Distribution of 14 elements in tissues and organs of oceanic seabirds

The concentrations of 14 trace elements (Li, V, Mn, Co, Cu, Zn, Se, Rb, Sr, Ag, Cd, Cs, Pb, and Hg) were determined in tissues and organs of three species and in the liver of 11 species of seabirds. Comparatively high concentrations of Li, Co, Sr, and V were found in the femur. Cd, Se, Cu, and Mn concentrations were relatively higher in the kidney than in other tissues and organs. Rb, Cs, and Pb concentrations were rather uniform among tissues. Concentrations of essential elements such as Mn, Cu, and Co were comparable among seabird species, except high Cu concentrations in northern giant petrel. Among nonessential elements, concentrations of Cd and Hg were variable according to seabird species. Pb levels were low in all the species. High Se levels (100 microg/g dry weight) were found in the liver of black-footed albatross and grey petrel. There were significant positive correlations between Se and Cd concentrations in three species and between Se and Hg in black-footed albatross, suggesting that Se has an antagonistic action on the toxic effects of Cd and Hg. Concentrations of Li, V, Ag, and Cs were usually low (less than 1 microg/g dry weight).     

Changes in the concentrations of trace elements in human milk during lactation

Inductively coupled plasma mass spectrometry (ICP-MS) was used to determine 18 trace elements (Ba, Be, Bi, Cd, Co, Cs, Cu, La, Li, Mn, Mo, Pb, Rb, Sb, Sn, Sr, Tl, and Zn) in 55 human milk samples from 46 healthy mothers collected during lactation periods extending to 293 days after birth. Se was quantified by hydride generation atomic absorption spectrometry (HG-AAS). To test the accuracy and the precision of the analytical procedure, milk powder reference materials (BCR 063 and BCR 150) were analyzed. The results obtained by ICP-MS and HG-AAS showed good agreement with the certified values. Whenever available, trace element concentrations determined in the human milk samples were compared to reliable literature data. The concentrations of Be (< 0.05 to 0.9 microgram/kg), Bi (< 0.09 to 2.0 micrograms/kg), Cs (1.7 to 7.7 micrograms/kg), La (< 0.05 to 3.7 micrograms/kg), Rb (440 to 1,620 micrograms/kg), and Tl (< 0.08 to 0.5 microgram/kg) are the first to be reported for human milk. The concentrations of the essential trace elements Cu (p < 0.005), Mn (p < 0.05), Mo (p < 0.0005), Se (p < 0.001), and Zn (p < 0.0005) significantly decreased and the concentrations of cobalt significantly increased (p < 0.005) in human milk during the course of lactation. All concentrations for the essential trace element tin in the human milk samples were below the method detection limit of 0.3 microgram/kg. Among the not essential and toxic elements-with the exception of Ba, Pb, and Tl-the trend toward lower concentrations with continuing lactation is much less pronounced than for the essential trace elements. With the exception of Se, the daily intakes of essential trace elements of fully breast-fed infants are considerably lower than dietary recommendations.     

The lithium ion: a foundation for psychopharmacological specificity

The preparation of hair for the determination of elements is a critical component of the analysis procedure. Open-beaker, closed-vessel microwave, and flowthrough microwave digestion are methods that have been used for sample preparation and are discussed. A new digestion method for use with inductively coupled plasma-mass spectrometry (ICP-MS) has been developed. The method uses 0.2 g of hair and 3 mL of concentrated nitric acid in an atmospheric pressure-low-temperature microwave digestion (APLTMD) system. This preparation method is useful in handling a large numbers of samples per day and may be adapted to hair sample weights ranging from 0.08 to 0.3 g. After digestion, samples are analyzed by ICP-MS to determine the concentration of Li, Be, B, Na, Mg, Al, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ge, As, Se, Rb, Sr, Zr, Mo, Pd, Ag, Cd, Sn, Sb, I, Cs, Ba, Pt, Au, Hg, Tl, Pb, Bi, Th, and U. Benefits of the APLTMD include reduced contamination and sample handling, and increased precision, reliability, and sample throughput.     

ICP-MS测定铜锌合金中痕量元素

研究了应用电感耦合等离子体质谱法 (ICP MS)测定铜锌合金中Mg ,Al,Ti,Cr ,Mn ,Ni,Cd ,In ,Sn ,Sb ,Tl,Pb ,Bi共13种痕量元素的分析方法。考察铜锌合金中 2 0余种痕量元素的质谱干扰情况及可能的消除方法。通过合适的仪器参数的设置和干扰的校正 ,对个别存在干扰的元素进行了分析 ;研究了非谱干扰对测定痕量元素的影响和内标校正的作用。仅用样品混合酸溶解 ,未进行基体分离或其他样品前处理。实验结果表明 ,对不同质量范围的待测元素以Sc ,La和Re多内标校正信号漂移及     

电感耦合等离子体原子发射光谱法测定

建立了电感耦合等离子体原子发射光谱（ICP AES）法测定锑精矿中4种元素Pb、Se、Te、Tl的定量分析方法。通过试验选择220353 nm、196026 nm、214282 nm、351923 nm分别作为Pb、Se、Te、Tl的分析谱线,无需进行光谱干扰校正。探讨了锑精矿的溶解方法,发现采用王水加氢氟酸溶解样品时,基体效应小,且Se、Te无挥发损失。方法的检出限均小于0010 μg/mL。对锑精矿实际样品进行分析,测定结果与ICP MS法测定值相一致。精密度试验结果表明,RSD（n=9）均小于4%,能满足日常分析对锑精矿中杂质元素的检测要求。     

Analysis of some herbal plants from India used in the control of diabetes mellitus by NAA and AAS techniques

Elemental analysis of some herbal plants used in the control of diabetes has been done by the techniques of Neutron Activation Analysis (NAA) and Atomic Absorption Spectroscopy (AAS). The elements Mn, Na, K, Cl, Al, Cu, Co, Pb, Ni, Cr, Cd, Fe, Ca, Zn and Hg are found to be present in different plants in various proportions.     

Mussels and algae as bioindicators for long-term tendencies of element pollution in marine ecosystems

Results of more than ten years of experience in the determination of metals in mussels and algae collected in the North Sea and the Baltic Sea are presented. The various elements determined here are Hg, As, Se, Cd, Pb, Cu, Na, K, S, P, Zn, Mn, Fe, Sr, Ca, Ba, Mg, Tl, Ni, Co using techniques such as cold vapor AAS, INAA, hydride generation AAS, electrothermal AAS, ICP-AES, IDMS and stripping voltammetry. The results indicate the occurrence of three groups of elements with respect to long-term tendencies of their concentrations. In the first group, the concentrations in both mussels and algae varied in the same manner; in the second group no change was observed in either matrix while in the third group, the concentrations of elements changed in an opposite manner.     

精锑中铜、铅、镉、锌、硒五元素的极谱快速连续测定研究

本文除提出了在１０％ＨＣｌＯ４－２．６％Ｈ３ＰＯ４－０．４％ＨＣＯＯＨ中测定微量铜、铅、镉、锌的新体系外,并巧妙地将作者原测硒体系结合起来,快速简便地完成题示之测定。方法己用于大批生产,效果良好。还对电极过程作了论述。     

Trace element correlations in the blood of Indian women with breast cancer

Fourteen minor (Na, K, P, Fe) and trace (Br, Co, Cr, Cs, Hg, Rb, Sb, Se, Sr, Zn) elements have been determined in pre- and postoperative blood samples of 10 breast-cancer-affected. Indian women and compared with controls. The study showed elevation of Cr, Hg, Fe, Rb, Sb, and Zn and lowering of Se, K, P, and Sr contents in the blood of cancer patients. Most elemental contents in pre- and postoperative stages remain unaltered except Br, Co, and Sb. Statistical significance of Fe, Se, Zn, and Hg levels has been tested by box plots. Lowering of Se in blood (-54.4%) is correlated with its enhancement in cancerous breast tissue (94.7%) of various clinical stages. Se/Zn and Se/Fe ratios are lowered in the blood of cancer patients, whereas Na/K ratio is only marginally enhanced. An attempt has been made to correlate Se levels with the dietary intake and breast cancer risk vis-a-vis American and Japanese women.     

微波消解-电感耦合等离子体质谱法测定煤飞灰中14种金属元素

使用HNO₃-HF混合酸体系微波消解煤飞灰样品,建立了电感耦合等离子体质谱法(ICP-MS)测定煤飞灰中14种痕量元素含量的分析方法。样品微波消解的程序为:0.2 g样品中加入10 mL HNO₃和5 mL HF,5 min加热到110 ℃保持5 min、5 min升温到150 ℃保持5 min、5 min升至190 ℃恒温30 min。实验对较高浓度元素Be、Co、Cr、Cu、Mn、Mo、Ni、Pb、Sn、V和Zn采取稀释10倍、降低总溶解性固体(TDS)含量后以外标法进行测定,Cd、Sb、Tl等低含量元素则采用标准加入法以消除基体干扰;方法检出限为0.001~0.04 mg/kg。将实验方法应用于煤飞灰标准物质SRM 1633c中11种金属元素(Be、Cd、Co、Cr、Cu、Mn、Ni、Pb、Sb、V、Zn)的测定,结果与认定值基本一致,相对标准偏差(RSD,n=6)为0.3%~3.6%,加标回收率在83%~112%之间。采用实验方法测定煤飞灰实际样品的结果与12个实验室采用电感耦合等离子体原子发射光谱法(ICP-AES)、ICP-MS、原子吸收光谱法(AAS)、X射线荧光光谱法(XRF)和滴定法等其他方法测得结果的平均值对比,经t检验统计表明无显著性差异。     

超纯氧化铁制备及其在电感耦合等离子体原子发射光谱法测定高纯铁化合物中杂质元素的应用研究

用电感耦合等离子体原子发射光谱法(ICP-AES)准确测定高纯铁化合物中的痕量杂质元素,需要更高纯度的铁作为基体,以研究它对测定杂质元素的干扰。为此,以分析纯硫酸亚铁为原料制备了高纯氧化铁,制得的高纯氧化铁中杂质元素Al、Cd、Co、Cr、Cu、Mg、Mn、Ni和Zn等的含量低于方法检出限。用制备的高纯氧化铁作为标准系列溶液的基体,得到了基体匹配的标准系列溶液,用此标准系列溶液绘制的校准曲线测定了GBW01402d高纯铁标准物质中杂质元素的含量,其测定值与认定值一致。研究了用无基体匹配标准溶液测定高纯铁及铁化合物中Al、Cd、Co、Cr、Cu、Mg、Mn、Ni和Zn等杂质时的干扰校正方法,结果表明:Al、Co、Cr、Cu、Mg和Zn受到的光谱干扰仅需采用离峰法校正即可,而Cd、Mn和Ni受到的光谱干扰则必需采用多元光谱拟合法校正。用拟定的校正方法测定高纯铁化合物中的痕量杂质元素,准确度高的元素有Al、Cd、Cr和Cu,准确度稍差的元素有Co、Mg、Mn、Ni和Zn。     

Trace element concentrations in higher fungi

The concentrations of ten trace elements, As. Br, Cd, Cu, Hg I, Mn, Se, Zn and V, have been determined in up to 27 species of higher fungi from several sites in Slovenia, Yugoslavia. Analyses were based on destructive neutron activation techniques. Data are presented and compared with the concentrations found in soils. Previously values were non-existent or scanty for these elements, so that the data represent typical levels for basidiomycetes. In addition to confirming high levels of mercury in many species, the survey also found that cadmium is accumulated to a surprising extent by most fungi, the average value being 5 ppm. Among other accumulations found was bromine by the genus Amanita, and selenium by the edible Boletus. Correlation analysis between all pairs of trace elements gave values for r of from 0.75 to 0.43 for 7 pairs (Cu and Hg, 0.75; Se and As, 0.69). As well as these features of biochemical interest, the values found and the pattern of accumulation suggest potential uses of fungi in environmental studies.     

电解分离-电感耦合等离子体发射光谱法测定纯铜中杂质元素

以硫硝混酸为电解液,控制电解电流为2 A,建立了电解分离-电感耦合等离子体发射光谱法测定纯铜中19种杂质元素（Mg、Bi、Al、P、Ti、Cr、Mn、Fe、Zn、Co、Ni、As、Se、Zr、Cd、Sn、Sb、Te 和 Pb）的方法。结果显示,在最佳实验条件下,大于99%的铜沉积至阴极,各杂质元素的回收率大于90%。研究了电解后电解液的酸效应和残余铜对测定的影响,结果表明,基体效应影响较小,可通过基体匹配来进一步消除其影响。各杂质元素的检出限在0.02～4 mg/kg之间。运用该方法测定纯铜标准物质GBW02141,各元素测定值与认定值吻合。以高纯铜空白样品做加标回收试验,除Bi外,各元素的加标回收率在90%～100%之间,相对标准偏差（RSD,n=5）在0.2%～7.2%之间。     

实验室土壤质控样品重金属测试结果允许相对误差判据研究

实验室内部质控体系对于维护检测实验室正常运转具有重要意义。定期核查质控样品分析结果并进行准确度评估,是质控体系正常运行的基本要求。合理选择评估判据是质控规范的重要内容。论文以土壤、沉积物系列标准样品中土壤详查目标重金属元素(As、Be、Cd、Co、Cr、Cu、Hg、Mo、Mn、Ni、Pb、Sb、Tl、V、Zn等)含量认定值及扩展不确定度数据为基础,利用非线性拟合工具,建立了目标元素允许相对误差经验模型,探讨并提出了实验室内部质控样品重金属元素分析结果合格性新判据,并与目前正在执行的地质部门质控规范和生态环境部相关质控技术规定进行了比较。提出的技术途径对于正在修订的地质部门实验室质控规范具有参考价值。     

密闭消解-电感耦合等离子体质谱法测定铅矿石中痕量镓铟铊镉锗

铅矿床具有较高品位的各种稀散元素,因此准确测定铅矿石中Ga、In、Tl、Cd、Ge,对于矿产资源的节约、开发利用等具有重要意义。采用密闭消解方式处理样品,同时在消解过程中加入H₂SO₄(1+4)并水浴加热以沉淀分离Pb基体,分别选择⁶⁹Ga、¹¹⁵In、²⁰⁵Tl、¹¹⁴Cd、⁷²Ge作为分析同位素,¹⁰³Rh为内标校正Ga、In、Cd、Ge,¹⁸⁷Re为内标校正Tl,实现了电感耦合等离子体质谱法对铅矿石中痕量稀散元素Ga、In、Tl、Cd、Ge的测定。实验表明,采用标准(STD)模式测定,Ga、Tl、Cd的背景等效浓度比动能歧视(KED)模式高出一个数量级,而In、Ge的背景等效浓度和KED接近,因此确定采用KED模式测定Ga、Tl、Cd,采用STD模式测定In、Ge;对KED模式下He气流速进行了优化,确定He气流速为5.8mL/min。方法线性方程的相关系数均不小于0.9992,Ga、In、Tl、Cd、Ge的方法检出限分别为0.0520、0.0392、0.0196、0.0212、0.0437μg/g。采用实验方法测定铅矿石实际样品中Ga、In、Tl、Cd、Ge,测得结果的相对标准偏差(RSD,n=6)为1.3%~5.0%,加标回收率为86%~112%。将实验方法应用于铅矿石标准物质中这5个元素的测定,所得结果与认定值吻合。     

Trace elements in formulas based on cow and soy milk and in Austrian cow milk determined by inductively coupled plasma mass spectrometry

With inductively coupled plasma-mass spectrometry (ICP-MS), the 18 trace elements Ba, (Be), (Bi), Cd, Co, Cs, Cu, La, Li, Mn, Mo, Pb, Rb, (Sb), (Sn), Sr, (Tl), and Zn were quantified in the digests of 13 formulas based on cow milk, of two formulas based on soy protein, of two milk powders, from which formulas were prepared, of two samples of Austrian cow milk, and in the water, with which the powders were suspended. Concentrations in parentheses were at or below the method detection limits in the formulas. The accuracy and precision of the analytical procedure tested with milk powder reference materials BCR 063 and BCR 150 were satisfactory. The concentrations of trace elements in the powders vary considerably from batch to batch. The ratios of high to low concentrations ranged from 1.1 to 4.8 and were higher for the essential trace elements Co, Cu, Mn, Mo, Sn, and Zn than for nonessential or toxic elements. The contribution of tap water from the water system of the city of Graz, Austria to the concentrations of trace elements in the formulas ranges from 45% for Pb to 0.2% for Rb and is negligible, for instance, for Cd, Cs, La, Mo, and Sn. Preformulas and follow-up formulas are partly supplemented with the essential trace elements Cu, Mn, and Zn and, therefore, concentrations of these trace elements in the formulas vary considerably. However, supplementation of a formula with a particular element must not necessarily result in higher concentrations compared to non-supplemented formulas. Concentrations of the essential elements were in the following ranges for preformulas, follow-up formulas, soy-based formulas (in microg/kg): Co, 8.3-11.2, 4.5-13, 5.0-5.7; Cu, 330-750, 27-730, 440-530; Mn, 33-580, 40-390, 440-530; Mo, 10-32, 9-39, 44-46; Sn, <0.44-3.8, <0.44-1.0, <0.44-5.8; Zn, 3340-11,380, 4120-7100, 5590-6,840. A preformula supplemented with Mn had a 10 times higher manganese concentration than preformulas without supplementation. Concentrations of all trace elements quantified were lower in cow milk than in formulas and do not meet the dietary requirements of infants.     

电感耦合等离子体质谱干扰对钢铁及合金痕量分析的影响

在采用电感耦合等离子体质谱对钢铁及合金进行痕量分析的过程中,由于该类样品的成分复杂,经酸消解后未进行基体分离而直接雾化进样,存在严重的质谱干扰和非谱干扰。本文通过对钢铁及合金的基体元素铁和镍,以及主要的合金元素如铬、钴、锰、锆、铌、钼和钨等,分别与溶剂、等离子气、空气等中主要元素所形成的质谱干扰进行全面系统的研究,对存在的干扰提供了定量化的数据,并提出了相应的校正方案和措施。应用所建立质谱较正方案对铁镍基合金GH167标准物质中Ga,Ag,Cd,In,Sn,Sb,Te,Tl,Pb和Bi等痕量元素进行了分析     

High-Purity Nickel Prepared by Electron Beam Melting: Purification Mechanism

A bulk cylindrical high-purity nickel ingot, with purity of more than 99.999 pct (5N) in mass, was obtained from the raw nickel with 99.95 pct (3N5) initial purity by virtue of double electron beam melting (EBM). A chemical analysis was performed by using glow discharge mass spectrometry (GDMS) analysis for all elements in the periodic table except carbon, nitrogen, and oxygen, which were tested by the high-performance combustion and fusion method. The major impurities B, Na, Al, Si, P, S, Ca, Ti, Cr, Fe, Cu, Co, Zn, As, Ag, Sb, and Pb showed an excellent removal effect with removal efficiency of more than 85 pct following the double EBMs. Li, Mg, Cl, K, V, Mn, Ga, Ge, Cd, Se, In, Sn, Tl, Au, and Pt were below the detection limit. No significant change in concentration was found for the refractory elements W, Mo, Ta, Nb, and Ir. Be, F, Sc, Se, Br, Rb, Sr, Zr, Y, Ru, Rh, Pd, Te, I, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Re, Os, Hg, Bi, Th, and U were not detectable following the purification as compared to the raw nickel. Gaseous impurities, C, N, O, especially for N, was removed sufficiently. Theoretical calculations for removal efficiency of impurity Fe based on the calculated vapor pressure, activity coefficient, and melt temperature were in good agreement with measured results, and the purification mechanism was ascribed to the evaporation of major impurities and subsequently evacuation by repetitive EBM.     

麦饭石中微量元素的加罩电极光谱分析

采用加罩电极发射光谱法测定了来自不同地区麦饭石样品和地质标样中36种痕量元素,对测定的最佳条件进行了系统研究。通过选择合适的曝光条件、内标元素和分析线对,连续测定了易挥发、中等挥发和难挥发元素。标样的测定值与认定值一致,标准偏差小于21%。对不同地区的样品测定结果表明:麦饭石中对人体有益的痕量元素含量高,而对人体有害的元素如砷、镉、铬、汞和铅等含量低。     

贵州丹寨县铅锌矿区小流域土壤重金属污染特征及生态风险评价

为探究贵州丹寨县铅锌矿区矿业活动对土壤系统运转对环境影响,以丹寨县兴仁镇铅锌矿区土壤为研究对象,采集小流域内河流周边不同土地利用类型土壤表层(0~20cm)的样品,分析测定土壤中Cu、Cd、Pb、Zn、Mn、Hg、As 7种重金属含量。应用单因子污染指数法、内梅罗综合污染指数法、地质累积指数法、潜在生态指数法对矿区不同土壤层重金属进行污染程度和潜在生态风险进行评价。结果表明,0~10cm土壤中Cu、Cd、Pb、Zn、Mn、Hg、As含量分别是贵州省土壤背景值的0.65、5.13、1.74、2.45、0.59、5.08、0.27倍。10~20cm土壤中Cu、Cd、Pb、Zn、Mn、Hg、As含量分别是贵州省土壤背景值的0.71、3.11、1.18、2.21、0.65、4.88、0.21倍。不同小流域与不同深度土层危害程度有所差异,通过评价结果得出研究区主要污染重金属元素为Cd、Hg,土壤重金属处于中等及以上潜在生态危害程度。