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采用ed-xrf对黄金首饰中有害元素进行定性分析的方法

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中国检验检测 2023年第2期31卷 27-30页

作者：王燕何婷黄佳南深圳市周大福珠宝制造有限公司贵金属检测中心深圳518081

传统化学分析法在分析有害元素方面存在破坏首饰、周期长、操作繁琐、试剂消耗量大和污染环境等问题,而现在有一种快速的无损检测方法即X射线荧光光谱法。本文从黄金首饰中引入有害元素的原因出发,通过采用ed-xrf(能量色散型X射线荧光... 详细信息

传统化学分析法在分析有害元素方面存在破坏首饰、周期长、操作繁琐、试剂消耗量大和污染环境等问题,而现在有一种快速的无损检测方法即X射线荧光光谱法。本文从黄金首饰中引入有害元素的原因出发,通过采用ed-xrf(能量色散型X射线荧光光谱仪)分析黄金首饰中的Pb、Hg、Cd、Cr、As这5种典型的有害元素的荧光谱图,,研究测试过程中的基体干扰因素和特征峰识别方法,探讨采用ed-xrf对有害元素进行快速、准确与可靠的定性分析对策。

关键词：有害元素黄金首饰 ed-xrf 定性分析特征峰

能量色散X射线荧光光谱法(ed-xrf)测定粗硒中的硒含量

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广州化工 2024年第2期52卷 170-172,186页

作者：周明俊张胜广东省科学院工业分析检测中心广东广州510650

针对容量法和重量法测定粗硒中硒含量过程中存在的流程长、操作繁琐等问题,本文考察了不同的压样条件,调整压力以及添加不同比例的纤维素、硼酸和碳酸锂等,最终选择采用碳酸锂作为混合剂,将粗硒粉末样品和碳酸锂粉末按照比例1∶1混匀,... 详细信息

针对容量法和重量法测定粗硒中硒含量过程中存在的流程长、操作繁琐等问题,本文考察了不同的压样条件,调整压力以及添加不同比例的纤维素、硼酸和碳酸锂等,最终选择采用碳酸锂作为混合剂,将粗硒粉末样品和碳酸锂粉末按照比例1∶1混匀,然后在压样机上用10 t压力压制成测试样片,并考察了测试样片的均匀性。在选定的工作条件下,采用能量色散X射线荧光光谱仪(ed-xrf)建立工作曲线,可以实现对粗硒中硒含量的定量测定,同时将测定结果与容量法测定结果进行对比,结果一致。本方法快速准确。

关键词：硒粗硒碳酸锂 ed-xrf 定量分析

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X荧光能谱法测定磷青铜、青铜标样中铜与锡

光谱实验室 1997年第1期14卷 55-57页

作者：李叶农郑荣华黄近丹张文芳福建省测试技术研究所福州市北环中路61号350003

本文提出X荧光能谱法测定磷青铜、青铜标样中铜与锡含量的方法。本方法采用能谱仪中定量分析软件,选择适当的工作条件,测定7个磷青铜,青铜中铜与锡、结果表明:磷青铜、青铜中铜含量在72.25％-94.50％之间,准确度＜0.2％,相对标准偏差＜0... 详细信息

本文提出X荧光能谱法测定磷青铜、青铜标样中铜与锡含量的方法。本方法采用能谱仪中定量分析软件,选择适当的工作条件,测定7个磷青铜,青铜中铜与锡、结果表明:磷青铜、青铜中铜含量在72.25％-94.50％之间,准确度＜0.2％,相对标准偏差＜05％。锡含量在4.24％-7.92％之间,准确度＜0.2％,相对标准偏差＜3％。

关键词： ed-xrf Sn Cu 磷青铜青铜标准样品锡铜测定 X荧光能谱法

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头发样的X射线荧光光谱的测定

福建分析测试 1995年第3期4卷 330-331页

作者：黄近丹郑荣华张文芳李叶农福建省测试技术研究所福州350003

本文采用 ed—xrf 法直接测定头发样中微量元素 Cu、Fe、Zn、Mg、Ca,试验了最佳工作条件,方法 RSD=1.3—7.1%,分析结果与原子吸收法测定值基本一致。

关键词： ed-xrf 头发微量元素

K Shell Fluorescence Parameters by Impact of 5.96 keV Photons on Ti and Its Compounds

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光谱学与光谱分析 2016年第12期36卷 4125-4129页

作者： O.K.KOEKSAL G.APAYDIN E.CENGZ Department of Physics Faculty of Sciences Karadeniz Technical University Trabzon 61080 Turkey

K shell fluorescence parameters of pure Ti and some of its compounds have been determined experimentally using an Ultra-LEGe detector with resolution 150 eV at *** samples were excited 5.96 keV photons emitted from a ^(55) Fe radioisotope source with 50 mCi *** experimental values of the K shell fluorescence parameters have been compared with the experimental and theoretical values available in the literature for pure Ti.

关键词： K Shell fluorescence parameters 55Fe radioactive source ed-xrf Titanium

Obsidians from Latium Settlements： Preliminary Study on Provenance and Supplying Dynamics Indexes

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Journal of Chemistry and Chemical Engineering 2012年第5期6卷 445-454页

作者： A. Macchia S. Plattner A. Manda L. Campanella D. Ferro M. Tiepolo M. Ferretti M. Malorgio A.Zarattini Italian Association of Conservation Scientists 00185 Rome ltaly Chemistry Department Sapienza University Rome 00185 Italy Istituto di Geoscienze e Georisorse 1GG- CNR c/o University of Pavia Pavia 27100 Italy CNR -lstituto per le Tecnologie Applicate ai Beni Culturali Montelibretti （Roma） 00016 Italy Superintendence for the Archaeological Patrimony of Latium Roma 00192 Italy

There are essentially six sources for obsidians in the Mediterranean Basin： Mount Arci in Sardinia, the islands of Lipari and Pantelleria in Sicily and Palmarola in Latium, as well as the islands of Melos and Gyali in the south-eastern part of Greece. Identification and quantification of principal and trace elements which compose this volcanic glass allow source tracking. The present study proposes a investigation methodology, which was developed on a sample set composed by archaeological obsidian findings from Neolithic sites in Latium; three different analytical techniques are compared： SEM-edXS, ed-xrf and LA-ICP-MS, in order to gather a wide data set to be compared with data in literature and to be processed by Principal Component Analysis （PCA） for assigning a provenance to each find.

关键词： Obsidian Latium SEM-edXS ed-xrf LA-ICP-MS.

Accuracy and Precision of Energy Dispersive X-Ray Fluorescence (edxrf) Analysis of Trace and Major Elements in Rock Standard Reference Materials Using Fine Powder

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Journal of Geoscience and Environment Protection 2023年第6期11卷 83-95页

作者： Jean Faustin Sabouang Jean Félix Beyala Ateba Cebastien Joel Guembou Shouop Josue Maya Cedric Tayou Kamkumo Lawan Loubou Mohamadou Augustin Simo National Radiation Protection Agency Yaounde Cameroon

In this work the performance of a screening analytical method for Energy Dispersive X-Ray Fluorescence (edxrf) analysis in terms of accuracy and precision was evaluated through analysis of rock standard reference materials. The method allowed the division of elements into four groups taking into account the excitation energies and measurement conditions of the sample. Two standard reference materials were used and 15 sample replicates were prepared and analyzed, then statistics were applied to assess the precision and accuracy of analytical results. The obtained results show that major compounds or elements (SiO2, P2O5, K2O, CaO, Fe2O3, Ti) can be determined in fine powder sample with a deviation lower than 15%, and a relative standard deviation in the range (1 - 10)%. The deviation was found to be lower than 5% for major compounds such as K2O, and CaO, which suggest that the edxrf is accurate in evaluating major elemental concentrations in rock samples. It was also found that the method seems to be more accurate and precise for major elements than for trace element investigation. This screening analytical method can be used for routine analysis with acceptable results, even though the method should be optimized to increase its precision and accuracy.

关键词： ed-xrf Screening Method Rock Material Accuracy Precision

On-line Determination of Rare Earth Distribution by Energy Dispersive X-ray Fluorescence Spectrometry

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On-line Determination of Rare Earth Distribution by Energy D...

基于矿物元素指纹分析技术的中国不同省份大豆产地溯源研究

第十六届全国稀土分析化学学术研讨会

作者： Qu Huayang Hu Shaocheng Lu Mingbo Wang Chaogang Hu Xueqiang Chen Jiwen NCS Testing Technology Co. Ltd. China Iron and Steel Research Institute Group

Rare earth elements（REEs） have been widely used in metallurgical machinery, electronic information, petrochemical, energy and other fields due to their unique physical and chemical properties. The REEs with enhanced optical, electrical and magnetic properties can be used to prepare advanced materials, such as fluorescent, polishing, catalytic and permanent magnetic materials. The indispensible REEs in the advanced materials, despite with trace amount, are known as "industrial vitamins". The preparation of unitary REE with high purity is fundamental to the industry of new rare earth material. The unitary REE is separated by hydrometallurgical process from rare earth concentrate with more than ten kinds of rare earth elements. The continuous separation process is evaluated by REE distributions. At present, most of the REE distributions in factories are obtained via artificial sampling coupled with ICP OES. The detection lags behind the production, resulting in unstable qualities of products. In order to determine the distributions of REEs on line, a XOR-50 rare earth distribution on-line analytical equipment was developed based on ed-xrf. A on-line determination of REE in rare earth separation process was established. The excitation voltage, current and filter were optimized according to the characteristics of REEs. The influence of the salinity was corrected by mathematical technique. The absorption enhancement effect was calculated by fundamental parameter method. The results of on-line detection are consistent with ICP OES. The relative standard deviation（n=11） of the main REEs（w＞ 1%） is less than 0.6%. The equipment can carry out automatically from the extraction solution in 1 minute. The measurement intervals can be set by the operator. Combining on-line introduction of the rare earth material, simultaneous analysis of multi elements, rapid detection in 1 minute, on-line analysis with self-starting and real-time transmission of the results, the method meets the r

关键词： ed-xrf Rare Earth Element Distribution On-line

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基于矿物元素指纹分析技术的中国不同省份大豆产地溯源研究

作者：赖翰卿吉林农业大学

学位级别：硕士

大豆作为我国重要的基础粮食作物,在全国均有广泛的种植,其品质优异,深受消费者青睐,但由于掺假和以次充好等问题屡禁不止,损害了消费者的利益以及身体健康,因此研究中国大豆产地溯源技术具有十分重要的意义。本研究主要为寻找中国不同... 详细信息

大豆作为我国重要的基础粮食作物,在全国均有广泛的种植,其品质优异,深受消费者青睐,但由于掺假和以次充好等问题屡禁不止,损害了消费者的利益以及身体健康,因此研究中国大豆产地溯源技术具有十分重要的意义。本研究主要为寻找中国不同省份地区大豆产地的矿物元素溯源指标,以提高矿物元素指纹分析技术在大豆产地溯源方面应用的准确性和稳定性。并探讨了便携式能量色散型X射线荧光光谱（ed-xrf）技术在矿物元素指纹分析技术方面应用的可行性。本研究采用电感耦合等离子质谱仪（ICP-MS）对中国5个省份主要大豆主产区（黑龙江、辽宁、内蒙古、新疆、河南）的296份大豆样品中多种矿物元素进行分析,方差分析结果表明:Mg、P、K、Ca、Mn、Fe、Cu、Zn、Rb这9种矿物元素在五大产地间存在显著差异（p＜0.05）;主成分分析结果表明:基于ICP-MS法得到的矿物元素经主成分分析后,得到三个主成分,累计方差贡献率为72.960%。主成分1有主要由Mg、P、K、Mn、Fe、Zn构成,主成分2主要由Ca、Rb构成,主成分3主要由Cu构成;但由于主成分分析并不能很好的将五个产地进行区分,本研究利用多层感知器建立大豆产地分类模型,通过优化隐藏层的神经元个数,最后确定了结构为9-5-5的产地分类模型,其训练集的准确率为100%、测试集准确率为98.3%、保持集准确率为98.4%。证明这9种矿物元素产地溯源指标结合多层感知器建立的产地分类模型可成功对中国不同省份的大豆进行分类。本研究优化了便携式ed-xrf仪器的辐照时间,发现300 s的样品辐照时间下,仪器的检测效率（检测速度、仪器精密度）最佳。采用标准样品法建立了Mg、K、Ca、Mn、Fe、Ni、Cu、Zn、Rb这9种元素的标准曲线。经过优化的仪器对上述样品中的多种矿物元素进行分析,方差分析结果表明:Mg、K、Ca、Mn、Fe、Ni、Cu、Zn、Rb这9种矿物元素在五大产地间存在显著差异;主成分分析结果表明:基于便携式ed-xrf技术得到的矿物元素经主成分分析后,得到三个主成分,累计方差贡献率为65.943%。主成分1主要由Cu、Zn、Ca构成,主成分2主要由Mg构成,主成分3主要由Mn、Ni构成;采用多层感知器构建大豆产地分类模型,优化隐藏层神经元个数,确定了结构为9-5-5的产地分类模型,模型训练集的准确率为99.4%、测试集准确率为94.1%、保持集准确率为96.5%。这证明便携式ed-xrf技术应用在食品产地溯源研究是可行的。

关键词：大豆矿物元素 ed-xrf 产地溯源主成分分析多层感知器