等离子炬-质谱技术测定白菜、萝卜、大豆、土壤中的痕量锰、钴、镍、铜、锌、砷、钼和锶

营养学家们已经确定了锰、钻、镍、铜、锌、砷、钼和锶等10多种人体所必需的痕量元素,它们对于维持人体的健康和长寿起着重要的生理作用。本文首次应用等离子炬-质谱技术测定了白菜、萝卜、大豆和土壤中这八种痕量元素的含量,并报告了它们的测定结果和标准偏差,其中土壤样品的测定值与参考值相比较,经 T 检验,两者之间在统计学上,没有显著性差异。实验证明该方法可对多种痕量元素同时定性、定量分析。操作简便、快速,灵敏度高;方法准确可靠,重现性好。为开展食品卫生学、营养学的研究,提供了更为先进的测试技术。     

交互模式-电感耦合等离子体质谱(ICP-MS)法测定生态地球化学植物样品中7种金属元素

植物样品中各元素的含量,是评价土壤质量及健康的重要指标。为满足测定大批量生态地球化学植物样品中多金属元素分析要求,建立了交互模式-电感耦合等离子体质谱(ICP-MS)法测定植物样品中7种痕量金属元素的定量分析方法。讨论了ICP-MS的STD、KED(He)、交互模式3种方法测定植物样品中7种金属元素结果。结果表明,利用工作曲线法配制Hg标准溶液,更改⁸²Se在线校正方程系数为1.83,在ICP-MS的交互模式下测定植物样品中⁸²Se、⁶³Cu、⁶⁰Ni、⁶⁶Zn、¹¹¹Cd、⁷⁵As、²⁰²Hg可以得到准确可靠的结果,克服了植物样品中Se和Hg元素测定的难题。基于所建方法各元素校准曲线系数>0.999,方法检出限为0.000 4～0.08 mg/kg,加标回收率在96.2%～107%,测定GBW10010a(大米)、GBW10012(玉米)、GBW10021(豆角)3种标准物质,结果均在参考值范围内,相对标...     

Determination of trace elements in metals and alloys by atomic-absorption spectroscopy using an induction-heated graphite well furnace as atom source

An induction-heated graphite furnace, coupled to a Unicam SP 90 atomic-absorption spectrometer, is described for the direct determination of trace elements in metals and alloys. The furnace is capable of operation at temperatures up to 2400 degrees , and has been used to obtain calibration graphs for the determination of ppm quantities of bismuth in lead-base alloys, cast irons and stainless steels, and for the determination of cadmium at the ppm level in zinc-base alloys. Milligram samples of the alloys were atomized directly. Calibration graphs for the determination of the elements in solutions were obtained for comparison. The accuracy and precision of the determination are presented and discussed.     

Flow methods for the determination of elements in solutions based on sorption preconcentration and inductively coupled plasma mass spectrometry

Methods involving an on-line combination of sorption preconcentration with the determination of elements by inductively coupled plasma mass spectrometry (ICP-MS) are considered. The reasons for the effect of the composition of the solution on the analytical signals in the determination of elements, the issues related to recording of nonstationary signals, and the procedures for the sorption preconcentration of elements in the corresponding flow systems are discussed. Some examples of the determination of elements in environmental samples, biological fluids, and other samples are given.     

Simultaneous substoichiometric determination of europium and terbium based on concentration dependent distribution

Methods for simultaneous determination of europium and terbium based on concentration dependent distribution is described. With these methods, the distribution ratios of elements are measured in two types of substoichiometric systems. Possibility of determining these elements simultaneously is investigated experimentally by using two pairs of substoichiometric complexans/excess extracting agents, such as DTPA/HTTA and EDTA/HTTA. Relative errors and precisions for simultaneous determination of the elements are less than 5%.     

Present-day methods for the determination of trace elements in oil and its fractions

The development and use of instrumental methods for the determination of a wide range of trace elements in oil is considered. Special attention is paid to methods of the direct introduction of samples into spectrometers. It is shown that preliminary sample preparation is in certain cases necessary for the determination of trace elements in oil. The main methods of sample preparation of oils, including methods of extraction of a series of trace elements from crude oil (extraction, membrane, sorption, etc.), are described.     

Substoichiometric and non-destructive determination of trace impurities in high-purity optical glasses by neutron activation analysis

A method of radioactivation analysis has been developed for the determination of 17 elements as impurities in high-purity optical glasses. The substoichiometric extraction of platinum with dithizone was studied and a simple procedure was proposed for the determination of platinum. Copper and manganese were also determined substoichiometrically by the extractions with dithizone and with thenoyltrifluoracetone, respectively. The non-destructive γ-ray spectrometry using a Ge(Li) detector has been applied for the determination of the other 14 elements (Ag, Co, Cr, Eu, Fe, Ir, Sc, Zn, Cs, Hf, Rb, Sb, Ta and Tb). Impurity elements at the ppb level were analysed by the proposed method and it is shown that the method is reliable for the determination of trace impurities in high-purity optical glasses.     

Mg(OH)_2共沉淀和直接稀释联用ICP-MS法准确测定海水中的多种常量-微量元素

对海水中多种常量/微量元素分别用Mg(OH)_2共沉淀和直接稀释ICP-MS法进行方法比较研究,分别确定了这些元素适宜的准确分析方法,为海水中常量/微量元素的ICP-MS测定提供了实用的检测手段。结果表明,Mg(OH)_2共沉淀法能够实现对V,Cr,Mn,Co,Cd及稀土元素(La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu)等19种微量元素的分离富集和准确测定;10倍直接稀释法能够同时准确测定海水中B,Sr,Li,Rb,I,V,Cr,As,Cd,U,Mo,Cu,Mn 13种微量元素,但不适合Zn,Ni,Co和Pb,以及稀土元素等在海水中浓度过低元素的测定;两种方法对适宜测定的元素均操作简便快速,具有较高的准确度和精密度。这两种方法联用,就可用约50 mL的海水实现大洋和近海海水中Co,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu(这15个元素采用Mg(OH)_2共沉淀法)及B,Sr,Li,Rb,I,V,Cr,As,Cd,U,Mo,Cu,Mn(这13个元素采用10倍直接稀释法)等28种元素的准确测定。     

Simultaneous determination of traces of impurities in high-purity molybdenum and molybdenum trioxide by coprecipitation and inductively coupled plasma-atomic emission spectrometry

Summary Inductively coupled plasma-atomic emission spectrometry (ICP-AES) has been developed for a simultaneous determination of traces of non-hydride-forming elements in high-purity Mo and molybdenum trioxide. Coprecipitation of diverse elements with lanthanum hydroxide is used to separate them from the Mo matrix and for concentration. Effects of pH and amount of La on the recoveries of diverse elements are discussed. Ten elements (Co, Cr, Cu, Fe, Mn, Ni, Ti, V, Zn, and Zr) are quantitatively recovered and determined. Matrix-matched calibration solutions are used for the determination.     

XRF and TXRF techniques for multi-element determination of trace elements in whole blood and human hair samples

XRF and TXRF were established as useful techniques for multi-element analysis of whole blood and human head hair samples. Direct-XRF with different collimation units and different X-ray excitation modes was successfully used for the determination of S, P, K, Ca, Fe, and Br elements in blood samples and K, Ca, Mn, Fe elements in human hair samples. Direct analysis by TXRF was used for the determination of Rb and Sr in digested blood and human hair samples, respectively, while, the co-precipitation method using APDC for TXRF analysis was used for the determination of Ni, Cu, Zn, and Pb elements in both matrices. As a result, the improved XRF and TXRF methods were applied for multi-element determination of elements in whole blood and human hair samples in non-occupational exposed population living in Damascus city. The mean concentrations of analyzed elements in both matrices were on the reported range values for non-occupational population in other countries.     

遗传光度法用于地质样品中多组分同时测定

将遗传算法（ＧＡ）用于地质样品中１５个稀土元素同时测定,分析结果与ＩＣＰ法进行了比较,大多数组分浓度的相对误差小于１０％,个别小于１６．２％,初步验证,遗传算法可以摆脱对校准模型的依赖。文中还讨论了变异概率,交配概率,种群数大小等因素的影响。     

Development of a method for the determination of heavy metals in calcified tissues by inductively coupled plasma-mass spectrometry

Calcified tissues are good indicators of exposure to environmental pollution since the mineral phase incorporates heavy metals to which it is exposed during development. Analysis of these specimens is difficult due to the low concentration of the elements of interest compared with the high concentration of the matrix elements. ICP-MS allows rapid multielement determination of samples and a method for the determination of trace elements in calcified tissues is presented with reference to an SRM of Bone Ash (NIST 1400).     

电感耦合等离子体质谱法(ICP-MS)测定古造液酒中微量元素含量及功能评价

目的测定古造液酒中微量元素含量,并与饮用白酒、国囍酒比较,看其微量元素含量高低情况。方法采用电感耦合等离子体质谱法(ICP-MS)测定微量元素含量。检测限为0.30~3.43μg·L~(-1),回收率范围在95.4%~104.3%,相对标准偏差(RSD)范围在1.1%~2.0%。结果测定方法准确可靠。古造液酒中的微量元素明显高于饮用白酒和国囍酒。结论古造液酒富含微量元素,具有较高的临床价值。     

Beseitigung des Matrixeffekts bei der Analyse von Edelmetallspuren mit induktiv gekoppeltem Plasma

Summary Spectral interferences associated with the determination of trace contents of Au, Ag, Pt and Pd in samples with complex matrices (hydrometallurgical solutions, metallurgical products and ore processing products) were investigated. It was found that it is necessary to separate Au, Pt and Pd from the matrix elements. The results obtained with various methods for separation and pre-concentration of these elements showed that in the case of hydrometallurgical solutions adsorption on activated carbon satisfies the requirements of analytical control. For the determination of these elements in ore processing products it is necessary to use additional extraction for their preconcentration. The most suitable organic solution found for the extraction of Au, Pt and Pd and their determination with ICP is isoamyl alcohol.     

Determination of trace elements in coal and coal fly ash by joint-use of ICP-AES and atomic absorption spectrometry

Microwave-acid digestion (MW-AD) followed by inductively coupled plasma-atomic emission spectrometry (ICP-AES), graphite furnace atomic absorption spectrometry (GFAAS), and hydride generation atomic absorption spectrometry (HGAAS) were examined for the determination of various elements in coal and coal fly ash (CFA). Eight certified reference materials (four coal samples and four CFA samples) were tested. The 10 elements (As, Be, Cd, Co, Cr, Mn, Ni, Pb, Sb, and Se), which are described in the Clean Air Act Amendments (CAAA), were especially considered. For coal, the HF-free MW-AD followed by ICP-AES was successful in the determination of various elements except for As, Be, Cd, Sb, and Se. These elements (except for Sb) were well-determined by use of GFAAS (Be and Cd) and HGAAS (As and Se). For CFA, the addition of HF in the digestion acid mixture was needed for the determination of elements, except for As, Sb, and Se, for which the HF-free MW-AD was applicable. The use of GFAAS (Be and Cd) or HGAAS (Sb and Se) resulted in the successful determination of the elements for which ICP-AES did not work well. The protocol for the determination of the 10 elements in coal and CFA by MW-AD followed by the joint-use of ICP-AES, GFAAS, and HGAAS was established.     

Determination of chromium,manganese, lead and cadmium in biological samples including hair using direct electrothermal atomic absorption spectrometry

Direct analysis of solid samples employing a laboratory assembled electrothermal atomic absorption spectrometer is demonstrated to be a feasible approach for determination of trace elements in plant tissue and hair samples for special applications in plant physiology and biomedical research. As an example, the kinetics of Cr uptake by cabbage and its distribution have been measured as a function of chromium speciation in the nutrient solution. Further, longitudinal concentration gradients of Cr, Pb and Cd have been measured in hair of various population groups exposed to different levels of these elements in ambient and/or occupational environments. The techniques are validated for the determination of these trace elements by neutron activation analysis, dissolution atomic absorption spectrometry and by analysis of certified reference materials. Slurry sample introduction is found appropriate for routine trace element determination and in homogeneity testing. Direct sample introduction is indispensable in the analysis of very small (< 1 mg) tissue biopsy samples in the determination of trace element distributions.     

电感耦合等离子体质谱（ICP-MS）法测定碳质板岩样品中铂族元素

碳质板岩属黑色岩系,与多种金属(包括贵金属)成矿有密切的联系。按照常规的分析方法,硫镍试金溶剂配方都不能对贵金属元素有较好的富集,影响贵金属元素的测定。根据石墨岩中样品的成份特征,对测定铂族元素的常规硫镍试金配方进行了改进,增加了硝酸钾和氧化镁,且无需加入锇稀释剂。通过实验选择了合适比例配料,熔融后粉碎镍扣,加入盐酸分解,碲共沉淀剂富集。过滤沉淀用王水溶解。用电感耦合等离子体质谱(ICP-MS)法测定,Lu作内标,对碳质板样品中的铂族元素进行了测定。结果表明,加标回收率为85%～105%,能够满足碳质板岩中铂族元素的分析测定要求。     

ICP-MS测定高纯氧化铒中稀土杂质的研究

从同位素的选择、基体效应,内标元素的选择及仪器工作等方面对实验参数进行了优化,重点研究了等离子体功率及仪器分辩率的改变对铒基体所形成的氢化物多原子离子干扰的影响。通过提高等离子体功率、改变仪器分辨率及数学方程校正等方法,减小和剔除了ErH对Ho和Tm测定的干扰。实验中选取Cs为内标元素,测定了不同含量的高纯氧化铒样品。分析结果与标准加入法结果进行了比较,之间无显著性差异。     

电感耦合等离子体质谱法测定三水铝土矿中的15种有效稀土元素

建立电感耦合等离子体质谱法测定三水铝土矿中15种有效稀土元素的分析方法。参考三水铝土矿中有效铝的概念,提出了有效稀土元素的概念,并对三水铝土矿中稀土元素的回收利用的可行性进行了评价。模拟低温拜耳法生产氧化铝的工艺,对三水铝土矿中稀土元素溶出过程中的氢氧化钠浓度、溶出温度及时间等条件进行了试验,采用90 g/L氢氧化钠结合微波消解技术对三水铝土矿进行分解,用ICP-MS法测定有效稀土元素,有效稀土元素测定结果的相对标准偏差为0.92%~7.40%(n=7),回收率为98.6%~101.2%。该方法可用于测定三水铝土矿中有效稀土元素,能够对三水铝土矿中稀土元素的回收利用价值进行评价。     

Analytical characterization of CuInS(2) semiconductor material

Systematic analytical procedures have been developed for determination of the stoichiometry of CuInS(2) and estimation of trace elements, including dopants and impurities, in the material. Samples of CuInS(2) are digested in an oxidizing acid to ensure completely transformation into Cu(2+), In(3+) and SO(4)(2-) ions. The stoichiometry determination is made sequentially by controlled potential electro-deposition of copper, followed by its EDTA titration, titrimetric determination of indium and gravimetric determination of sulphate, in a single sample solution. The relative errors for the determination of Cu and In are found to be -0.08% and +0.11% respectively, fulfilling the requirement for accurate stoichiometry assessment; that for S is -0.66%, which though rather high is still acceptable. For the determination of trace elements in CuInS(2), multistage combined procedures are employed. Cu in the sample solution is removed by electro-deposition and In by extraction of HInBr(4) with isopropyl ether, then most of the trace elements are finally determined by atomic-absorption spectrometry, and the rest by neutron-activation analysis. All the steps involved in the procedures have been optimized by using radioisotopes as tracers. By the procedures developed, a wide range of trace elements in CuInS(2), down to submicrogram level, can be determined.