ICP—MS分析人血清中微量元素

用ＩＣＰ－ＭＳ分析人血清中２２种元素，为克服基体抑制效应，采用内标元素Ｓｃ和Ｉｎ分别校正质量数８０以下和８０以上元素的测定，获得满意的结果，通过对牛血清标准物质的测定，检验分析结果的准确性和方法的可靠性。     

献血员血清中20种元素的ICP-MS测定

用电感耦合等离子体质谱（ＩＣＰ－ ＭＳ） 测定献血员血清中２０ 种元素, 采用多元素内标法校正基体效应引起的系统误差, 加入内标元素Ｓｃ 、Ｉｎ 和Ｔｌ 分别校正质量数＜ １００ 、１００ ～１８０ 和＞ １８０ 的元素测定, 用牛血清标样ＧＢＷ ０９１３１ 为质控标准物质, 检验方法的可靠性。 测定了献血组和健康对照组血清中微量元素含量, 进行数理统计, 检验其差异性。     

产妇血及其新生儿脐带血中铁、锌、铜、硒含量的研究

选取包头市区正常产妇６８名及其所生新生儿作为研究对象。分娩后抽取产妇肘静脉血及新生儿脐动脉血，分析其血清中铁、锌、铜、硒的含量．研究结果揭示：新生儿脐带血清中铁、铜、硒的含量均高于产妇血清中的含量，铁与铜有显著性差异（Ｐ＜０．０５），硒的差异不显著（Ｐ＞０．０５）；而锌则相反，新生儿脐带血清中的含量低于产妇血清中的含量，二者有高度显著性差异（Ｐ＜０．０１）。产妇血清中Ｆｅ／Ｚｎ、Ｃｕ／Ｚｎ、Ｓｅ／Ｚｎ比值分别为３．８３、２．７８、０．０８；而新生儿脐带血清中Ｆｅ／Ｚｎ、Ｃｕ／Ｚｎ、Ｓｅ／Ｚｎ比值则各为９．５６、６．８０、０．１９，进一步说明新生儿脐带血清中的锌含量降低，其它元素含量增加。     

电热蒸发进样电感耦合等离子体原子发射光谱（ETV－ICP－AES）联用技术研究

本文采用国产部件组装了一套ＥＴＶ－ＩＣＰ－ＡＥＳ仪器体系，对装置的连接及操作参数进行优化。深入系统地考察了分析物的蒸发过程和传输过程，提出了难熔元素的蒸发和传输机理。研究了ＥＴＶ－ＩＣＰ－ＡＥＳ中基体效应，提出了以聚四氟乙烯为氟化剂，氟化辅助ＥＴＶ－ＩＣＰ－ＡＥＳ测定难熔元素的新方法，应用于环境和生物标样中痕量元素分析，获得满意结果。     

慢性支气管炎与17种元素的关系分析

采用ＩＣＰ－ＭＳ法对１３例慢性支气管炎急性发作期患者血清１７种元素进行测试，并与对照组比较，结果Ｓｒ，Ａｌ，Ｆｅ，Ｚｎ，Ｉ，Ｂ，Ｃａ等７种元素有显著差异，提示患者体内存在多种元素代谢紊乱，建议在治疗过程中注意纠正元素代谢紊乱，以利于改善病情。     

气相色谱－原子发射光谱联用仪测定18种安眠镇静药的元素比例及其在中毒病人全血样品中的应用

采用气相色谱－原子发射光谱联用仪（ＧＣ－ＡＥＤ）测定了１８种安眠镇静药的元素组成和元素比例。根据气相色浴－质谱（ＧＣ－ＭＳ）测定的分子量数据推测出它们的分子式，结果与实际值一致。以元素组成、元素比例和保留时间为判据，对一例中毒患者全血样品进行了定性分析，发现血中含有苯巴比妥。     

气相色谱－原子发射光谱联用仪测定18种安眠镇静药的元素比例及其在中毒病人全血样品中的应用

 采用气相色谱－原子发射光谱联用仪（ＧＣ－ＡＥＤ）测定了１８种安眠镇静药的元素组成和元素比例。根据气相色浴－质谱（ＧＣ－ＭＳ）测定的分子量数据推测出它们的分子式，结果与实际值一致。以元素组成、元素比例和保留时间为判据，对一例中毒患者全血样品进行了定性分析，发现血中含有苯巴比妥。     

全反射X射线荧光光谱法同时测定地气样品中锰,镍,铜,锌,铅,铷和锶

论述了利用自行研制的有３个反射体的全反射分析装置，用钼靶Ｘ光管激光发，以Ｓｅ为内标，同时测定了地气样品中Ｍｎ，Ｎｉ，Ｃｕ，Ｚｎ，Ｐｂ，Ｒｂ和Ｓｒ等元素。对纳克级元素含量，方法的精密度为７．２％，绝对检出限为１０＾１０－１０＾－１１ｇ。其分析结果的准确度与无火焰原子吸收相符。     

全反射X射线荧光光谱法同时测定地气样品中锰、镍、铜、锌、铅、铷和锶

论述了利用自行研制的有３个反射体的全反射分析装置，用钼靶Ｘ光管激发，以Ｓｅ为内标，同时测定了地气样品中Ｍｎ、Ｎｉ、Ｃｕ、Ｚｎ、Ｐｂ、Ｒｂ和Ｓｒ等元素。对纳克级元素含量，方法的精密度为７．２％．绝对检出限为１０－１０～１０－１１。其分析结果的准确度与无火焰原子吸收相符。     

微乳液的增敏作用研究—5—Br—PADAP分光光度测定锰（Ⅱ）

以含水量８０％的Ｏ／Ｗ型ＳＤＳ／正丁醇／正庚烷／水微乳液为介质，以５－Ｂｒ－ＰＡＤＡＰ为显色剂，分光光度测定Ｍｎ（Ⅱ）。表观摩尔吸光系数ε５７０－１．０８×１０＾ｄ５Ｌ．ｍｏｌ＾－ｄ１．ｃｍ＾－１，与相同含水量的ＳＤＳ胶束体系相比，测定灵敏度有显著提高，改善了实验条件。方法用于铝合金和茶叶中Ｍｎ（Ⅱ）的测定，结果令人满意。     

Separation of lithium from sodium,beryllium and other elements by cation-exchange chromatography in nitric acid-methanol

Lithium can be separated from sodium, beryllium and many other elements by eluting lithium with 1 M nitric acid in 80% methanol from a column of AG50W-X8 sulphonated polystyrene cation-exchange resin. The separation factor is not quite as large as that in 1 M hydrochloric acid in 80% methanol, but many elements, such as Zn, Cd, In, Pb(II), Bi(III) and Fe(III), which form chloride complexes in 1 M HCl-80% methanol are retained quantitatively together with Na, Be, Mg, Ca, Mn(II), Al, Ti(IV), U(VI), and many other elements, when 1 M HNO3-80% methanol is used for elution of lithium. A method for the accurate determination of traces of lithium in rock samples is described, and some results obtained are presented together with relevant distribution coefficients, elution curves and results for the analysis of synthetic mixtures.     

Determination of the chemical composition of the South Pole aerosol by instrumental neutron activation analysis

Atmospheric particulate samples were collected at the geographic South pole, using cellulose and polycarbonate filters and cascade impactors. The samples were analysed for 40 elements by instrumental neutron activation analysis. From the filter samples atmospheric concentrations for 33 elements could be obtained. The highest atmospheric concentrations were found for S: 49 ng/standard cubic meter (SCM) of air, Na: 3.3 ng/SCM and Cl: 2.6 ng/SCM. In the cascade impactor samples, only a few elements were observed above blank. For these elements it could be concluded that they are associated for over 80–90% with submicron size paricles.     

藏药牦牛角中微量元素及其特征

采用日立１８０／８０原子吸收光谱仪、ＷＹＤ－２型氢化物原子荧光光谱仪测定了传统藏药牦牛角中的Ｃｕ、Ｚｎ、Ｆｅ、Ｍｎ、Ｃｏ、Ｓｅ、Ａｓ,Ｈｇ、Ｐｂ、Ｃｄ等１０种元素含量。结果表明,由于牦牛生活在青藏高原这一特独生境条件下,其角含有丰富的微量元素。     

Quantitative separation of gallium from zinc, copper, indium, iron(III) and other elements by cation-exchange chromatography in hydrobromic acid-acetone medium

Gallium can be separated from Zn, Cu(II), In, Cd, Pb(II), Bi(III), Au(III), Pt(IV), Pd(II), Tl(III), Sn(IV) and Fe(III) by elution of these elements with 0.50M hydrobromic acid in 80% acetone medium, from a column of AG50W-X4 cation-exchange resin. Gallium is retained and can be eluted with 3M hydrochloric acid. Separations are sharp and quantitative except for iron(III) which shows extensive tailing. With 0.20M hydrobromic acid in 80% acetone as eluting agent, all the species above except iron(III) and copper(II) can be separated from gallium with very large separation factors. Only a 1-g resin column and small elution volumes are required to separate trace amounts and up to 0.5 mmole of gallium from more than 1 g of zinc or the other elements. Hg(II), Rh(III), Ir(IV), Se(IV), Ge(IV), As(III) and Sb(III) have not been investigated, but should be separated together with zinc according to their known distribution coefficients. Relevant elution curves, results for the analysis of synthetic mixtures and for amounts of some elements remaining in the gallium fraction are presented.     

Multi-element characterization of tobacco smoke condensate

In an interlaboratory study, 57 elements were assayed and 35 of them determined in cigarette smoke condensate of two different cigarette brands. The methods applied included inductively coupled plasma mass spectrometry, total reflection X-ray fluorescence analysis, instrumental neutron activation analysis and atomic absorption spectrometry. The main components carbon, hydrogen and nitrogen were determined by a CHN-combustion method. Sulphur was determined by a method based on the formation of hydrogen sulphide and precipitation micro-titrimetry. Considering the occurring concentrations and the toxicity, the most relevant elements in cigarette smoke condensate are arsenic, cadmium and lead which have relatively high transfer rates from tobacco into smoke.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday     

Design and Critical Evaluation of Improved Electrothermal Vaporization Flame Atomic Absorption/Emission Spectrometry for Direct Determination of Trace Metals in Microliter Samples

Improved tantalum-filament electrothermal vaporization flame atomic absorption spectrometry (ETV-FAAS) was developed and used for the direct determination of trace metals in microliter samples. Studies have been made for optimizing the experimental parameters that affect the performance of sample introduction to the flame. Linear calibration graphs are shown for the elements Mn (10–200 ng), Pb (5–200 ng), Cu (5–100 ng), Cd (5–50 ng), Li (1–20 ng), Na (10–80 ng), and K (10–80 ng), using only 10 μl of standard solutions. The detection limits of the elements by ETV-FAAS were much lower than those of conventional FAAS. Absolute detection limits for all elements studied were less than 0.1 ng. The relative standard deviation values for the elements were <10%. The developed method was also applied to the determination of lead concentration in blood samples.     

Distributions of major-to-ultratrace elements among the particulate and dissolved fractions in natural water as studied by ICP-AES and ICP-MS after sequential fractionation.

In order to elucidate the distributions of the elements among the particulate and dissolved fractions in pond water, major-to-ultratrace elements in different sizes of particles as well as in the filtrate passed through the 0.05 microm filter were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The different sizes of particle samples (ca. 100-300 microg each) were collected on the membrane filters with pore sizes of 10, 3.0, 1.2, 0.4, 0.2 and 0.05 microm, respectively, by sequential fractionation. As a result, about 40 elements in different sizes of particles could be determined by ICP-AES and ICP-MS, after acid digestion using HNO3/HF/HClO4. Then, the fractional distribution factors of major-to-ultratrace elements among the particulate and dissolved fractions were estimated from the analytical results. The total contents of Al, Fe, Ti, REEs (rare earth elements), Bi, Pb and Ag in the particulate fractions (larger than 0.05 microm) were more than 80-90%, while those of Ca, Sr, Cs, W, Ba, Mn and Co in the dissolved fraction, which corresponded to the filtrate passed through the 0.05 microm membrane filter, were more than 80%. It was further found that the fractional distributions of Cu and Zn in the dissolved fraction were ca. 50%. In addition, the enrichment factors (EFs) of the elements in the particulate fractions with particle sizes of 3.0-10 microm and 0.05-0.2 microm were estimated to elucidate their geochemical characteristics in natural water.     

南方紫花苜蓿植株中微量元素含量分析

采用原子吸收分光光度法对12个苜蓿品种植株的地上部分Fe、Zn和Mn等3种微量元素含量进行了测定分析。结果表明,紫花苜蓿地上部全株中人体所需Fe、Mn和Zn等微量元素含量丰富,Fe质量分数为211.35~300.19μg/g;Zn质量分数为42.80~57.65μg/g;Mn质量分数为55.31~91.19μg/g。并且,不同品种植株中微量元素含量由高到低顺序均为Fe、Mn、Zn。     

Determination of rare earth and other trace element abundances in human kidney stones and brain tissue by instrumental neutron activation analysis

We have used INAA to analyze more than 30 minor and trace elements in 10 human kidney stones (phosphate and oxalate types). In addition we also analyzed human brain tissue samples for trace elements by INAA to determine the limitations of the method. Samples were taken from the temporal and frontal cortex of the brain of a patient that suffered from dialysis encephalopathy (where an increased Al content is expected), as well as a number of control samples. Trace elements were analyzed to study possible compositional differences other than the Al content. The analyses were done using large volume HPGe detectors; because of the low abundances, accuracy and precision vary between 3–80% for individual elements. We found a difference between the rare earth element (REE) patterns for apatite and oxalate kidney stones, and a fractionation compared to typical REE contents in plants. For the brain samples there is evidence for differences between the dialysis patient and the control samples not only for Al, but also for some other elements including the REEs, but most differences are minimal, and may not be significant.     

四川乌蒙山区表层土壤中养分元素地球化学特征与评价

土壤中养分元素作为植物生命物质的来源具有重要作用。四川乌蒙山区土地质量地球化学调查评价显示,麻城乡、摩尼镇以较一等和二等土地为主。表层土壤中有效铁、铜、锌、硫的含量丰富和很丰富占比超过80%,有效钼和锰的含量丰富和很丰富占比超过50%。部分地区磷、有机质、氧化钙、硼较为缺乏,需要根据区域元素缺乏种类,分布范围,有针对性地补施相应的肥料。