X—射线荧光光谱测定钙质贝壳中17种元素

为适应古地球化学环境和古生态研究的需要,本文实验了用XRF粉末压片法测定贝壳中17种元素。文中重点讨论了少量样品压片和薄片(及薄样)装样方法。     

全反射X射线荧光光谱法测定松子仁中16种矿物元素的含量

提出了全反射X射线荧光光谱法测定松子仁中钾、钙、钛、钒、铬、锰、铁、钴、镍、铜、锌、砷、硒、铷、锶和铅等16种矿物元素的含量。松子仁样品在MWS-2微波消解系统中,于180℃下微波消解50min,以镓为内标物。各元素的检出限在0.003~0.142mg·kg-1之间。应用所提出的方法分析花粉标准物质(GBW 10026),所得测定值与认定值一致。采用本方法和电感耦合等离子体质谱法对松子样品进行测定,结果表明:两者的测定结果无显著性差异,本方法测得各元素的相对标准偏差(n=6)在0.8%~4.7%之间。     

微波消解-ICP-AES法测定氧化铝中杂质元素

采用微波消解法,将样品用磷酸溶解,用ICP-AES测定氧化铝中Na、K、Ca、Si、Fe、Ti、Mn、Zn、Cu、V、Cr和B等12种杂质元素,采用测定标样、加标回收试验和精密度试验证明该方法简便快速,准确可靠。     

ICP-AES法测定枸橼酸铋制剂中的杂质元素

采用微波消解的方法溶样,用ICP-AES法同时测定了枸橼酸铋制剂中的Ca、Mg、Cr、Mn等杂质元素的含量,考察了微波消解的条件和基体元素Bi对被测元素分析谱线强度的影响。方法的检出限为0．6～16ng／mL,相对标准偏差为1．58％～6．64％,加标回收率为92％～104％。该方法简单、快速、准确,结果令人满意。     

微波消解-ICP-AES法测定化妆品中8种有毒元素

采用微波消解-电感耦合等离子体发射光谱法(ICP-AES)对化妆品中Ba、Pb、Cd、Sb、Se、Cr、Hg、As8种有毒元素进行同时测定,通过试验确定了仪器参数和各元素的分析线。8种元素的浓度在0～10mg/L均与响应值呈线性关系,相关系数大于0.9995。8种元素测定结果的相对标准偏差均小于10%(n=3),方法检测限小于0.04mg/kg。样品中各元素的加标回收率为82.1%～108.7%。该方法适用于大批量的化妆品检测。     

微波消解ICP-MS法测定锂离子电池石墨负极材料中9种痕量元素

建立微波消解–ICP–MS法测定锂离子电池石墨负极材料中Al,Cr,Cu,Fe,K,Na,Ni,Pb,Zn 9种痕量元素含量的方法。采用硝酸–盐酸体系微波消解样品,稀释后用ICP–MS法测定样品消解溶液中9种痕量元素的含量。在优化仪器工作参数后,采用同位素和He模式克服质谱干扰。9种元素的质量浓度与质谱强度具有良好的线性关系,线性相关系数为0.999 1~0.999 8,检出限为0.132~3.700 mg/kg。加标回收率为98.4%~101.0%,测定结果的相对标准偏差为0.3%~3.6%(n=6)。该方法测定结果准确可靠,可用于锂离子电池石墨负极材料中痕量元素的测定。     

ICP-MS法测定赤霞珠葡萄叶片中的54种元素

以Rh作内标,建立电热板消解.电感耦合等离子体质谱(ICP-MS)同时检测葡萄叶片中54种元素的方法.在优化电子控温加热板的消解条件和仪器测定条件下,该方法对各元素的检出限为0.002～48.7 μg/L,各元素相对标准偏差在0.05%～7.0%,54种元素的加标回收率均在85%～105%范围内.国家一级标准物质灌木枝叶(GBW07602)的验证分析显示测定值与参考值基本相吻合,表明本方法具有准确、可靠、灵敏感度高及多元素同时分析等特点.应用此法,分析并比较了怀来(河北)、云南、宁夏、烟台、新疆5个葡萄酒产区赤霞珠葡萄叶片中的54种元素,结果显示这5个地区的稀土元素及必需微量元素B、V、Cr、Mn、Fe、Co、Ni、Sr、Mo、Sn的含量存在较为明显的差异.     

大洋多金属结核中27个元素的快速分析

利用飞利浦PW2400X射线荧光光谱仪测定了多金属结核中的Na2O、MgO、Al2O3、SiO2、P2O5、SO3、Cl、K2O、CaO、TiO2、V、Mn、Fe、Co、Ni、Cu、Zn、As、Rb、Sb、Y、Zr、Mo、Ba、La、Ce和Pb27种组分。采用粉末直接压片法制样,理论α系数（对分析线波长大于铁吸收限的元素）和以RhKβ１康普顿峰为背景的峰／背比法９对于其分析线波长小于铁吸收限的元素）校正元素间的吸收－增强效应,用国际锰结核标准样品建立校准方程（同时包括谱线重叠校正项）,方法经标准物质检验,具有较好准确度,能满足大洋多金属结构资源调查、评价要求。对主、次和绝大多数痕量组分,方法的相对标准偏差（ＲＳＤ,n=10）小于５％。与其他多元素分析方法相比,制样简单快速,而且是一种“环境友好”的“绿色”分析方法。     

微波消解/ICP-MS法测定镰形棘豆中18种元素含量

利用微波消解/ICP-MS法对青海省不同生长地点的镰形棘豆中18种元素进行了含量测定.方法的加样回收率在96.42%~104.29%之间,相对标准偏差在0.87%~2.13%之间,具有较高的准确度和精确度.结果表明镰形棘豆含有丰富的微量元素,同时重金属元素含量较低.试验结果为镰形棘豆的药效性和药理毒理提供了理论依据.     

Total Reflection X-ray Fluorescence attachment module modified for analysis in vacuum

Based on the design of the low cost Total Reflection X-Ray Fluorescence attachment module available since 1986 from Atominstitut (WOBRAUSCHEK-module) which can be attached to existing X-ray equipment, a new version was developed which allows the analysis of samples in vacuum. This design was in particular possible as the Peltier cooled light weight Silicon Drift Detector is following all adjustment procedures for total reflection as angle rotation and linear motion. The detector is mounted through a vacuum feed and O-ring tightening to the small vacuum chamber. The standard 30 mm round quartz, Si-wafer or Plexiglas reflectors are used to carry the samples. The reflectors are placed on the reference plane with the dried sample down looking facing in about 0.5 mm distance the up looking detector window. The reflectors are resting on 3 steel balls defining precisely the reference plane for the adjustment procedure. As the rotation axis of the module is in the plane of the reflector surface, angle dependent experiments can be made to distinguish between film and particulate type contamination of samples. Operating with a Mo anode at 50 kV and 40 mA with a closely attached multilayer monochromator and using a 10 mm² KETEK silicon drift detector with 8 μm Be window, a sensitivity of 70 cps/ng for Rb was measured and detection limits of 2 pg were obtained.     

微波消解石墨炉原子吸收光谱法测定松花粉中铅的测量不确定度评定

介绍了石墨炉原子吸收光谱法测定松花粉中铅的不确定度评定方法。通过不确定度评定得出不确定度分量的主要来源为样品制备过程所带来的不确定度,其中,消解样品所引入的不确定度贡献最大;根据最小二乘法拟合校准曲线计算的标准不确定度次之;而重复性实验以及标准储备液校准稀释所带来的不确定度相对于前两者小很多。     

Total Reflection X-Ray Fluorescence Determination of Rare Earth Elements in Mineral Water Using a Combined Preconcentration Technique

A combined approach for the simultaneous determination of lanthanum, cerium, praseodymium, neodymium, and samarium in mineral water in the range from?·?10^?2 to 10¹?µg/L by total reflection X-ray fluorescence analysis is reported. The combined technique of preconcentration of the rare earth elements ions includes the codeposition of their hydroxides on a collector and dispersive liquid–liquid microextraction by chloroform to form complexes with 1-(2-pyridylazo)-2-naphthol. The results for the determination of lanthanum and light lanthanides in natural water samples with the combined approach are in good agreement with measurements obtained by inductively coupled plasma–mass spectrometry.     

微波消解-ICP-AES法同时测定绞股蓝中4种微量元素

采用微波消解法,以HNO3-H2O2对样品进行处理,用电感耦合等离子体发射光谱法(ICP-AES)同时测定了绞股蓝中的铁、锰、铜、锌4种微量元素。结果表明,所测样品中的元素含量按铁、锰、锌、铜顺序递减,各元素测定结果的相对标准偏差在1.0%~3.8%之间,回收率在88%~97%之间。方法简单,有实用意义。     

微波消解-电感耦合等离子体原子发射光谱法测定膨润土中6种元素

膨润土样品用硝酸、盐酸、氢氟酸在超级微波消解仪中进行消解,消解完毕后加入高氯酸加热除去有机物、碳类。采用电感耦合等离子体原子发射光谱法测定样品溶液中钙、镁、磷、锰、铁、钛等6种元素的含量。6种元素的质量浓度在一定范围内与其对应的发射强度呈线性关系,方法的检出限(3s)为0.001~0.009mg·L-1。方法应用于膨润土样品的分析,测定值的相对标准偏差(n=11)为0.74%~2.7%。用标准加入法做方法的回收试验,测得回收率为96.0%~102%,方法测定值与X射线荧光光谱法测定结果相符。     

Quantitative determination on heavy metals in different stages of wine production by Total Reflection X-ray Fluorescence and Energy Dispersive X-ray Fluorescence: Comparison on two vineyards

The purpose of this study is to determine the elemental content, namely heavy metals, of samples of vine-leaves, grapes must and wine. In order to assess the influence of the vineyard age on the elemental content throughout the several stages of wine production, elemental determinations of trace elements were made on products obtained from two vineyards aged 6 and 14 years from Douro region. The elemental content of vine-leaves and grapes was determined by Energy Dispersive X-Ray Fluorescence (EDXRF), while analysis of the must and wine was performed by Total Reflection X-ray Fluorescence (TXRF).     

电感耦合等离子体质谱法测定工业纯铁中13种元素

工业纯铁样品用盐酸、硝酸、氢氟酸微波消解,消解液用水定容至100.0mL,采用电感耦合等离子体质谱法测定上述溶液中硼、镁、钙、钛、铬、镍、铜、锆、铌、锡、锑、铅、铋等13种元素的含量。采用内标法定量,13种元素的线性范围均为0.000 10%~0.015 00%,检出限(3s)为0.24~0.66μg·L^-1。用标准加入法做方法的回收试验,测得回收率为84.0%~106%。方法应用于纯铁标准样品(GBW 01401b、GBW 01402g、SRM 2167、YSBC 11247-2007)的分析,测定值与认定值相符,测定值的相对标准偏差(n=6)为0.80%~9.6%。     

ICP-OES同时测定三元复合肥中六种微量元素

用微波消解／电感耦合等离子体发射光谱法（ICP—OES）同时测定了三元复合肥中的铜、铁、锌、镍、锰、钼6种微量元素。结果表明,该法具有简便、快速、结果可靠、检出限低、良好的精密度、精确度、高回收率以及能够同时测量多种元素的优点;通过对比实验测量得到了有效态微量元素的浓度和微量元素的总量,结果显示大部分微量元素是以有效态形式存在于复合肥中。因此,该法可以作测量复合肥类产品中的微量元素的一种参考使用方法。     

微波消解-ICP-OES测定蜂花粉中钙元素的含量

采用微波消解-ICP-OES法测定了4种蜂花粉中钙元素的含量,测定用标准曲线方程为：y=129．89 x-19．367,线性相关系数r=0．9998。结果表明,蜂花粉中含有大量的钙元素,4种蜂花粉中钙元素测定最高质量分数为1399mg／kg,最低质量分数为1171mg／kg,平均质量分数为1302．5mg／kg,可见蜂花粉是极具保健价值的营养品。     

Application of Total Reflection X-Ray Fluorescence Spectrometry in the Textile Industry

 In the present study, the determination of arsenic, lead, cadmium, chromium, cobalt, copper, nickel, mercury and zinc in various cloth samples produced in Kayseri-Turkey was performed after extraction with artificial sweat solution and decomposition with nitric acid. TXRF is shown to be suitable for the determination of 7 trace elements, down to the 0.001 (cobalt) to 0.004 (copper) mg/kg level in textile extract except for mercury and cadmium. The extractable part of the toxic metals by artificial sweat solution is relatively low. In a few extracts the concentration values of Pb and Ni have exceeded their critical values of 0.2 mg/kg for lead and 1.0 mg/kg for nickel given by ?ko-Tex and determined for babys cloths. In addition, it was observed that the element pattern of textile samples resembled ‘finger print type’, TXRF-spectra. This technique can also be used for the identification of textile sample in forensic investigation. Received April 16, 2001 Revision October 1, 2001.