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Article(id=1147999669768155431, tenantId=1146029695717560320, journalId=1146123346816638986, issueId=1147997645471216289, articleNumber=1000-8063(2024)01-0036-06, orderNo=null, doi=10.13426/j.cnki.yky.2023.04.03, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1681228800000, receivedDateStr=2023-04-12, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1751634050074, onlineDateStr=2025-07-04, pubDate=1708358400000, pubDateStr=2024-02-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1751634050074, onlineIssueDateStr=2025-07-04, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1751634050074, creator=13701087609, updateTime=1751634050074, updator=13701087609, issue=Issue{id=1147997645471216289, tenantId=1146029695717560320, journalId=1146123346816638986, year='2024', volume='43', issue='1', pageStart='1', pageEnd='98', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=0, articleOrder=1, issueType=-1, specialIssue=null, createTime=1751633567445, creator=13701087609, updateTime=1762910967272, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1195298488901714724, tenantId=1146029695717560320, journalId=1146123346816638986, issueId=1147997645471216289, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1195298488901714725, tenantId=1146029695717560320, journalId=1146123346816638986, issueId=1147997645471216289, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=36, endPage=41, ext={EN=ArticleExt(id=1147999669977870632, articleId=1147999669768155431, tenantId=1146029695717560320, journalId=1146123346816638986, language=EN, title=Determination of Uranium Content in Natural Uranium Products by X-ray Fluorescence Spectrometry, columnId=1195095623629291715, journalTitle=Uranium Mining and Metallurgy, columnName=ANALYSIS AND INSTRUMENT, runingTitle=null, highlight=null, articleAbstract=

A method for determining uranium content in natural uranium products (U3O8) by wavelength dispersive X-ray fluorescence spectrometry was established using solution sample preparation and strontium carbonate as the internal standard. The method determines that the weight of the sample is 1.00 g, and the weight of the internal standard strontium carbonate is 0.600 g. The sample is digested with 15 mL of phosphoric acid and 2 mL of nitric acid to a constant volume of 200 mL. After stirring with magnetic force, the volume of the solution is controlled using a disposable plastic pipette and an electronic scale. Instrument measurement conditions selection feature X-ray line: U-Lα1,Sr-Kα1, channel mask 34 mm, primary collimator 150 μm. The linear correlation coefficient of the working curve of the method is 0.999 8, and the relative standard deviation (RSD) is between 0.031% and 0.050%, indicating good precision; The relative error between the measurement results and the recommended value of the reference material is not less than 0.034%, with good accuracy. Compared with the potentiometric titration method, the absolute deviation of this method is between 0.010% and 0.126%, and the results are accurate and reliable, meeting the requirements for rapid batch analysis of natural uranium products.

, correspAuthors=Shuguang ZHU, Jinliang LIU, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=ZHU Shuguang, ZHANG Xin, LIU Jinliang, LIU Chao, SONG Maosheng, YAN Feiyan, WANG Long, LIU Yue, YANG Liyuan), CN=ArticleExt(id=1147999670787371310, articleId=1147999669768155431, tenantId=1146029695717560320, journalId=1146123346816638986, language=CN, title=溶液制样—波长色散X射线荧光光谱法测定天然铀产品中的铀含量, columnId=1195095623952253124, journalTitle=铀矿冶, columnName=分析·仪表, runingTitle=null, highlight=null, articleAbstract=

采用溶液制样,以碳酸锶为内标物,建立了用波长色散X射线荧光光谱法测定天然铀产品(U3O8)中铀含量的方法。样品称样质量为1.00 g,内标物碳酸锶称样质量为0.600 g,采用15 mL磷酸和2 mL硝酸消解样品,定容至200 mL后,用磁力搅拌混匀,采用一次性塑料吸管和电子秤控制取液体积。仪器测量条件选择特征X谱线:U-Lα1,Sr-Kα1,通道面罩34 mm,初级准直器150 μm。该方法工作曲线的线性相关系数为0.999 8,相对标准偏差(RSD)为0.031%~0.050%,精密度较好;测定结果与标准物质推荐值之间的相对误差不劣于0.034%,准确度较好。与电位滴定法对比,该法绝对偏差为0.010%~0.126%,结果准确可靠,能够满足天然铀产品快速批量分析的要求。

, correspAuthors=朱曙光, 柳金良, authorNote=null, correspAuthorsNote=
柳金良(1986—),男,湖南衡东人,学士,高级工程师,主要从事分析化学、仪器分析研究工作。
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朱曙光(1974—),男,湖南汝城人,硕士,高级工程师,主要从事矿山工程、化学工艺、分析化学工作。

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朱曙光(1974—),男,湖南汝城人,硕士,高级工程师,主要从事矿山工程、化学工艺、分析化学工作。

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朱曙光(1974—),男,湖南汝城人,硕士,高级工程师,主要从事矿山工程、化学工艺、分析化学工作。

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tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=EN, label=Fig. 1, caption=The linear relationship between IU/ISr and mU, figureFileSmall=XfplK1R2mzyRZCTYA1vy9g==, figureFileBig=Msa8LMDwAyGtLtpnS3KgPA==, tableContent=null), ArticleFig(id=1195800196341870964, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=CN, label=图1, caption=铀、锶强度比与铀质量的线性关系, figureFileSmall=XfplK1R2mzyRZCTYA1vy9g==, figureFileBig=Msa8LMDwAyGtLtpnS3KgPA==, tableContent=null), ArticleFig(id=1195800196434145654, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=EN, label=Table 1, caption=

Instrument measurement conditions

, figureFileSmall=null, figureFileBig=null, tableContent=
分析线 晶体 准直器
宽度/μm		 探测器 滤光片/
μm		 电压/
kV		 电流/
mA		 2θ/(°) PHD 测量时间/s
峰值 背景1 背景2 LL UL 峰值 背景1 背景2
U-Lα LiF220 150 HiperScint Al 200 60 60 37.266 -2.472 1.411 15 78 50 10 10
Sr-Kα LiF220 150 HiperScint Al 200 60 60 35.797 -1.009 2.864 15 78 50 10 10
), ArticleFig(id=1195800196501254519, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=CN, label=表1, caption=

仪器测量条件

, figureFileSmall=null, figureFileBig=null, tableContent=
分析线 晶体 准直器
宽度/μm		 探测器 滤光片/
μm		 电压/
kV		 电流/
mA		 2θ/(°) PHD 测量时间/s
峰值 背景1 背景2 LL UL 峰值 背景1 背景2
U-Lα LiF220 150 HiperScint Al 200 60 60 37.266 -2.472 1.411 15 78 50 10 10
Sr-Kα LiF220 150 HiperScint Al 200 60 60 35.797 -1.009 2.864 15 78 50 10 10
), ArticleFig(id=1195800196568363385, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=EN, label=Table 2, caption=

Selection of sample mass for internal standard substance

, figureFileSmall=null, figureFileBig=null, tableContent=
称样质量/g 测量强度/kcps 强度比
GBW04205 SrCO3 IU ISr IU/ISr
1.004 12 0.400 81 431.047 8 290.388 5 1.484 4
1.004 87 0.500 55 424.738 5 351.581 4 1.208 1
1.007 28 0.600 20 422.391 2 413.064 9 1.022 6
1.006 25 0.700 74 415.535 1 473.961 8 0.876 7
), ArticleFig(id=1195800196660638075, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=CN, label=表2, caption=

内标物称样量选择试验

, figureFileSmall=null, figureFileBig=null, tableContent=
称样质量/g 测量强度/kcps 强度比
GBW04205 SrCO3 IU ISr IU/ISr
1.004 12 0.400 81 431.047 8 290.388 5 1.484 4
1.004 87 0.500 55 424.738 5 351.581 4 1.208 1
1.007 28 0.600 20 422.391 2 413.064 9 1.022 6
1.006 25 0.700 74 415.535 1 473.961 8 0.876 7
), ArticleFig(id=1195800196723552637, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=EN, label=Table 3, caption=

The main characteristic X-ray line parameters of U and Sr

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 特征X谱线 波长/nm 激发电势/keV 相对强度
U Kα1 0.012 6 115.610 -
Lα1 0.091 1 21.764 100
Lα2 0.092 3 20.938 10
Lβ1 0.072 0 17.160 50
Sr Kα1 0.087 5 16.101 100
Kα2 0.088 0 2.220 50
Kβ1 0.078 3 2.008 15
), ArticleFig(id=1195800196811633023, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=CN, label=表3, caption=

U和Sr的主要特征X谱线参数

, figureFileSmall=null, figureFileBig=null, tableContent=
元素 特征X谱线 波长/nm 激发电势/keV 相对强度
U Kα1 0.012 6 115.610 -
Lα1 0.091 1 21.764 100
Lα2 0.092 3 20.938 10
Lβ1 0.072 0 17.160 50
Sr Kα1 0.087 5 16.101 100
Kα2 0.088 0 2.220 50
Kβ1 0.078 3 2.008 15
), ArticleFig(id=1195800196878741889, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=EN, label=Table 4, caption=

Precision experiment results

, figureFileSmall=null, figureFileBig=null, tableContent=
编号 w(U)/% w(U)平均
值/%		 标准偏差
(SD)/%		 相对标准偏差
(RSD)/%
HS-1 83.578 83.538 83.546 83.551 83.599 83.593 83.568 0.026 0.031
HS-2 83.703 83.750 83.805 83.739 83.761 83.728 83.748 0.034 0.041
HS-3 84.030 83.941 83.977 83.934 83.972 83.913 83.961 0.041 0.049
HS-4 82.501 82.439 82.406 82.409 82.429 82.438 82.437 0.034 0.042
HS-5 84.613 84.676 84.644 84.566 84.673 84.660 84.639 0.042 0.050
HS-6 84.123 84.070 84.058 84.081 84.052 84.048 84.072 0.028 0.033
), ArticleFig(id=1195800196945850755, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=CN, label=表4, caption=

精密度试验结果

, figureFileSmall=null, figureFileBig=null, tableContent=
编号 w(U)/% w(U)平均
值/%		 标准偏差
(SD)/%		 相对标准偏差
(RSD)/%
HS-1 83.578 83.538 83.546 83.551 83.599 83.593 83.568 0.026 0.031
HS-2 83.703 83.750 83.805 83.739 83.761 83.728 83.748 0.034 0.041
HS-3 84.030 83.941 83.977 83.934 83.972 83.913 83.961 0.041 0.049
HS-4 82.501 82.439 82.406 82.409 82.429 82.438 82.437 0.034 0.042
HS-5 84.613 84.676 84.644 84.566 84.673 84.660 84.639 0.042 0.050
HS-6 84.123 84.070 84.058 84.081 84.052 84.048 84.072 0.028 0.033
), ArticleFig(id=1195800197008765317, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=EN, label=Table 5, caption=

Accuracy experiment results

, figureFileSmall=null, figureFileBig=null, tableContent=
标准物质
编号		 w(U)/% w(U)/% 相对误差
(RE)/%
平均值 推荐值
GBW04205 84.680 84.736 84.666 84.703 84.694 84.650 84.688 84.711 0.027
GBW04201 84.705 84.726 84.696 84.788 84.693 84.745 84.726 84.754 0.034
定值样1# 84.631 84.630 84.682 84.670 84.619 84.655 84.648 84.670 0.026
定值样2# 84.659 84.682 84.635 84.677 84.578 84.576 84.635 84.650 0.018
), ArticleFig(id=1195800197101040007, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=CN, label=表5, caption=

准确度试验结果

, figureFileSmall=null, figureFileBig=null, tableContent=
标准物质
编号		 w(U)/% w(U)/% 相对误差
(RE)/%
平均值 推荐值
GBW04205 84.680 84.736 84.666 84.703 84.694 84.650 84.688 84.711 0.027
GBW04201 84.705 84.726 84.696 84.788 84.693 84.745 84.726 84.754 0.034
定值样1# 84.631 84.630 84.682 84.670 84.619 84.655 84.648 84.670 0.026
定值样2# 84.659 84.682 84.635 84.677 84.578 84.576 84.635 84.650 0.018
), ArticleFig(id=1195800197172343177, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=EN, label=Table 6, caption=

Comparison experiment results of analytical methods

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号 w(U)/% 绝对偏差/%
X射线荧光光谱法 电位滴定法
ZGH-1 83.709 83.769 0.060
ZGH-2 83.756 83.863 0.107
ZGH-3 83.748 83.799 0.051
ZGH-4 82.212 82.176 0.036
ZGH-5 81.913 82.001 0.088
ZGH-6 82.784 82.887 0.103
ZGH-7 81.716 81.678 0.038
ZGH-8 82.653 82.582 0.071
ZGH-9 83.417 83.363 0.054
ZGH-10 83.180 83.075 0.105
ZGH-11 82.803 82.792 0.012
ZGH-12 82.625 82.537 0.088
ZGH-13 83.111 83.100 0.011
ZGH-14 83.472 83.591 0.119
ZGH-15 83.270 83.255 0.015
ZGH-16 83.759 83.715 0.044
ZGH-17 83.811 83.686 0.125
ZGH-18 83.834 83.720 0.114
ZGH-19 83.656 83.670 0.014
ZGH-20 83.667 83.560 0.107
), ArticleFig(id=1195800197239452043, tenantId=1146029695717560320, journalId=1146123346816638986, articleId=1147999669768155431, language=CN, label=表6, caption=

分析方法比对试验

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号 w(U)/% 绝对偏差/%
X射线荧光光谱法 电位滴定法
ZGH-1 83.709 83.769 0.060
ZGH-2 83.756 83.863 0.107
ZGH-3 83.748 83.799 0.051
ZGH-4 82.212 82.176 0.036
ZGH-5 81.913 82.001 0.088
ZGH-6 82.784 82.887 0.103
ZGH-7 81.716 81.678 0.038
ZGH-8 82.653 82.582 0.071
ZGH-9 83.417 83.363 0.054
ZGH-10 83.180 83.075 0.105
ZGH-11 82.803 82.792 0.012
ZGH-12 82.625 82.537 0.088
ZGH-13 83.111 83.100 0.011
ZGH-14 83.472 83.591 0.119
ZGH-15 83.270 83.255 0.015
ZGH-16 83.759 83.715 0.044
ZGH-17 83.811 83.686 0.125
ZGH-18 83.834 83.720 0.114
ZGH-19 83.656 83.670 0.014
ZGH-20 83.667 83.560 0.107
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溶液制样—波长色散X射线荧光光谱法测定天然铀产品中的铀含量
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朱曙光 1 , 张鑫 2, 3 , 柳金良 2, 3 , 刘朝 2, 3 , 宋茂生 2, 3 , 鄢飞燕 2, 3 , 王龙 4 , 刘悦 4 , 杨立远 5
铀矿冶 | 分析·仪表 2024,43(1): 36-41
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铀矿冶 | 分析·仪表 2024, 43(1): 36-41
溶液制样—波长色散X射线荧光光谱法测定天然铀产品中的铀含量
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朱曙光1, 张鑫2, 3, 柳金良2, 3, 刘朝2, 3, 宋茂生2, 3, 鄢飞燕2, 3, 王龙4, 刘悦4, 杨立远5
作者信息
  • 1 湖北三〇三库,湖北 武汉 430000
  • 2 核工业230研究所,湖南 长沙 410007
  • 3 湖南省伴生放射性矿产资源评价与综合利用工程技术研究中心,湖南 长沙 410007
  • 4 中国铀业有限公司,北京 100013
  • 5 中国原子能工业有限公司,北京 100032

    • 朱曙光(1974—),男,湖南汝城人,硕士,高级工程师,主要从事矿山工程、化学工艺、分析化学工作。

通讯作者:

柳金良(1986—),男,湖南衡东人,学士,高级工程师,主要从事分析化学、仪器分析研究工作。
Determination of Uranium Content in Natural Uranium Products by X-ray Fluorescence Spectrometry
ZHU Shuguang1, ZHANG Xin2, 3, LIU Jinliang2, 3, LIU Chao2, 3, SONG Maosheng2, 3, YAN Feiyan2, 3, WANG Long4, LIU Yue4, YANG Liyuan5
Affiliations
  • 1 Hubei 303 Warehouse, Wuhan 430000, China
  • 2 Research Institute No. 230, CNNC, Changsha 410007, China
  • 3 Hunan Engineering Technology Research Center for Evaluation and Comprehensive Utilization of Associated Radioactive Mineral Resources, Changsha 410007, China
  • 4 China National Uranium Co., Ltd., CNNC, Beijing 100013, China
  • 5 China Nuclear Energy Industry Corporation, Beijing 100032, China
出版时间: 2024-02-20 doi: 10.13426/j.cnki.yky.2023.04.03
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摘要
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采用溶液制样,以碳酸锶为内标物,建立了用波长色散X射线荧光光谱法测定天然铀产品(U3O8)中铀含量的方法。样品称样质量为1.00 g,内标物碳酸锶称样质量为0.600 g,采用15 mL磷酸和2 mL硝酸消解样品,定容至200 mL后,用磁力搅拌混匀,采用一次性塑料吸管和电子秤控制取液体积。仪器测量条件选择特征X谱线:U-Lα1,Sr-Kα1,通道面罩34 mm,初级准直器150 μm。该方法工作曲线的线性相关系数为0.999 8,相对标准偏差(RSD)为0.031%~0.050%,精密度较好;测定结果与标准物质推荐值之间的相对误差不劣于0.034%,准确度较好。与电位滴定法对比,该法绝对偏差为0.010%~0.126%,结果准确可靠,能够满足天然铀产品快速批量分析的要求。

波长色散X射线荧光光谱法  /  天然铀产品  /  铀含量

A method for determining uranium content in natural uranium products (U3O8) by wavelength dispersive X-ray fluorescence spectrometry was established using solution sample preparation and strontium carbonate as the internal standard. The method determines that the weight of the sample is 1.00 g, and the weight of the internal standard strontium carbonate is 0.600 g. The sample is digested with 15 mL of phosphoric acid and 2 mL of nitric acid to a constant volume of 200 mL. After stirring with magnetic force, the volume of the solution is controlled using a disposable plastic pipette and an electronic scale. Instrument measurement conditions selection feature X-ray line: U-Lα1,Sr-Kα1, channel mask 34 mm, primary collimator 150 μm. The linear correlation coefficient of the working curve of the method is 0.999 8, and the relative standard deviation (RSD) is between 0.031% and 0.050%, indicating good precision; The relative error between the measurement results and the recommended value of the reference material is not less than 0.034%, with good accuracy. Compared with the potentiometric titration method, the absolute deviation of this method is between 0.010% and 0.126%, and the results are accurate and reliable, meeting the requirements for rapid batch analysis of natural uranium products.

wavelength dispersive X-ray fluorescence spectrometry  /  natural uranium product  /  uranium content
朱曙光, 张鑫, 柳金良, 刘朝, 宋茂生, 鄢飞燕, 王龙, 刘悦, 杨立远. 溶液制样—波长色散X射线荧光光谱法测定天然铀产品中的铀含量. 铀矿冶, 2024 , 43 (1) : 36 -41 . DOI: 10.13426/j.cnki.yky.2023.04.03
ZHU Shuguang, ZHANG Xin, LIU Jinliang, LIU Chao, SONG Maosheng, YAN Feiyan, WANG Long, LIU Yue, YANG Liyuan. Determination of Uranium Content in Natural Uranium Products by X-ray Fluorescence Spectrometry[J]. Uranium Mining and Metallurgy, 2024 , 43 (1) : 36 -41 . DOI: 10.13426/j.cnki.yky.2023.04.03
正文
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天然铀产品(U3O8)中的铀含量检测结果是贸易结算的主要依据,其准确性和时效性尤为重要。常见的铀含量测定方法有氧化还原滴定法[1-2]、库仑滴定法[3-4]、同位素稀释质谱法等[5],这些方法测定准确度高,但存在操作流程较长、程序繁琐、人为因素影响大等缺点,很难满足天然铀产品快速批量分析的要求。
近年来,X射线荧光法经过不断完善和发展,已经成为一种广泛应用于冶金、建材、地矿、商检、环保、食品卫生、有色金属等领域的分析方法。该技术用X射线照射样品表面,不会对仪器进样系统造成污染,具有快速、重现性好的优点,对高含量铀的测定具有优势。X射线荧光光谱法在检测铀领域应用广泛[6-11],前人研究了以锶作内标物,采用X射线荧光光谱法测定天然铀产品中的铀[12-14];以及研究了采用X射线荧光光谱法测定天然铀产品中铀含量不确定度[15]等。笔者总结前人的经验,利用X射线荧光法的优点,采用波长色散X射线荧光光谱法(以下简称XRF),对天然铀产品中铀含量进行检测,并对测定条件进行了优化。
1 试验部分
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1.1 主要仪器设备与试剂材料
1.1.1 仪器设备
AxiosMAX型波长色散X射线荧光光谱仪,最大功率为4.0 kW,最大激发电压为60 kV,最大电流为160 mA;SSTmAX超尖锐端窗铑靶X光管,SuperQ5.1A软件,氦气光路系统,分析范围B~U,荷兰PANalytical公司。分析天平,精度为0.01 mg,德国Sartorius公司。磁力搅拌器,最大转速为1 400 r/min。电子秤,精度为0.01 g。
1.1.2 试剂材料
试验用标准物质为八氧化三铀中铀和杂质元素成分分析标准物质GBW04205(铀质量分数84.711%)和八氧化三铀成分分析标准物质GBW04201;选用定值样1#、定值样2#、进口八氧化三铀样品为试验材料;硝酸、磷酸,均为分析纯;碳酸锶(SrCO3)、氦气,纯度均优于99.99%;试验用水为二次去离子水。
1.2 试验方法
1.2.1 样品前处理
称取样品1.00 g(精确到0.01 mg)及105℃烘干4 h的碳酸锶0.600 g(精确到0.01 mg)于250 mL锥形瓶中,用去离子水冲洗瓶壁,加入15 mL磷酸和2 mL硝酸,置于200℃电炉上,加热消解至清亮;取下稍冷后,放入磁转子,用去离子水冲洗瓶壁加入水至100 mL,再加入10 mL硝酸,置于200 ℃电炉上,加热10 min取下;加水至200 mL,用磁力搅拌器搅拌1 min,用一次性塑料吸管吸取20 g溶液,置于XRF液体样品杯中,待测。
1.2.2 样品测量
输入按1.2.1步骤制备的溶液名称,在氦气氛围中用波长色散X射线荧光光谱仪测量样品元素分析线的强度,测量条件见表1。
2 结果与讨论
收起
2.1 样品前处理条件的选择
2.1.1 天然铀产品称样量的确定
通常,根据质量具有代表性、方法误差允许、客户要求、溶样条件等原则确定称样量。依据贸易方规定的称样量不应低于1.00 g的要求,对最低1.00 g是否满足准确度要求进行验证。实验室采用精度为十万分之一的天平,依据天平称量不确定度为0.03 mg,则称样的相对标准不确定度为0.03×10-3/1.00×100%=0.003%,满足天然铀贸易中规定的准确度小于0.1%的要求。同时,为避免天然铀的溶解损失,确定天然铀产品(U3O8)的称样量为1.00 g,即贸易方规定的最小称样量。
2.1.2 内标物称样量的确定
一般内标物和分析物的谱线强度应基本相同,XRF采用内标法精密度更小[16-17]。依据内标元素和分析元素的吸收和增强效应要基本相同的原理,铀的分析线为U-Lα 0.091 1 nm,选择吸收和增强效应基本相同的相邻谱线确定Sr-Kα 0.087 7 nm为内标特征线。实验室常见的锶化合物有SrSO4、SrCO3、Sr(NO3)2、SrCl2等,SrSO4是一种微溶物质,在酸溶液中易沉淀;SrCl2在空气中易形成带结晶水的化合物,不稳定;Sr(NO3)2是一种易制爆品,且难以获得高级别的纯度,因此,SrSO4、Sr(NO3)2、SrCl2均不符合内标物应是一种已知含量的物质或高纯物质的选取条件。
本法选择纯度大于99.99%且易溶于酸的SrCO3作为锶内标化合物。称取1.00 g八氧化三铀标准物质GBW04205和不同量的SrCO3,用磷酸-硝酸消解,上机测试其光强度,并计算铀锶的强度比,SrCO3称样量确定试验见表2。可以看出,当内标物碳酸锶称样质量在0.600 20 g时,其光强度和1.00 g八氧化三铀标样的光强度接近。因在日常分析的天然铀样品中铀含量与标样接近,因此本法内标物SrCO3称样质量以0.600 g为宜。
2.1.3 溶样方式的确定
XRF前处理制样方式,通常有压片法、熔片法和溶液法,鉴于天然铀产品具有放射性,为防止压片法、熔片法在压片和搅拌环节中产生吸入性粉尘辐射危害,本法采用溶液制样方式。溶液制样遵循先消解后提取的原则,消解可保证样品溶解完全,提取可保证酸度的一致性及残渣的溶解。消解过程中先加入15 mL磷酸、2 mL硝酸;由于在消解过程中硝酸易挥发,因此在消解完全后,再加入10 mL硝酸溶解提取。这样既可保证硝酸浓度的一致性,在硝酸溶液下也能增加天然铀和内标物的溶解度。
2.1.4 定容体积的确定
样品称样质量为1.00 g,内标物(碳酸锶)称样质量为0.600 g,在消解样品时加入磷酸,混合溶液的盐分和黏度均较大,天然铀产品中含有的硫酸根[18-19]可能会和锶盐形成SrSO4。因SrSO4微溶,为增加其溶解度,定容体积以200 mL为宜。
2.1.5 混匀和测量取液方式确定
溶液在定容后,混匀。混匀方式一般有玻璃棒搅拌、磁力搅拌、震荡摇匀等。玻璃棒搅拌、震荡摇匀均存在溶液撒溅和二次污染的风险;而聚四氟乙烯磁子具有防止溶液爆沸的功能,本法选择磁力搅拌混匀方式。
XRF溶液法是将溶液移至液体样杯中,用X射线照射液体表面,同时测量目标元素的特征X射线荧光强度,依据强度或强度比值大小以及曲线计算出目标物的含量。实验室移取溶液一般采用移液管和移液枪方式,移液管取样有润洗、清洗步骤,存在操作人员对天然铀放射性溶液接触的风险;移液枪在锥形瓶中取液,也存在放射性污染枪体的风险。考虑到内标法可抵消测量体积的影响,分析中只需粗略控制测量体积,本方法采用一次性塑料吸管和电子秤控制取液体积的方法,降低天然铀接触风险。
2.2 仪器测量条件的选择
2.2.1 特征X射线的选择
特征X射线产生于原子内层电子的跃迁,基本上与化学状态无关,其波长仅与原子序数相关。同一原子序数的不同线系相对强度K系>L系>M系,铀和锶的主要特征X谱线和对应的相对强度[20]135见表3。
由表3可见,U-Kα1的激发电势为115.610 keV,实验室的X射线荧光仪电压无法做到激发铀的K线系。基于优先选取相对强度最大的谱线原则,同时考虑基体中谱线重叠的干扰,确定特征X谱线以U-Lα1,Sr-Kα1为宜。
2.2.2 通道面罩的选择
在准直器和试样间装有可供选择的通道面罩(24、30、34 mm),其作用相当于光栅,可消除样杯盒发射的X射线荧光干扰。由于试验所采用的液体样杯内径为37 mm,为确保样品强度最大,选择34 mm的通道面罩。
2.2.3 准直器的选择
准直器由一组间隔相等的平行金属箔叠积而成,用于截取来自样品或晶体的发散光,汇聚成一束基本平行的光,然后投射到晶体表面或探测器窗口。准直器分为初级准直器和次级准直器。初级准直器安装在样品和晶体之间,主要用于提高光束的准直度和分辨率,消除样品的不均匀性影响,有150 μm和300 μm两种规格;次级准直器设置在晶体和探测器间,可排除晶体的二次发射,降低背景值,为固定规格。溶液中U、Sr浓度较高,为提高仪器分辨率,选择150 μm的初级准直器。
2.3 基体校正及结果计算
溶液法制样是将样品消解为酸溶液,可以消除样品间密度和成分的不均匀性,以及粒度、矿物效应;同时可降低各组分间的吸收-增强效应[21]。但铀溶液仍然存在组分间吸收-增强效应、不同浓度的酸基体、液体试样气泡、热膨胀、体积不一致等因素的影响,需要进行基体校正。
前述分析了Sr-Kα和U-Lα为相邻谱线,吸收和增强效应基本一致,因此实验采用内标法即铀和锶的强度比(IU/ISr)校正基体差异和物理状态不一致的影响。结果计算公式为
wU=[IU/ISr×E+B]/mU×100%,
式中:wU—U元素的含量,%;IU—U元素的测量强度,kcps;ISr—Sr元素的测量强度,kcps;E—校准曲线的斜率;B—校准曲线的截距;mU—天然铀产品的称样量,g。
2.4 工作曲线
称取GBW04205标准样品0.93、0.95、0.97、0.99、1.01、1.03 g(精确到0.01 mg),对应的铀质量为0.787 81、0.804 75、0.821 70、0.838 64、0.855 58、0.872 52 g; 同时称取碳酸锶0.600 g(精确到0.01 mg)。按照1.2.1步骤制成溶液,依次用X射线荧光光谱仪测量铀和锶的荧光强度,对应铀强度分别为414.332 0、411.691 4、411.917 0、433.718 0、428.178 8和436.230 3 kcps;对应锶强度分别为438.174 0、426.853 4、417.981 8、431.378 9、417.576 6和416.895 4 kcps。以铀、锶荧光强度比值(IU/ISr)为横坐标,铀质量(mU)为纵坐标,绘制工作标准溶液曲线,结果见图1。
由图1可见,方法工作曲线为y=83.852x-0.425 5,线性相关系数(R2)为0.999 8,铀、锶强度比与铀质量呈良好的线性关系。
2.5 方法精密度试验
选取6个不同批次的样品,每个样品分别称取6份,按1.2.1步骤以及优化的前处理和仪器测量条件进行铀的精密度试验,测定结果见表4。铀测定结果的相对标准偏差(RSD)在0.031%~0.050%,满足实际生产中精密度小于0.1%的要求,方法精密度较好。
2.6 方法准确度试验
取4个标准物质(含2个定值样)按未知样品进行检测,结果见表5。
由表5可见,本法测定结果与标准物质推荐值之间的相对误差较小,满足贸易质控中规定标准样品的测定值与标准值差限值(0.1%)要求,方法准确度较好。
2.7 方法比对试验
抽取20个样品采用本方法进行测试,为验证方法的可靠性,同时用电位滴定法进行比对试验,并计算2种方法的绝对偏差,结果见表6。2种方法测定结果的绝对偏差为0.010%~0.126%,表明采用X射线荧光法测定铀的方法准确可靠,满足贸易中不同方法差值应小于0.2%的要求。
3 结论
收起
建立了采用溶液法制样—波长色散X射线荧光光谱法测定天然铀产品中铀含量的方法,并对样品前处理和仪器测量条件进行了优化。该法优于传统的电位滴定法,精密度高,准确度好,能够满足天然铀产品快速批量分析的要求。
基金
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  • 中国核工业地质局XT-CT铀矿物原位识别技术及X射线荧光法精密测定天然铀产品中铀含量的方法研究项目(2019-17-04)
文献
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doi: 10.13426/j.cnki.yky.2023.04.03
  • 接收时间：2023-04-12
  • 首发时间：2025-07-04
  • 出版时间：2024-02-20
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  • 收稿日期：2023-04-12
基金
中国核工业地质局XT-CT铀矿物原位识别技术及X射线荧光法精密测定天然铀产品中铀含量的方法研究项目(2019-17-04)
作者信息
    1 湖北三〇三库,湖北 武汉 430000
    2 核工业230研究所,湖南 长沙 410007
    3 湖南省伴生放射性矿产资源评价与综合利用工程技术研究中心,湖南 长沙 410007
    4 中国铀业有限公司,北京 100013
    5 中国原子能工业有限公司,北京 100032

通讯作者:

柳金良(1986—),男,湖南衡东人,学士,高级工程师,主要从事分析化学、仪器分析研究工作。
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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