

Xiaolin Hou1, Xiaolin Hou2, Xiongxin Dai•
Lanzhou University1, Technical University of Denmark2
01 Jan 2020
TL;DR: In this article, the authors present the principles of liquid scintillation counting (LSC) measurement techniques and focus on the practical issues in the LSC determination of environmental radionuclides, as well as the status of the present research progress in these aspects.
Abstract: Liquid scintillation counting (LSC) is a major method for the measurement of beta-emitting and some alpha-emitters. It has been applied in many aspects such as the monitoring of environmental radioactivity, the behavior of radionuclides in the environment, and the characterization of nuclear waste for the decommissioning of nuclear facilities. Radionuclides are also widely applied to the investigation of environmental processes. However, the level of radionuclides in the environment is normally very low, and the resolution of LSC alone is not sufficiently high to identify and quantitatively measure different radionuclides. Low background LSC and chemical separation and purification are needed. This chapter aims to present the principles of LSC measurement techniques for the above purposes and focus on the practical issues in the LSC determination of environmental radionuclides, as well as the status of the present research progress in these aspects. The principles of low-level counting using LSC including the methods for reducing the background in the LSC instrument and practical issues in sample preparation are presented. The principles and applications for the measurement of alpha-emitters using LSC with the alpha/beta discrimination features are presented. The main application of triple-to-double coincidence ratio–based LSC in normal and Cerenkov counting models are also described. Most of the effort of this chapter focuses on the application of LSC in the determination of different anthropogenic and naturally occurring radionuclides, including tritium, 14C, 55Fe, 63Ni, 89,90Sr, 90Y, 99Tc, 241Pu, 36Cl, 41Ca, 129I, 210Po, 210Pb, isotopes of uranium, thorium, radium, and radon. Besides the LSC measurement methods, the detailed and practical chemical separation of these radionuclides from different sample matrices, as well as the sample preparation methods for LSC measurement are discussed based on the open publications and the experiences of the authors.

12 citations

Journal Article•DOI•
Intercomparison exercise on difficult to measure radionuclides in activated steel: statistical analysis of radioanalytical results and activation calculations

[...]

Anumaija Leskinen1, Susanna Salminen-Paatero2, Celine Gautier3, Antti Räty1, Merja Tanhua-Tyrkkö1, Pascal Fichet3, Tommi Kekki1, Wenzhong Zhang2, Jacques Bubendorff3, Elodie Laporte3, Gabriel Lambrot3, René Brennetot3 •
VTT Technical Research Centre of Finland1, University of Helsinki2, Université Paris-Saclay3
01 May 2020-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: In this paper, the results obtained during an intercomparison exercise for the determination of difficult to measure radionuclides in activated reactor pressure vessel (RPV) steel samples were reported.
Abstract: This paper reports the results obtained during an intercomparison exercise for the determination of difficult to measure radionuclides in activated reactor pressure vessel (RPV) steel samples. In total, eight laboratories participated analysing 14C, 55Fe and 63Ni activity concentrations in RPV steel. In addition, some laboratories also analysed 60Co activity concentrations. Corresponding activity concentrations were also determined using activation calculations. Robust statistical techniques were utilised for the analysis of the results according to ISO 13528 standard. The results showed good agreement for 55Fe and 63Ni results whereas 14C results had significant differences. 60Co results were in quite good agreement.

6 citations

Journal Article•DOI•
Intercomparison exercise on difficult to measure radionuclides in activated concrete - statistical analysis and comparison with activation calculations

[...]

Anumaija Leskinen1, Celine Gautier2, Antti Räty1, Tommi Kekki1, Elodie Laporte2, Margaux Giuliani2, Jacques Bubendorff2, Julia Pauliina Laurila3, Julia Pauliina Laurila4, Kristian Otto Aleksi Kurhela4, Kristian Otto Aleksi Kurhela3, Pascal Fichet2, Susanna Salminen-Paatero3 •
VTT Technical Research Centre of Finland1, Université Paris-Saclay2, University of Helsinki3, Helsinki Metropolia University of Applied Sciences4
28 Jun 2021-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: In this article, the results obtained in a Nordic Nuclear Safety Research project during the second intercomparison exercise for the determination of difficult to measure radionuclides in decommissioning waste are reported.
Abstract: This paper reports the results obtained in a Nordic Nuclear Safety Research project during the second intercomparison exercise for the determination of difficult to measure radionuclides in decommissioning waste. Eight laboratories participated by carrying out radiochemical analysis of 3H, 14C, 36Cl, 41Ca, 55Fe and 63Ni in an activated concrete. In addition, gamma emitters, namely 152Eu and 60Co, were analysed. The assigned values were derived from the submitted results according to ISO 13,528 standard and the performance assessments were determined using z scores. The measured results were compared with activation calculation result showing varying degree of comparability.

5 citations

Journal Article•DOI•
Method for sequential determination of 55 Fe and 63 Ni in leaching solution from cement solidification

[...]

Lijuan Song, Ma Lina, Yan Ma, Yonggang Yang1, Xiongxin Dai1 •
Soochow University (Suzhou)1
01 Mar 2019-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: In this article, a method for sequential determination of 55Fe and 63Ni in leaching solution of cement solidification using liquid scintillation counting (LSC) was developed, and the performance of the method was examined.
Abstract: A method for sequential determination of 55Fe and 63Ni in leaching solution of cement solidification using liquid scintillation counting (LSC) was developed. In this method, 55Fe and 63Ni were first precipitated in the form of hydroxide and subsequently purified by anion exchange chromatography and dimethylglyoxime precipitation. After the purification, 55Fe and 63Ni were determined by LSC. The performance of the method was examined, and minimum detectable activity concentration was determined to be 0.82 Bq L−1 for 55Fe and 0.42 Bq L−1 for 63Ni in leaching solution samples with a counting time of 1 h. High decontamination factors for 55Fe and 63Ni were also obtained.

3 citations

References
More filters
Journal Article•DOI•
Determination of 59Ni in radioactive waste

[...]

O. Fišera, F. Šebesta1•
Czech Technical University in Prague1
01 Aug 2010-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: In this article, a composite material PAN-DMG, containing chelating agent dimethylglyoxime (DMG) immobilized in a porous matrix of binding polymer polyacrylonitrile (PAN), was used for nickel separation and concentration.
Abstract: Composite material PAN-DMG, containing chelating agent dimethylglyoxime (DMG) immobilized in porous matrix of binding polymer polyacrylonitrile (PAN), was used for nickel separation and concentration. Method for preparation of 59Ni source for low energy photon spectrometry was developed using homogeneous precipitation of nickel with DMG. The proposed method was tested with two types of real radioactive waste (boric acid concentrate from nuclear power plant (NPP) evaporator and spent ion exchanger from NPP).

12 citations

"A comparative study using liquid sc..." refers background or methods in this paper

  • ...In recent years, many radiochemical procedures based on Ni resin have been applied on many nuclear materials [5, 6, 12, 13, 15, 17, 27]....

    [...]

  • ...It corresponds to the radiochemical method described by Eichrom Technologies [26] and applied in many reported works [6, 12, 13, 15, 17, 27]....

    [...]

  • ...Some authors also prepared in-house Ni resins which relies on the same principle [15, 27]....

    [...]

Journal Article•DOI•
Rapid separation of nickel for 59 Ni and 63 Ni activity measurement in radioactive waste samples

[...]

Chang Heon Lee, Kwang Soon Choi, Byoung Chul Song, Yeong-Keong Ha, Kyuseok Song 
30 Apr 2013-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: In this paper, a peristaltic pump with sixteen channels and the same number of Ni-Resin columns was constructed for the quantification of Ni and 63Ni in radioactive wastes discharged from nuclear power plants and various research activities related to the nuclear fuel cycle.
Abstract: A separation procedure of Ni has been described for the quantification of 59Ni and 63Ni in radioactive wastes discharged from nuclear power plants and various research activities related to the nuclear fuel cycle. For a rapid separation of the Ni-nuclides in sixteen sample solutions in 0.2 M NH4-oxalate, a separation system composed of a peristaltic pump with sixteen channels and the same number of Ni–Resin columns was constructed. After sorption of the Ni-nuclides by sequentially passing 100 mL of the sample solution in 0.2 M NH4-oxalate, 130 mL of 0.1 M NH4-oxalate solution and 10 mL of deionized water as a wash into the columns, these were purely recovered by passing 10 mL of 9 M HCl into the Ni–Resin columns stacked in series on the anion exchange resin columns. The separation of the Ni-nuclides in sixteen sample solutions can be achieved within 7 h. The chemical yield of the proposed procedure is 92.3 ± 0.8 % (n = 5) and the gravimetric recovery in the preparation stage of the Ni-nuclide sources is also acceptable, 88.5 ± 1.3 % (n = 5).

9 citations

"A comparative study using liquid sc..." refers background or methods in this paper

  • ...Aliquots were prepared for the determination of stable metal elements and gamma emitting radionuclides by ICP-AES and gamma spectrometers respectively....

    [...]

  • ...In recent years, many radiochemical procedures based on Ni resin have been applied on many nuclear materials [5, 6, 12, 13, 15, 17, 27]....

    [...]

  • ...This hypothesis was confirmed by gamma and ICP-AES measurements....

    [...]

  • ...The recovery yield of the overall radiochemical procedure is generally determined from the measurement of stable Ni by atomic absorption spectroscopy (AAS) [12] or inductively coupled plasma-atomic emission spectroscopy (ICP-AES) [5, 13, 15, 17]....

    [...]

  • ...Organic complexing agents, such as citric acid [6, 12, 21], tartaric acid [9, 21] or oxalic acid [5] are generally introduced to prevent the precipitation of Fe and the other metal elements at basic pH....

    [...]

Journal Article•DOI•
Application of procedures for low level radionuclide analysis in environmental monitoring for the purpose of clearance measurements of materials from decommissioning of nuclear facilities

[...]

U. Hoeppener-Kramar, M. Pimpl, F. Willmann
01 Dec 1997-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: In this paper, the procedures for the analysis of radionuclides of prior interest for decommissioning measures are outlined, together with the respective sample decomposition methods, for which adequate procedures were not available, new methods were developed.
Abstract: Materials from decommissioning of nuclear facilities can be re-used without restrictions, if their mass specific activities are in accordance to the guidelines for allowable concentrations. To determine the nuclide specific activity level of representative samples, a “clearance laboratory” was installed at the Research Center Karlsruhe. For the purpose of low level radionuclide analysis, procedures, developed for environmental monitoring, were successfully adapted to decommissioning materials. For radionuclides, for which adequate procedures were not available, new methods were developed. The procedures for the analysis of radionuclides of prior interest for decommissioning measures are outlined, together with the respective sample decomposition methods.

8 citations

Journal Article•DOI•
Identification of 63ni and 60co produced in a steel sample by thermal neutrons from the hiroshima atomic bomb

[...]

Kiyoshi Shizuma1, Kazuo Iwatani1, Hiromi Hasai, Takamitsu Oka2, Masaharu Hoshi1, S. Shibata3, Mineo Imamura3, T.-A. Shibata3 •
Hiroshima University1, Kure University2, University of Tokyo3
01 Jan 1997-Nuclear Instruments & Methods in Physics Research Section A-accelerators Spectrometers Detectors and Associated Equipment
TL;DR: In this article, the long-lived residual radioactivity 63Ni produced by the (n, γ) reaction was detected for the first time from a steel plate sampled at near the hypocenter of the Hiroshima atomic bomb.
Abstract: Long-lived residual radioactivity 63Ni produced by the (n, γ) reaction was detected for the first time from a steel plate sampled at near the hypocenter of the Hiroshima atomic bomb. Nickel and cobalt were chemically separated and enriched from the steel sample. Low energy beta rays of 63Ni were measured with a low-background liquid scintillation counter and gamma-rays of 60Co were measured with a low background Ge detector. Specific activities were determined as 0.0063±0.0004 Bq mg−1 for 63 Ni Ni and 8.70±0.46 Bq mg−1 for 60 Co Co at the time of the bomb explosion. Comparisons with the calculated yield based on the current dosimetry system DS86 neutrons were also given.

8 citations

"A comparative study using liquid sc..." refers background in this paper

  • ...Ni is then back-extracted in aqueous solution, mostly with hydrochloric acid [11, 16, 18]....

    [...]

  • ...The Ni(DMG)2 complex is first extracted in an organic solvent [20], commonly chloroform [8, 10, 11, 18, 20] which has a higher Ni extraction capacity [20]....

    [...]

Journal Article•DOI•
Determination of difficult to measure radionuclides in primary circuit facilities of NPP V1 Jaslovske Bohunice

[...]

Boris Remenec1, Silvia Dulanská1, L’ubomír Mátel1•
Comenius University in Bratislava1
04 Aug 2013-Journal of Radioanalytical and Nuclear Chemistry
TL;DR: In this paper, the results of difficult to measure radionuclides in primary circuit facilities of nuclear power plant V1 in Jaslovske Bohunice (NPP V1) are presented.
Abstract: Results of difficult to measure radionuclides in primary circuit facilities of nuclear power plant V1 in Jaslovske Bohunice (NPP V1) are presented. Samples from steam generator, main circulation pump and pressurizer were analyzed. Activity concentrations of 55Fe, 63,59Ni, 90Sr, 99Tc, 93Mo, 94Nb, transuranic elements were determined. Analytical and sampling methods are briefly described for the determination of difficult to measure radionuclides. The presented results have been successfully used for characterization of the waste during the decommissioning of NPP V1 nuclear reactors.

7 citations

"A comparative study using liquid sc..." refers background or methods in this paper

  • ...Aliquots were prepared for the determination of stable metal elements and gamma emitting radionuclides by ICP-AES and gamma spectrometers respectively....

    [...]

  • ...In recent years, many radiochemical procedures based on Ni resin have been applied on many nuclear materials [5, 6, 12, 13, 15, 17, 27]....

    [...]

  • ...This hypothesis was confirmed by gamma and ICP-AES measurements....

    [...]

  • ...The recovery yield of the overall radiochemical procedure is generally determined from the measurement of stable Ni by atomic absorption spectroscopy (AAS) [12] or inductively coupled plasma-atomic emission spectroscopy (ICP-AES) [5, 13, 15, 17]....

    [...]

  • ...Stable Fe, Co and Ni concentrations were measured using an ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectroscopy) Activa M spectrometer (HORIBA Jobin– Yvon, Longjumeau, France)....

    [...]

Related Papers (5)
Determination of 63Ni and 55Fe in nuclear waste samples using radiochemical separation and liquid scintillation counting

[...]

11 Apr 2005-Analytica Chimica Acta
Xiaolin Hou, Lars Frosig Østergaard, Sven Poul Nielsen
Measurement of63Ni in highly radioactive Hanford waste by liquid scintillation counting

[...]

01 May 1994-Journal of Radioanalytical and Nuclear Chemistry
J. H. Kaye, R. S. Strebin, Ahmad E. Nevissi
Evaluation of a direct extraction/liquid scintillation counting technique for the measurement of uranium in water

[...]

01 Jul 1995-Journal of Radioanalytical and Nuclear Chemistry
J. D. Leyba, H. S. Vollmar, Robert A. Fjeld, Timothy A. DeVol, David D. Brown, J. R. Cadieux 
A procedure for the separation of79Se from fission products and application to the determination of the79Se half-life

[...]

01 Jun 1997-Journal of Radioanalytical and Nuclear Chemistry
Li Chunsheng, Guo Jingru, Li Daming
The simple radiochemical determination of 90Sr in environmental solid samples by solvent extraction

[...]

08 Mar 2011-Journal of Radioanalytical and Nuclear Chemistry
Filiz Karacan
Frequently Asked Questions (1)
Q1. What are the contributions in this paper?

23 A comparative study using liquid scintillation counting was performed to measure 63 Ni in 24 low and intermediate level radioactive waste.