Determination of ultra-trace concentrations of elements in high purity tellurium by inductively coupled plasma mass spectrometry after Fe(OH)(3) coprecipitation

In this work, a method was established for the determination of impurities in high purity tellurium by inductively coupled plasma mass spectrometry (ICP-MS) after Fe(OH)(3) coprecipitation. After comparison of coprecipitation ability and separation efficiency between Fe(OH), and Al(OH)(3), Fe(OH)(3) was chosen as the precipitate. A separation factor of 160 for 200 mg tellurium was obtained under conditions of pH 9 and 2 mg of Fe3(+). The 13 elements, such as Bi, Sn, Pb, In, Tl, Cd, Cu, Co, Ni, Zn, Ti, Be and Zr, could be almost completely coprecipitated under these conditions. In addition, Te memory effect imposed on the ICP-MS instrument was assessed, as well as Te matrix effect that caused the low recovery of Ga, As, Sb and V in real sample was discussed. Finally, the method was evaluated through recovery test and was applied to practical sample analysis, with detection limits of most of the elements being below 0.15 mug g(-1) and R.S.D. below or at approximately 10%, which indicated that this method could fully satisfy the requirements for analysis of 99.999% similar to 99.9999% high purity Te.

Determination of ultra-trace rare-earth elements in human plasma by inductively coupled plasma mass spectrometry

Inductively coupled plasma mass spectrometry (ICP-MS),a highly sensitive inorgnic analytic technique,fits to determine ultra-nace rare-earth elements in human plasma. Under the optimized conditions detection limits for 15 rare-earth elements are in the range of 0.7 (for Eu)-5.4 (for Gd) ng.L-1. Indium as an internal standard element is used to compensate for matrix suppression effect and sensitivity drift. Three kinds of preparation methods, diluted with 1% HNO3, digested with HNO3-H2O2 and with HNO3-HClO4, are checked and compared,and the former is the simplest way to be measured. The samples diluted with 1% HNO3, stored in 4 degrees C, are very steady for 16 days. With the method, 11 healthy plasma samples in Changchun area of China are analysed.

Trace analysis of Zn-doped compound semiconductor material by resonant ionization mass spectrometry

An experimental setup and the procedure for the laser resonant ionization mass spectrometry (RIMS) have been described. Both an optical spectrum and a mass spectum have been shown. The detection limit that can be reached by using this procedure has been estimated.

TRACE ANALYSIS AT A MERCAPTOACETIC ACID-MODIFIED ELECTRODE

The strong chelating ability of mercaptoacetic acid for certain metal ions is exploited for a new; kind of voltammetric sensor. Specifically, a glassy carbon electrode (GCE) surface was covalently covered br; mercaptoacetic acid. The preparation of mercap

Anodic Stripping Voltammetry at Bismuth-Coated and Uncoated Carbon Microdisk Electrodes:Application to Trace Metals Analysis in Flood Samples

This article reports on the performance of a bismuth-coated carbon microdisk electrode (BiFμE) for the determination of trace heavy metals by anodic stripping voltammetry (ASV). The BiFμE was prepared by electrodeposition of a metallic bismuth film onto the microdisk, by applying an in-situ electroplating procedure. To test the performance of the BiFμE, ASV measurements were performed on synthetic solutions containing Cd2+, Pb2+, and Cu2+ as target ions. The results indicated that cadmium and lead gave well-defined ASV peaks with no interference, and their quantitative determination could be carried out straightforwardly. In particular, linear calibration curves over the range 5.0 x 10-8-1.0 x 10-6M for both ions, and detection limits of 7.8 and 2.9 nM, for cadmium and lead, respectively, after applying a 60 sec preconcentration step, were obtained. The reproducibility was also satisfactory, the relative standard deviation (RSD) being within 2.5% for both ions. Copper, instead, gave an ASV response that. in most experimental conditions, overlapped with that of bismuth. This circumstance made the determination of copper at the BiFμE difficult. Since the latter element could be detected reliably at the uncoated carbon microdisk electrode (CμE), both BiFμE and CμE were employed, respectively, for the determination of lead and copper ions in drinking water, wine, and tomato sauce.

Capillary liquid chromatographic-high-resolution mass spectrometric analysis of ribonucleotides

A method of capillary HPLC-high-resolution MS was developed for the trace analysis of ATP, GTP, dATP and dGTP Dimethylhexylamine (DMHA) was used as ion-pairing agent for the HPLC retention and separation of the nucleotides and positive ion electrospray time-of-flight MS was used for the detection. The application of capillary HPLC allowed minimal usage of DMHA while providing excellent peak retention and resolution, which significantly reduced the ion suppression in electrospray ionization-MS analysis and thus increased the sensitivity. Adduct ions of nucleotides and DMHA were used as quantitative ions in order to achieve the best sensitivity. DMHA concentration at 5 mM in the aqueous mobile phase at pH 7 was found to be the optimal conditions for the C Is capillary column. The method was applied to determine ATP level in cultured C6 glioma cells that were treated with toxic concentrations of Zn. The results showed that the cellular ATP level decreased from 2.7 pmol/cell (<10% cell death) in average control cell samples to 0.36 pmol/cell as the concentration of Zn increased to 120 mg/l (>35% cell death) in culture medium.

铂族元素分析方法研究及其在有关地质问题中的应用

Characterization of Platinum Group Elements (PGE) has been applied to earth, space and environmental sciences. However, all these applications are based on a basic prerequisite, i.e. their concentration or ratio in the research objects can be accurately and precisely determined. In fact, development in these related studies is a great challenge to the analytical chemistry of the PGE because their content in the geological sample (non-mineralized) is often extremely low, range from ppt (10~(-12)g/g) to ppt (10~(-9)g/g). Their distribution is highly heterogeneous, usually concentrating in single particle or phase. Therefore, the accurate determination of these elements remains a problem in analytical chemistry and it obstructs the research on geochemistry of PGE. A great effort has been made in scientific community to reliable determining of very low amounts of PGE, which has been focused on to reduce the level of background in used reagents and to solve probable heterogeneity of PGE in samples. Undoubtedly, the fire-assay method is one of the best ways for solving the heterogeneity, as a large amount of sample weight (10-50g) can be hold. This page is mainly aimed at development of the methodology on separation, concentration and determination of the ultra-trace PGE in the rock and peat samples, and then they are applied to study the trace of PGE in ophiolite suite, in Kudi, West Kunlun and Tunguska explosion in 1908. The achievements of the study are summarized as follows: 1. A PGE lab is established in the Laboratory of Lithosphere Tectonic Evolution, IGG, CAS. 2. A modified method of determination of PGE in geological samples using NiS Fire-Assay with inductively coupled plasma-mass spectrometry (ICP-MS) is set up. The technical improvements are made as following: (1) investigating the level of background in used reagents, and finding the contents of Au, Pt and Pd in carbonyl nickel powder are 30, 0.6 and 0.6ng/g, respectively and 0.35, 7.5 and 6.4ng, respectively in other flux, and the contents of Ru, Rh, Os in whole reagents used are very low (below or near the detection limits of ICP-MS); (2) measuring the recoveries of PGE using different collector (Ni+S) and finding 1.5g of carbonyl nickel is effective for recovering the PGE for 15g samples (recoveries are more than 90%), reducing the inherent blank value due to impurities reagents; (3) direct dissolving nickel button in Teflon bomb and using Te-precipitation, so reducing the loss of PGE during preconcentration process and improving the recoveries of PGE (above 60% for Os and 93.6-106.3% for other PGE, using 2g carbonyl nickel); (4) simplifying the procedure of analyzing Osmium; (5)method detection limits are 8.6, 4.8, 43, 2.4, 82pg/g for 15g sample size ofRu, Rh, Pd, Ir, Pt, respectively. 3. An analytical method is set up to determine the content of ultra-trace PGE in peat samples. The method detection limits are 0.06, 0.1, 0.001, 0.001 and 0.002ng/mL for Ru, Rh, Pd, Ir and Pt, respectively. 4. Distinct anomaly of Pd and Os are firstly found in the peat sampling near the Tunguska explosion site, using the analytical method. 5. Applying the method to the study on the origin of Tunguska explosion and making the following conclusions: (1) these excess elements were likely resulted from the Tunguska Cosmic Body (TCB) explosion of 1908. (2) The Tunguska explosive body was composed of materials (solid components) similar to C1 chondrite, and, most probably, a cometary object, which weighed more than 10~7 tons and had a radius of more than 126 m. 6. The analysis method about ultra-trace PGE in rock samples is successfully used in the study on the characteristic of PGE in Kudi ophiolite suite and the following conclusions are made: (1) The difference of the mantle normalization of PGE patterns between dunite, harzburgite and lherzolite in Kudi indicates that they are residual of multi-stage partial melt of the mantle. Their depletion of Ir at a similar degree probably indicates the existence of an upper mantle depleted Ir. (2) With the evolution of the magma produced by the partial melt of the mantle, strong differentiation has been shown between IPGE and PPGE; and the differentiation from pyroxenite to basalt would have been more and more distinct. (3) The magma forming ophiolite in Kudi probably suffered S-saturation process.

激光稳频的共焦法布里-珀罗干涉仪

针对多普勒激光雷达激光源短期频率漂移低于1 MHz的要求,设计了一种共焦干涉仪作为频率标准进行稳频。通过对三种不同材料制成的共焦法布里-珀罗(Fabry-Perot)干涉仪中心频率随温度漂移情况进行分析对比,选用零膨胀微晶玻璃材料制作共焦法布里-珀罗干涉仪,腔镜和隔离器通过光胶的方式进行组合,并且置于温控精度优于0.01 K的双层密封温控箱中。经过实验测量,共焦法布里-珀罗干涉仪的自由光谱范围为370 MHz,透射谱半峰全宽(FWHM)为1.7 MHz,精细度为220。采用该共焦干涉仪进行稳频,理论稳频精度可达0.15 MHz,满足激光多普勒雷达单频激光源的稳频要求。

用于多普勒测风雷达的单频全固态激光器稳频

采用Pound-Drever-Hall技术，对用于多普勒测风雷达的种子注入激光器的主动激光器进行稳频，将其频率锁定在一个特殊设计的法珀腔上。该法珀腔总体采用零膨胀微晶玻璃材料制成，具有极高的温度稳定性。使用计算机采集鉴频信号并且进行处理。锁定后，1秒内激光器的相对频率漂移为±25kHz，一小时内的相对频率漂移为±55kHz，满足多普勒测风雷达的要求。

基于法珀标准具的激光稳频方法理论研究

介绍了使用法珀(Fabry-Perot,F-P)标准具作为频率标准的三种稳频方法,并且进行理论分析,分别得出了各种方法的鉴频曲线.通过对鉴频曲线进行比较发现边频锁定技术具有斜率大、信号强、控制范围广的优点,优于另外两种方法,是一种理想的激光稳频技术.

注入锁定激光器的边带锁频技术稳频系统优化分析

介绍了边带锁频技术稳频方法，推导出鉴频曲线，对稳频控制过程进行了分析．建立了注入锁定激光器的边带锁频技术稳频系统理论模型，讨论了相关参量对稳频效果的影响并且进行了优化．结果表明，增加入射光强，采用窄线宽的法布里一珀罗以及对法布里一珀罗进行高准确度温控都可以增强稳频效果．提出适用于注入锁定激光器的两种稳频方案并进行比较．