萃取分离-ICP-MS测定高纯铝中痕量元素

利用吡咯烷二硫代氨基甲酸铵(APDC)-CHCl_3萃取分离体系结合ICP-MS对高纯铝中的Co、As、Mo、In、Sn、Sb、Cd、Ag、Pd、Au进行测定,建立了测定高纯铝中痕量元素的方法.实验分别考察了仪器工作参数,萃取酸度,络合剂用量对于杂质元素测定结果的影响,选择了最佳实验条件.各元素的回收率在77.6%～112.2%之间,检出限0.02～0.6 ng/mL,RSD为1.6%～7.2%.     

电感耦合等离子体质谱法测定高纯氧化钽中28种痕量杂质元素

建立了用电感耦合等离子体质谱仪(ICP-MS)测定高纯氧化钽中28种痕量杂质元素的方法。讨论了质谱干扰及接口效应,采用标准加入法消除基体效应。各元素的方法检出限为0.001~0.1μg/g,回收率为90%~115%,方法适用于纯度为99.999%的高纯氧化钽中痕量杂质元素的测定。     

Isotope measurements in uranium using a quadrupole inductively coupled plasma mass spectrometer (ICPMS)

A series of measurements were carried out to establish the reliability associated with isotope ratio (235/238) measurements on uranium samples using a quadrupole inductively coupled plasma mass spectrometer (ICPMS). Figures of merit related to the isotopic measurements were determined using non certified as well as certified materials provided by the New Brunswick Laboratory (NBL). The experimental results showed that repeatability is around 0.5% while reproducibility was calculated as 0.27%. Mass discrimination was determined as 0.03% per mass unit and the system linearity check over five orders of isotope ratios yielded a mass discrimination factor (K factor) of 1.0002±0.0081 (0.81%, 2s). The mean error of measurement obtained from six different certified reference materials was 0.77%.     

Determination of impurities in strontium titanate ceramics by inductively coupled plasma mass spectrometry

The determination of impurities in SrTiO₃ by ICPMS was investigated. The sample was decomposed with hydrochloric and hydrofluoric acids in a PTFE pressure vessel. The internal standard method using Au was selected to eliminate an ion count suppression by the Sr and Ti matrix. Impurities at sub g/ml level in SrTiO₃ were determined. The detection limits were in the range of 0.008 to 0.01 g/g.     

电感耦合等离子体质谱法测定烟酰胺药物元素杂质

建立了烟酰胺药物中30种元素杂质的ICP-MS分析方法,并根据USP< 233>进行了验证,在优化的实验条件下,本方法的检出限在4.0×10-4～0.4μg/L之间,加标回收率在86.3％～116.0％之间,与ICP-OES检测结果基本一致.用所建立方法对烟酰胺以及稳定性样品进行了元素杂质检测,根据样品制备工艺初步判断元素杂质的来源.     

电感耦合等离子体质谱法测定烟酰胺药物元素杂质

建立了烟酰胺药物中30种元素杂质的ICP-MS分析方法,并根据USP< 233>进行了验证,在优化的实验条件下,本方法的检出限在4.0×10-4～0.4μg/L之间,加标回收率在86.3％～116.0％之间,与ICP-OES检测结果基本一致.用所建立方法对烟酰胺以及稳定性样品进行了元素杂质检测,根据样品制备工艺初步判断元素杂质的来源.     

Determination of plutonium by inductively coupled plasma mass spectrometry (ICP-MS)

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.     

Determination of trace impurities in high-purity cadmium by high-resolution inductively coupled plasma mass spectrometry.

Trace impurities in high-purity cadmium were determined by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). To overcome some potentially problematic spectral interference, measurements were acquired in both medium and high-resolution modes. The matrix effects due to the presence of excess HCl and cadmium were evaluated. The optimum conditions for the determination were tested in this experiment and discussed. The detection limits ranged from 0.01 to 0.27 microg g-1, depending on the elements. The results for the determination of 22 trace elements in high-purity cadmium are presented.     

A rapid method for uranium isotope ratio measurement by inductively coupled plasma mass spectrometry

Uranium isotope ratio U 234/238 can be measured by commercial high-performance inductively coupled plasma mass spectrometry (ICP-MS) with good precision and accuracy (relative standard deviation RSD<2%). The method is based on acquiring the data using a peak jump mode and a collecting signal 10 times longer for low abundance isotopes. Uranium isotope standards U-005 to U-200 from the National Bureau of Standards (NBS) were used for method development. The optimum uranium concentration range for analysis for dissolved samples is from 50 to 200 g l^–1.     

膜去溶-ICP-MS法测定高纯Eu_2O_3中14种痕量稀土杂质

研究了不需基体分离,膜去溶-ICP-MS法直接测定高纯Eu2O3中的14种痕量稀土杂质的分析方法。讨论了Eu基体产生的多原子离子对被测元素的质谱干扰。使用膜去溶后,待测元素灵敏度提高3倍左右,EuO/Eu产率从去溶前的0.016%降低为0.0007%。建立了Tm的数学校正方程,通过膜去溶结合数学校正可将Eu基体对Tm干扰完全消除。14种稀土杂质的检出限和(∑RE)为70 ng/L,测定下限和(∑RE)为0.54μg/g。对6N高纯Eu2O3样品进行了分析,样品回收率为96%~109%,RSD小于10%。所建立的方法对Eu2O3标准样品的测定结果与国家标准方法测定结果相一致。     

电感耦合等离子体-质谱法测定高纯硫粉末中17种痕量杂质

建立电感耦合等离子体-质谱(ICP-MS)法测定高纯硫粉中Si、P、V、Cr、Mn、Ni、Co、Cu、As、Zn、Zr、Cd、In、Sb、Te、Pb、Bi等17种痕量金属杂质含量的方法。样品用HClO4溶解后挥发硫基体,使样品中杂质元素得到富集,各杂质元素的方法检出限为0.1～50ng/g。方法加标回收率为83%～117%。各杂质元素均为10ng/mL的混合标准溶液平行7次测定的相对标准偏差均小于5%。该方法能够满足纯度为99.999%～99.9999%的高纯硫样品中杂质测定的需要。     

Determination of uranium in marine sediment pore waters by isotope dilution inductively coupled plasma mass spectrometry

Inductively coupled plasma mass spectrometry (ICP-MS) was used in an isotope dilution mode to assay small-volume (0.25 ml) sediment pore waters for their uranium contents, using ²³⁶U as the spike. The only pretreatment required was a simple dilution by a factor of 20, which gave sufficient volume for three replicate analyses per sample. Rapid and accurate results were obtained for a variety of samples and standards, ranging in concentration from 0.05 to 10 ng U ml^?1. A suite of 30 samples can be analysed in less than 6 h by this method. The relative standard deviation was better than 1.9%, with a detection limit, based on 3σ background, of 2 pg U ml^?1 in solution (40 pg ml^?1 in samples). Sea water is a difficult matrix for ICP-MS and thus the method is generally suitable for uranium determinations in many other sample solutions.     

Determination of long-lived radionuclides in concrete matrix by laser ablation inductively coupled plasma mass spectrometry

A laser ablation system using a Nd:YAG laser was coupled both to a quadrupole inductively coupled plasma (ICP) mass spectrometer and to a double-focusing sector field ICP mass spectrometer. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for the determination of long-lived radionuclides in a concrete matrix. The investigated samples were two laboratory standards with a concrete matrix, which we doped with different long-lived radionuclides (e.g. ⁹⁹Tc, ²³²Th, ²³³U, ²³⁷Np) from the ng g⁻¹ to μ g⁻¹ concentration range and an undoped concrete material (blank). Detection limits for long-lived radionuclides in the 10 ng g⁻¹ range are reached for LA-ICP-MS using the quadrupole mass spectrometer. With double-focusing sector field ICP-MS, the limits of detection are in general one order of magnitude lower and reach the sub ng g⁻¹ range for ²³³U and ²³⁷Np. A comparison of mass spectrometric results with those of neutron activation analysis on undoped concrete sample indicates that a semiquantitative determination of the concentrations of the minor and trace elements in the concrete matrix is possible with LA-ICP-MS without using a standard reference material.     

Determination of thorium and uranium in activated concrete by inductively coupled plasma mass spectrometry after anion-exchange separation

A sensitive analytical method was established for the determination of Th and U in activated concrete samples. The method combines an anion-exchange separation step with an ICP-MS determination technique. In the ICP-MS measurement, a few μg mL^–1 of Al and Ca, a few ng mL^–1 of Mn, La, Ce, Nd and Pb and pg mL^–1 amounts of Li, Zr, Nb and Ba coexisting in the anion-exchange fraction of Th and U did not interfere. No adverse interference effects were observed in real sample analyses. The obtained detection limits (3σ, n = 10) of Th and U were 2.3 and 1.8 pg mL^–1, respectively. The analytical precisions for ca. 5 μg g^–1 Th and ca. 1 μg g^–1 U in real activated concrete samples were equally less than 7% RSD. The accuracies obtained by the analysis of GSJ rock standard samples were –18.1 to 0.4% for the Th determination and –14.0 to –5.7% for the U determination. The method uses the conventional absolute calibration curve. The internal standard calibration is unnecessary.     

Determination of uranium in organic solutions by inductively coupled plasma atomic emission spectrometry

The determination of uranium in organic solutions by inductively coupled plasma atomic emission spectrometry is reported. The conditions for achieving plasma stability were determined as well as the optimum conditions (RF power, observation height and argon flow) of a spectrometer for analysis of U(II) 367.007 nm in three organic solvents, xylene, kerosine and benzene. The effects of RF power and observation height on signal-to-back-ground ratio and the detection limits are considered. Spectral interferences due to CN band are discussed.A part of this work was presented at the Second Karlsruhe International Conference on Analytical Chemistry in Nuclear Technology Karlsruhe, FRG, June 5–9, 1989.     

Neptunium determination by inductively coupled plasma mass spectrometry (ICP-MS)

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.     

Determination of thorium and uranium in activated concrete by inductively coupled plasma mass spectrometry after anion-exchange separation

A sensitive analytical method was established for the determination of Th and U in activated concrete samples. The method combines an anion-exchange separation step with an ICP-MS determination technique. In the ICP-MS measurement, a few μg mL^–1 of Al and Ca, a few ng mL^–1 of Mn, La, Ce, Nd and Pb and pg mL^–1 amounts of Li, Zr, Nb and Ba coexisting in the anion-exchange fraction of Th and U did not interfere. No adverse interference effects were observed in real sample analyses. The obtained detection limits (3σ, n = 10) of Th and U were 2.3 and 1.8 pg mL^–1, respectively. The analytical precisions for ca. 5 μg g^–1 Th and ca. 1 μg g^–1 U in real activated concrete samples were equally less than 7% RSD. The accuracies obtained by the analysis of GSJ rock standard samples were –18.1 to 0.4% for the Th determination and –14.0 to –5.7% for the U determination. The method uses the conventional absolute calibration curve. The internal standard calibration is unnecessary. Received: 14 March 1999 / Revised: 13 July 1999 / Accepted: 15 July 1999     

Determination of vanadium by reaction cell inductively coupled plasma mass spectrometry

Recent advances in inductively coupled plasma mass spectrometry (ICP-MS) have included the addition of interference reduction technologies, such as collision and reaction cells, to improve its detection capability for certain elements that suffer from polyatomic interferences. The principle behind reaction cell (RC)-ICP-MS is to remove a particular polyatomic interference by dissociation or formation of a different polyatomic species that no longer interferes with the analyte of interest. However, some interferences cannot be removed by commonly reported reaction gases, such as hydrogen, oxygen, or methane, necessitating using more reactive and hazardous gases, such as ammonia. The current study investigates oxygen as a reaction gas in RC-ICP-MS to specifically react with vanadium analyte ions, rather than the interferents, to produce a polyatomic analyte species and thereby provide a way to analyze for vanadium in complex environmental matrices. The technique has been tested on a series of river water, tap water, and synthetic laboratory samples, and shown to be successful in vanadium analyses in high chloride and sulfate matrices. The zinc isobaric interference on the new vanadium oxide analyte at m/z 67 is also investigated, and can be corrected by using a standard mathematical correction equation. The results of this study further increase the utility of RC-ICP-MS analytical techniques for complex environmental matrices.