萃取-非水介质氢化物发生-ICP-AES中的干扰及Ni-Fe基合金的分析

本文结合溶剂萃取研究了非水介质中氢化物发生-ICP-AES的分析条件、干扰等因素的影响。利用KI~+H_2SO_4/MIBK萃取体系将As,Sb,Bi萃取到MIBK中而与基体元素分离,然后将该有机相与甲酸按等体积混合后,即可直接进行氢化物发生-ICP-AES分析。还对影响萃取和氢化物发生的一些因素及共存元素的干扰进行了讨论。该方法应用于Ni-Fe基合金中As和Sb的分析,取得了较满意的结果。

Interface of chip-based capillary electrophoresis-inductively coupled plasma-atomic emission spectrometry (CE-ICP-AES)

An interface of chip-based capillary electrophoresis (CE)-inductively coupled plasma-atomic emission spectrometry (ICP-AES) that is based on cross-flow nebulization has been developed. A polydimethylsiloxane (PDMS) CE-chip with conventional cross channel layout was used. A stainless steel tube was placed orthogonal to the exit of the CE separation channel for cross flow nebulization. A supplementary flow of buffer solution at the channel exit was used to improve nebulization efficiency. Two capillaries were inserted into the CE chip near the inlet of the separation channel for sample and buffer solution injection. Syringe pumps were used to manipulate the flow rate and flow direction of the sample, buffer, and supplementary buffer solution. Peak broadening due to the shape (bulb and tube-shaped) and size of the spray chambers was studied. The smaller tube-shaped spray chamber was used because of smaller peak broadening effect due to aerosol transport. The nebulization and transport efficiency of the CE-ICP interface was approximately 10%. Ba2+ and Mg2+ ions were eluted from the CE-chip within 30 s. Resolution of the Ba2+ and Mg2+ peaks was 0.7 using the chip-based CE-ICP-AES system.

ICP发射光谱法中粉末进样方法的研究及水系沉积物样品的分析

用ICP-AES法分析样品时，多数样品为溶液。处理难溶样品费时多，易沾污，有时需加入大量试剂；使空白或背景增大影响分析灵敏度。本文研究将固体粉末悬沲体直接引入等离子体的进样方法，试图建立一种快速，简便并能满足一定精度和灵敏度要求的分析方法。本文使用美国Baird PS-1型光电直读ICP发射光谱仪器，自制改进型的GMK雾化器，研究了影响粉末悬沲体样品谱线强度、背景强度和线背比的因素；谱线干扰及其校正；用一套人工合成样品做工作曲线及水系沉积物样品的分析。我们从实验中观察到：1. 粉末粒度是影响进样的重要因素，粒径越小，谱线强度越大。2. 入射功率增大时，所有研究元素的谱线强度和背景强度都增大，但多数元素的线背比下降。3. 载气流量较小时，硬线的强度及线背比较大；反之则软线强度及线背比较大。所有元素的背景强度都随载气流量增加而减小。4. 观察高度较低，硬线强度及线背比较大，反这则软线强度及线背比较大；多数元素的背景强度随观察高度增高而减小。5. 向粉末悬沲体中加入少量异丙醇，多数元素的背景强度减少，谱线强度及线背比增大。6. 增大样品提升率，谱线强度和线背比都随之增大。7. 增大粉末悬沲体的浓度，谱线强度增加，但浓度太大易堵，我们认为浓度为10mg/ml较合适。本文用元素间干扰比较正谱线干扰，用不同形态的样品（溶液和固体粉末悬浮体）测定其干扰比，发现它的干扰比数值相近。用一套人工合成样品做工作曲线，动态范围较宽，检出限与溶液法相当。相对标准偏差为1.4 ～ 4.6%，相关系数大于0.997。我们还用八个GSD水系沉积物标准参考样品做校准曲线，检出限和相对标准偏差，实验表明：加大功率有助于克服粒度和矿物组成不同等因素对分析元素的影响，八个GSD样品与人工合成标样符合较好。用直接粉末法分析样品时有基体干扰，用GSD样品做的检出限和相对标准偏差都不如合成样品。用该方法分析人工材料中的杂质可能更为合适。

高纯金属钕中镧、铈、镨、钐和钇的ICP光谱测定

本文提出了用ICP-AES直接同时测定高纯金属钕中镧、铈、镨、钐和钇的新方法。描述了在钕样品溶液中加入乙醇后对测定灵敏度的影响,乙醉量的影响以及ICP的几个主要工作参数的选择等。当样品溶液中稀土元素的总浓度为5毫克/毫升,乙醇浓度为70%(V/V)时,测定下限分别为镧0.0020%,铈0.0030%,镨0.010%,钐0.0050%和钇0.0010%其相对标准偏差为2.9-5.7%。

Thickness And Component Distributions Of Yttrium-Titanium Alloy Films In Electron-Beam Physical Vapor Deposition

Thickness and component distributions of large-area thin films are an issue of international concern in the field of material processing. The present work employs experiments and direct simulation Monte Carlo (DSMC) method to investigate three-dimensional low-density, non-equilibrium jets of yttrium and titanium vapor atoms in an electron-beams physical vapor deposition (EBPVD) system furnished with two or three electron-beams, and obtains their deposition thickness and component distributions onto 4-inch and 6-inch mono-crystal silicon wafers. The DSMC results are found in excellent agreement with our measurements, such as evaporation rates of yttrium and titanium measured in-situ by quartz crystal resonators, deposited film thickness distribution measured by Rutherford backscattering spectrometer (RBS) and surface profilometer and deposited film molar ratio distribution measured by RBS and inductively coupled plasma atomic emission spectrometer (ICP-AES). This can be taken as an indication that a combination of DSMC method with elaborate measurements may be satisfactory for predicting and designing accurately the transport process of EBPVD at the atomic level.

Origin of Chinese ancient glasses;study on the earliest Chinese ancient glasses

The earliest Chinese ancient glasses before the West Han Dynasty (200 BC) from different regions are studied. The glass samples were unearthed from Hunan, Hubei, Yunnan, Sichuan, Guizhou, Guangdong and Xinjiang of China. The chemical composition of these glasses samples is analyzed by proton induced X-ray emission (PIXE) technique, energy dispersive X-ray fluorescence (EDXRF) method and inductively coupled plasma atomic emission spectrometry (ICP-AES). It is shown that the glass chemical compositions belong to barium-lead silicate BaO-PbO-SiO2, potash soda lime silicate K2O (Na2O)-CaO-SiO2 (K2O/Na2O > 1), soda potash lime silicate Na2O (K2O)-CaO-SiO2 (K2O/Na2O < 1) and potash silicate K2O-SiO2 glass systems, respectively. The origins of the earliest Chinese ancient glasses are discussed from the archaeological and historical points of view. These four types of Chinese ancient glasses were all made in Chinese territory using local raw materials. The glass preparation technology was related to the Chinese ancient bronze metallurgy and proto-porcelain glaze technology. The glass technology relationship between the East and the West is analyzed at the same time.

中国出土的一批战国古玻璃样品化学成分的检测

对化学成分体系的确定是中国古代玻璃研究中很重要的一个方面，为此，用外束质子激发X荧光技术（PIXE）、电感耦合等离子体原子发射光谱分析（ICP-AES）等方法，对新疆、湖北、河南和重庆等地区出土的一批战国时期的玻璃珠（包含镶嵌玻璃珠）、玻璃璧样品进行了检测。结果表明，战国时期中国境内同时存在PbO-BaO-siO2、K2O-SiO2、Na2O-CaO-SiO2三种硅酸盐玻璃，分布的地域范围从中国的新疆东部一直到长江、黄河流域，以及南方的四川、贵州等地区。中国古代的PbO-BaO-SiO2和K2O-SiO玻

广西合浦地区出土汉代古玻璃的质子激发X荧光分析

采用改进的外束质子激发x射线荧光、电感耦合等离子体原子发射光谱分析等技术，对广西合浦地区出土的一批汉代古玻璃样品的化学成分和结构特性等进行了检测。结果表明：两汉时期，合浦地区的古代玻璃存在K2O—SiO2、PbO-BaO-SiO2、PbO—SiO2、Na2O-K2O-PbO-SiO2、（Na2O）K2O-CaO—SiO2等多种类型，但绝大多数为K2O—SiO2玻璃。表面风化可引起K2O-SiO2玻璃表面K2O等助熔剂的流失和富硅层的形成。综合化学成分以及器型特征，认为我国汉代K2O—SiO2玻璃制造技术可

Growth and spectroscopic characteristics of Yb : GSO single crystal

For the first time, a high optical quality 10 at.% Yb3+-doped gadolinium oxyorthosilicate laser crystal Gd2SiO5 (GSO) was grown by the Czochralski (Cz) method. The segregation coefficient of Yb3+ was studied by the inductively coupled plasma atomic emission spectrometer (ICP-AES) method. The crystal structure has monoclinic symmetry with space group P2(1)/c; this was determined by means of an x-ray diffraction analysis. The absorption spectra, fluorescence spectra and fluorescence decay curves of Yb3+ ions in a GSO crystal at room temperature were also studied. Then, the spectroscopic parameters of Yb:GSO were calculated. The advantages of the Yb:GSO crystal include high crystal quality, quasi-four-level laser operating scheme, high absorption cross-sections and particularly broad emission bandwidth (similar to 72 nm). The results indicated that the Yb:GSO crystal seemed to be a very promising laser gain medium in diode-pumped femtosecond laser and tunable solid state laser applications when LD pumped at 940 and 980 nm.

Czochralski growth and crystal structure of cerium-doped Lu2Si2O7 scintillator

Cerium-doped lutetium pyrosilicate crystal, Ce:Lu2Si2O7 (Ce:LPS), was grown by the Czochralski method. The segregation coefficient of Ce3+ ion was studied by the ICP-AES method. X-ray diffraction analysis showed that the structure of Ce:LPS crystal was monoclinic symmetry with space group of C2/m. Perfect cleavage planes (110) and imperfect cleavage planes (001) were observed by optical microscope. The reasons why it is difficult to grow crack-free crystals were studied. After optimized growth parameters, a Ce:LPS crystal with dimension of Phi 25 x 30 mm was grown, which is colorless, high optical quality, cracking-free and no inclusions. The transmittance of Ce:LPS crystal from 380 to 800 nm is over 82% and there is no observable absorption. (c) 2005 Elsevier B.V. All rights reserved.

Yb：FAP晶体的生长及光谱性能

应用中频感应提拉法生长出不同掺杂浓度的Yb：FAP激光晶体，运用电感耦合等离子体原子发射光谱仪（ICP-AES）测定了Yb^3＋离子存Yb：FAP晶体中的分凝系数约为0．03。随着晶体的生长，晶体中Yb^3＋离子的轴向浓度逐渐增大。研究Yb：FAP晶体在77K和300K温度下的吸收光谱发现，振动谱的变化主要是由电子-声子近共振耦合作用引起的。系统地研究了不同Yb^3＋离子掺杂浓度Yb：FAP晶体的吸收光谱和荧光光谱。通过吸收光谱的测量计算了晶体的吸收截面。Yb：FAP晶体在904nm和982nm处存在Yb

Yb：FAP晶体生长

采用中频感应提拉法生长了Yb：FAP晶体。对晶体生长中影响晶体质量的因素特别是原料的处理、CaF2的挥发等进行了研究和讨论。运用ICP-AES测定Yb^3＋离子在Yb：FAP晶体中的分凝系数。对Yb：FAP晶体进行了高分辨X射线的四圆衍射实验，结果表明晶体具有比较高的晶格完整性。

Growth and spectral properties of Yb : FAP single crystal

In this paper, single crystal of ytterbium (Yb) doped Ca-5(PO4)(3)F (FAP) has been grown along the c-axis by using the Czochralski method. The segregation coefficients of Yb3+ in the Yb:FAP crystal has been determined by ICP-AES method. The absorption spectrum, fluorescence spectrum and fluorescence lifetime of the Yb:FAP crystal has been also measured at room temperature. In the absorption spectra, there are two absorption bands at 904 and 982 nm, respectively, which are suitable for InGaAs diode laser pumping. The absorption cross-section (sigma(abs)) is 5.117 x 10(-20) cm(2) with an FWHM of 4 nm at 982 nm. The emission cross-section is (sigma(em)) 3.678 x 10(-20) cm(2) at 1042 nm. Favorable values of the absorption cross-section at about 982 nm are promising candidates for laser diode (LD) pumping. (c) 2005 Elsevier B.V. All rights reserved.

ARL—3520AES电感耦合等离子体发射光谱仪疑难故障的分析与排除

介绍了在瑞士ＡＲＬ公司生产的ＩＣＰ—３５２０ＡＥＳ型电感耦合等离子体原子发射光谱仪上存在的一种疑难故障的分析与排除过程，对同类型仪器的故障分析有借鉴作用．