共查询到20条相似文献,搜索用时 15 毫秒
1.
T. P. Fischer S. Shuttleworth P. A. O’Day 《Analytical and bioanalytical chemistry》1998,362(5):457-464
The accurate measurement of ultra-trace concentrations of rare metals and platinum group elements in volcanic fluids is complicated by interferences, complex matrices, and preferential element partitioning. We analyzed condensed, high-temperature magmatic fluids collected from Kudryavy volcano (Kurile Islands, Russia) for Be, B, Rb, Sr, Mo, Ru, Rh, Pd, Cd, W, Re, Pt, Pb, Bi, and U using ICP-MS. The samples had three different matrices: 5 mol L–1 sodium hydroxide (NaOH, pH = 11), gas condensates of sulfuric acid (H2SO4, pH = 0), and solid elemental sulfur. Interferences and suppression/enhancement effects were investigated using standards in concentrated NaOH and H2SO4 solutions to determine adequate dilution for sample analyses, which then required very low levels of element detection (< 1 μg L–1 for most elements). Depending on the field sampling technique of volcanic gas vents, our results show significant differences in concentrations of some trace elements due to the precipitation of solid sulfur during gas condensation and variations in element volatility as a function of temperature. 相似文献
2.
Z. Arslan N. Ertas J. F. Tyson P. C. Uden E. R. Denoyer 《Analytical and bioanalytical chemistry》2000,366(3):273-282
A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and Tl, it was possible to obtain accurate results despite the 35–¶40% suppression in the signals. Isobaric overlap was only a problem in the cases of 42Ca and 78Se; 44Ca and 77Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased. 相似文献
3.
Determination of trace elements in marine plankton by inductively coupled plasma mass spectrometry (ICP-MS) 总被引:3,自引:0,他引:3
Arslan Z Ertas N Tyson JF Uden PC Denoyer ER 《Fresenius' Journal of Analytical Chemistry》2000,366(3):273-282
A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and T1, it was possible to obtain accurate results despite the 35-40% suppression in the signals. Isobaric overlap was only a problem in the cases of 42Ca and 78Se; 44Ca and 77Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased. 相似文献
4.
Jörgen Riondato F. Vanhaecke L. Moens Richard Dams 《Analytical and bioanalytical chemistry》2001,370(5):544-552
In the framework of an international certification campaign, sector-field inductively coupled plasma mass spectrometry (sector-field ICP–MS) was used for the accurate determination of the rare earth elements in five candidate reference materials: aquatic plant, calcareous soil, mussel tissue, river sediment, and tuna muscle. All samples were taken into solution by use of microwave-assisted or mixed microwave-assisted / open beaker acid digestion. Subsequently, the samples were appropriately diluted and subjected to ICP–MS analysis. Except for Sc, all the elements involved were determined at low mass resolution (R = 300). For Sc, application of a higher resolution setting (R = 3000) was required to separate the analyte signal from those of several molecular ions which gave rise to spectral overlap at low mass resolution. Some of the heavier REE can also suffer from spectral overlap attributed to the occurrence of oxide ions (MO+) of the lighter REE and Ba. This spectral overlap could be successfully overcome by mathematical correction. Matrix effects were overcome by use of two carefully selected internal standards, such that external calibration could be used. On each occasion, a geological reference material was analyzed as a quality-control sample and the reliability of all results obtained was additionally checked by means of chondrite normalization. For tuna muscle the content of all REE was below the limit of detection. For calcareous soil and river sediment, low to sub μg g–1 values were observed, whereas the REE content of aquatic plant and mussel tissue was considerably lower (low to sub ng g–1). Overall, the results obtained were in excellent agreement with the average values, calculated on the basis of all “accepted” values, obtained in different laboratories using different techniques. 相似文献
5.
建立了微波消解-内标法-标准加入-ICP-MS法测定高纯黄金中铝、砷、铋、铬、铁、铅、锑、硒、碲、铱等痕量元素的分析方法.从试样溶解方式、内标元素及同位素的选择、仪器检测模式的优化及降低基体抑制效应等方面进行优化.实验加标回收率为99.5% ~110%,相对标准偏差(RSD)为0.050% ~6.5%.实验的准确度和精... 相似文献
6.
Riondato J Vanhaecke F Moens L Dams R 《Fresenius' Journal of Analytical Chemistry》2001,370(5):544-552
In the framework of an international certification campaign, sector-field inductively coupled plasma mass spectrometry (sector-field ICP-MS) was used for the accurate determination of the rare earth elements in five candidate reference materials: aquatic plant, calcareous soil, mussel tissue, river sediment, and tuna muscle. All samples were taken into solution by use of microwave-assisted or mixed microwave-assisted / open beaker acid digestion. Subsequently, the samples were appropriately diluted and subjected to ICP-MS analysis. Except for Sc, all the elements involved were determined at low mass resolution (R = 300). For Sc, application of a higher resolution setting (R = 3,000) was required to separate the analyte signal from those of several molecular ions which gave rise to spectral overlap at low mass resolution. Some of the heavier REE can also suffer from spectral overlap attributed to the occurrence of oxide ions (MO+) of the lighter REE and Ba. This spectral overlap could be successfully overcome by mathematical correction. Matrix effects were overcome by use of two carefully selected internal standards, such that external calibration could be used. On each occasion, a geological reference material was analyzed as a quality-control sample and the reliability of all results obtained was additionally checked by means of chondrite normalization. For tuna muscle the content of all REE was below the limit of detection. For calcareous soil and river sediment, low to sub microg g(-1) values were observed, whereas the REE content of aquatic plant and mussel tissue was considerably lower (low to sub ng g(-1)). Overall, the results obtained were in excellent agreement with the average values, calculated on the basis of all "accepted" values, obtained in different laboratories using different techniques. 相似文献
7.
S. Tonouchi H. Habuki K. Katoh K. Yamazaki T. Hashimoto 《Journal of Radioanalytical and Nuclear Chemistry》2002,252(2):367-371
Inductively coupled plasma mass spectrometry (ICP-MS) has been applied to the measurement of plutonium isotopes in soils. In the ICP-MS, a calibration curve method was conveniently utilized even in high viscosity solution using a Babington nebulizer. Plutonium concentrations in soil around the Kashiwazaki-Kariwa nuclear power station were found to be in the range of 0.054 to 1.0 Bq/kg with an average of 0.27 Bq/kg. The ratios of 239Pu/240Pu were also obtained with the ICP-MS to investigate the origin of Pu-isotopes. On the basis of this result, the origin of the Pu-isotopes was attributed to be fallout from the past atmospheric nuclear tests. 相似文献
8.
Determination of trace elements in granites by inductively coupled plasma mass spectrometry 总被引:66,自引:0,他引:66
Proposed is a simple and reliable method for the dissolution of granite and the determination of 38 elements by inductively coupled plasma mass spectrometry. One hundred milligrams of sample are digested with 1 ml of HF and 0.5 ml of HNO(3) in screw top PTFE-lined stainless steel bombs at 190 degrees C for 12 h. Insoluble residues are dissolved using 8 ml of 40% HNO(3) (v/v) heated to 110 degrees C for 3 h. Six granite standard reference materials (GSR-1, JG-2, G-2, NIM-G, SG-3, SG-1a) were studied. Analytical calibration was accomplished using aqueous standard solutions. Rhodium was used as an internal standard to correct for matrix effects and instrument drift. We report data for: Li, Be, Sc, V, Cr, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Cs, Ba, Hf, Ta, W, Pb, Th, U and 14 of the rare earth elements. The recoveries for most of these elements in granite ranged from 90 to 110%. 相似文献
9.
为快速、准确测定韭菜中多元素含量,采用微波消解法对韭菜中样品进行消解处理,优化了前处理方法、ICP-MS工作条件和检测方法,利用微波消解-电感耦合等离子体质谱法测定韭菜中Pb、Cd、Se、As、Zn、Cu、Ni、Fe、Cr、Ca、K等11种元素含量。结果表明,在硝酸-双氧水(7:1)体系中,消解功率1550W,温度梯度为120℃-160℃-195℃,总时长为45min,赶酸温度选择150℃,可将韭菜完全消解,并且ICP-MS射频功率设为1550W,运用在线内标的检测方式降低非质谱干扰。11种元素回归系数R2均大于0.999,方法检出限为0.002~0.100μg/kg,方法定量限为0.006~0.300μg/kg。方法回收率88.0%~102.7%,相对标准偏差为1.8%~4.6%,可以满足韭菜中多种元素同时测定的需求。方法具有灵敏度高、线性范围宽、准确性高等特点,可为韭菜样品的多元素同时测定提供可靠的方法支撑。 相似文献
10.
Determination of trace elements in residual oil by high-resolution inductively coupled plasma mass spectrometry 总被引:2,自引:0,他引:2
Hualin Xie Kelong Huang Jinchun Liu Xidu Nie Liang Fu 《Analytical and bioanalytical chemistry》2009,393(8):2075-2080
An analytical method using high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous
determination of 20 elements, including Na, Mg, Al, Ca, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Mo, Cd, Sn, Sb, Ba, and Pb
elements, in residual oil was described. The sample was dissolved in HNO3 by microwave digestion, and then the above 20 elements in the solution were analyzed directly by HR-ICP-MS. Most of the spectral
interferences could be avoided by measuring in the high-resolution mode. The matrix effect caused by the sample-digesting
solution and corrected by Sc, Rh, and Bi as the internal standard elements was studied in detail. The optimum condition of
the determination was also tested and discussed. The result showed that the detection limits of the method were in the range
of 0.014 to 11.6 μg L−1; the relative standard deviation was less than 3.8% and recoveries in the samples were in the range of 88.4% to 108.0%. This
method can be used to determine the trace elements in residual oil with the features of accurate, rapid, and convenient determination. 相似文献
11.
D. E. Vance V. F. Belt T. J. Oatts D. K. Mann 《Journal of Radioanalytical and Nuclear Chemistry》1998,234(1-2):143-147
The determination of neptunium-237 (237Np) traditionally has been performed by alpha spectrometry or neutron activation analysis. These methods are labor intensive
and require several days for completion. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a possible alternative for237Np determinations. This paper describes the analytical method developed for samples that have significant levels of uranium
present. The lower reporting limits achievable by ICP-MS are competitive with the counting methods, but the real advantage
for this laboratory lies in the lower cost and faster turnaround time provided by ICP-MS. 相似文献
12.
采用微波消解前处理方法,结合电感耦合等离子体质谱技术,建立了板栗中钠(Na)、钾(K)、镁(Mg)、锰(Mn)、铁(Fe)、钒(V)、钴(Co)等19种矿物元素及镧(La)、铈(Ce)、镨(Pr)、钕(Nd)、钐(Sm)、铕(Eu)、钆(Gd)、铽(Tb)、镝(Dy)、钬(Ho)、铒(Er)、铥(Tm)、镱(Yb)、镥(Lu)、钇(Y)等15种稀土元素的同时分析测定方法。该方法检出限为0.0027~0.78μg?L-1,相对标准偏差为1.4%~6.3%。通过国家标准物质GBW10019苹果的准确率实验验证,测定结果均在标准证书值范围内。实验结果表明,该方法适用于板栗中矿物元素及稀土元素的同时测定。 相似文献
13.
电感耦合等离子体质谱法测定血液和精液中的硼 总被引:3,自引:0,他引:3
采用HNO3-H2O2和氨水-甘露醇两种方法处理样品,电感耦合等离子体质谱法(ICP-MS)测定血液和精液中的硼。Be作内标补偿基体效应,并用标准加入法验证了方法的可靠性,标准加入法与外标法测定结果相吻合。在测定B的同时,还可进行Cr、Cu、Cd、Ba、Sr、Mn、Co、Tl、Li、Pb、Zn、Sc、Ti、V、As等多元素测定。两种样品处理方法的测定值呈显著正相关(r=0.99919)。方法检出限为0.11ng/mL(氨水-甘露醇法),0.06ng/mL(HNO3-H2O2)。已用于测定某硼矿区血液和精液样品中的硼。 相似文献
14.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for the sensitive multi-element analysis
of traces and ultra-traces in geological samples. In order to prepare homogeneous targets the powdered geological samples
were melted together with a lithium-borate mixture (90% Li2B4O7, 10% LiBO2) in a muffle furnace at 1050 °C. The quantification of the analysis results was carried out using the BCR-2G and BM standard
reference material (SRM). The experimentally determined relative sensitivity coefficients (RSC) for both SRMs vary between
0.2 and 3 for most of the elements, whereas the relative standard deviation (RSD) of the determination (N = 3) of the concentration
was 5–20%. The analysis results of LA-ICP-MS for various geological samples are in agreement with those of other methods.
Received 31 March 1999 / Revised: 26 May 1999 / Accepted: 31 May 1999 相似文献
15.
Determination of trace elements in steel by laser ablation inductively coupled plasma mass spectrometry. 总被引:3,自引:0,他引:3
A rapid quantitative analysis of the trace elements in steel by laser ablation inductively coupled plasma mass spectrometry is described. The conditions for laser ablation and normalization methods to improve the analytical precision are given. The optimum conditions for laser ablation were achieved when the ion yield was a maximum at the focus position in the fixed Q pulse mode, and above the focus position in the Q-switched pulse mode. It was found that the fixed Q pulse mode was most suitable for the determination of trace metal elements in steel, and that the Q-switched pulse mode was most suitable for both non-metallic elements and elements with a high boiling-point. In order to improve the analytical precision for those elements with a strong background intensity, normalization methods with both the matrix ion, 57Fe+, and 38Ar+ are proposed. 相似文献
16.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for the sensitive multi-element analysis of traces and ultra-traces in geological samples. In order to prepare homogeneous targets the powdered geological samples were melted together with a lithium-borate mixture (90% Li2B4O7, 10% LiBO2) in a muffle furnace at 1050?°C. The quantification of the analysis results was carried out using the BCR-2G and BM standard reference material (SRM). The experimentally determined relative sensitivity coefficients (RSC) for both SRMs vary between 0.2 and 3 for most of the elements, whereas the relative standard deviation (RSD) of the determination (N = 3) of the concentration was 5–20%. The analysis results of LA-ICP-MS for various geological samples are in agreement with those of other methods. 相似文献
17.
Determination of cosmochemically volatile trace elements in chondritic meteorites by inductively coupled plasma mass spectrometry 总被引:1,自引:0,他引:1
We have developed a method for the quantification of 14 cosmochemically moderately volatile to highly volatile trace elements (Cu, Zn, Ga, Se, Rb, Ag, Cd, In, Sn, Sb, Te, Cs, Tl, and Bi) in chondritic meteorites by ICPMS. The method utilizes internal standardization via addition of Be, Rh, Re, and U and multiple single point matrix-matched external calibrations with Allende standard reference meteorite to provide drift corrected calibration within an ICPMS procedure. We have demonstrated our method's precision and accuracy by performing replicate dissolutions and analyses of 0.05-0.10 g samples of a homogenized sample of the CM2 Murchison meteorite and compared our results to literature values for this meteorite. Our procedure allows for a rapid and accurate determination of the cosmochemically important VTEs in chondritic meteorites providing the means for an even more comprehensive elemental analysis of a single sample of chondritic material. 相似文献
18.
建立一种碱熔样-ICP-MS直接分析稀土荧光粉中微量杂质元素(非稀土杂质和稀土杂质元素)的新方法。此方法测定限达到:非稀土元素0.007-1.036μg/g,稀土元素0.001-0.057μg/g,精密度<10%。方法预处理简单、检出限低、重现性好,为高纯稀土荧光粉成品的质量控制提供了可靠地分析手段。 相似文献
19.
为准确定量拟黑多刺蚁体内的微量元素,采用微波消解法,以HNO_(3)-H_(2)O_(2)混合酸为消解体系对样品进行前处理,选择合适的同位素,以^(103)Rh为内标测定^(52)Cr、^(55)Mn、^(60)Ni、^(63)Cu、^(66)Zn、^(75)As、^(78)Se、^(88)Sr和^(114)Cd,以^(185)Re为内标测定^(202)Hg和^(208)Pb,建立了电感耦合等离子体质谱法测定拟黑多刺蚁中11种微量元素的方法。实验发现,以HNO_(3)-H_(2)O_(2)为消解体系,样品消解完全;采用KED模式消除质谱干扰,以内标法校正基体效应;通过绘制校准曲线及测定流程空白,各元素校准曲线的相关系数均大于0.999,方法检出限为0.0005~0.011 mg/kg,方法定量限为0.0016~0.033 mg/kg。对拟黑多刺蚁实际样品进行测定,各元素的相对标准偏差(RSD,n=9)在1.2%~5.5%,加标回收率为91.2%~107%;经过实验室间比对实验,相对偏差为-3.15%~2.74%;测定六个不同产地的拟黑多刺蚁样品,结果显示不同产地样品除Cd外,其他10种微量元素的含量均存在较大差异。测定结果稳定可靠,能满足拟黑多刺蚁中11种微量金属元素含量的分析检测要求。 相似文献
20.
Hans Vanhoe Carlo Vandecasteele Jacques Versieck Richard Dams 《Mikrochimica acta》1989,99(3-6):373-379
A method was developed for the determination of Fe, Co, Cu, Zn, Rb, Mo and Cs in human serum by ICP-MS. Sample preparation was kept as limited as possible: Serum samples were diluted with nitric acid and indium was added as internal standard. The results for Fe, Co, Cu, and Zn were corrected for interferences from polyatomic ions using a suitable blank solution. No interferences occur for the considered isotopes of Rb, Mo, and Cs. A second-generation human serum reference material was analyzed, in order to test the accuracy and precision of the analytical procedure. The results obtained are in good agreement with the certified values.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, AustriaResearch Director of the National Fund for Scientific Research (Belgium) 相似文献