POM／EVA共混物的研究

用力学测试、扫描电镜（ＳＥＭ）、热分析（ＤＳＣ）等手段研究了聚甲醛（ＰＯＭ）与乙烯－醋酸乙烯酯共聚物（ＥＶＡ）共混物（ＰＯＭ／ＥＶＡ）的力学性能及其微同形态；用聚甲醛与马来酸二丁酯（ＤＢＭ）的接枝物（ＰＯＭ－ｇ－ＤＢＭ）作相溶剂，能改变共的两相间的粘结力，从而提出了共混物的力学性能，ＳＥＭ观察表明接枝物的加入改变了ＰＯＭ／ＥＶＡ共混物的断裂方式，微观形态及结晶性能，对其热性能影响不大；通过改变ＰＯ     

气动雾化进样时微波等离子体炬作为激发光源的性能研究

以气动雾化进样研究了微波等离子体炬（ＭＰＴ）放电作原子发射光谱法激发光源的性能，包括ＭＰＴ的获得、操作参数的影响、样品引入及其分析性能，并与微波诱导等离子体进行了比较，证明ＭＰＴ放电作激发光源有良好的分析性能．     

气动雾化进样时微波等离子体炬作为激光发源的性能研究

以气动雾化进样研究了微波等离子体矩（ＭＰＴ）放电作原子发射光谱法激光发源的性能，包括ＭＰＴ的获得、操作参数的影响、样品引入及其分析性能，并与微波诱导等离子体进行了比较，证明了ＭＰＴ放电作激发光源有良好的分析性能。     

流动注射在线液－液萃取循环雾化ICP发射光谱法测定水中痕量重金属

叙述了流动注射在线液－液萃取循环雾化ＩＣＰ摄谱法测定水样中痕量镉、钴、铜、铁、钼、镍、钒等重金属的分析方法，采用ＡＰＤＣ为螯合剂将待测元素萃取在ＭＩＢＫ中，直接注入可拆式循环雾化系统进行ＩＣＰ摄谱法测定。方法简便、快速，适合于水样中μｇ·Ｌ￣（－１）级重金属元素测定。     

MZrO3（M=Ba,Sr,Ca）水热合成中结构与反应活性的关系

ＭＺｒＯ_３（Ｍ＝Ｂａ，Ｓｒ，Ｃａ）水热合成中结构与反应活性的关系郑文君，庞文琴（吉林大学化学系，长春，１３００２３）关键词水热合成，ＭＺｒＯ_３（Ｍ＝Ｂａ，Ｓｒ，Ｃａ），结构，反应活性钙钛矿型复合氧化物ＭＺｒＯ３（Ｍ＝Ｂａ，Ｓｒ，Ｃａ）是重要的功能陶...     

有机试剂雾化进样电感耦合等离子体原子发射光谱特性的研究

利用流动注射技术对有机试剂雾化进样情况下电感耦合等离子体（ＩＣＰ）的特性进行了研究。考察了有机试剂对ＩＣＰ放电外观的影响。对ＩＣＰ的局部热平衡状态作了判定。由Ｍｇ２７８．３０ｎｍ和Ｍｇ３３３．６７ｎｍ二线法对有机试剂负载和水负载情况下ＩＣＰ的激发温度分别作了计算。讨论了试剂分子裂解产物的光谱干扰问题。     

表面热电离质谱的进展

本文评述了表面热电离质谱（ＴＩＭＳ），特别是负离子质谱（ＮＴＩ－ＭＳ）对非金属和具有高电离电位的金属元素的同位素测定的进展，引用文献３４篇。     

对甲基酚醛树脂热裂解产物的固体^13C NMR

对甲基酚醛树脂热裂解产物的固体~（１３）ＣＮＭＲ谢德民，张建国，王存国，王荣顺（东北师范大学化学系，长春，１３００２４）关键词对甲基酚醛树脂，裂解，固体~（１３）Ｃ，ＮＭＲ酚醛树脂经热裂解制备的聚并苯导电材料在空气中稳定，由裂解温度可控制碳化程度，其本...     

离聚物及其共混体系的研究 Ⅰ．聚合物链引入同种离子的增容作用

 通过苯乙烯（Ｓ）及甲基丙烯酸正丁酯（ｎＢｍａ）分别与少量的甲基丙烯酸（Ｍａａ）和马来酸酐（Ｍａｎ）共聚，从而在聚苯乙烯（ＰＳ）及聚甲基丙烯酸丁酯（ＰＢｍａ）链上分别引入了功能基因羧酸基和酸酐基，制得共聚物ＳＭａａ、ＢｍａＭａａ、ｓＭａｎ及ＢｍａＭａｎ．通过将这些共聚物分别交换上金属离子制备得相应的离聚物（Ｉｏｎｏｍｅｒ）及其共混物．红外光谱（ＩＲ）、差示扫描量热法（ＤＳＣ）及透射电镜（ＴＥＭ）的研究结果表明，共混物两组分均具有同种（负）电荷时，仍表现明显的增容作用．     

离聚物及其共混体系的研究 Ⅰ．聚合物链引入同种离子的增容作用

通过苯乙烯（Ｓ）及甲基丙烯酸正丁酯（ｎＢｍａ）分别与少量的甲基丙烯酸（Ｍａａ）和马来酸酐（Ｍａｎ）共聚，从而在聚苯乙烯（ＰＳ）及聚甲基丙烯酸丁酯（ＰＢｍａ）链上分别引入了功能基因羧酸基和酸酐基，制得共聚物ＳＭａａ、ＢｍａＭａａ、ｓＭａｎ及ＢｍａＭａｎ．通过将这些共聚物分别交换上金属离子制备得相应的离聚物（Ｉｏｎｏｍｅｒ）及其共混物．红外光谱（ＩＲ）、差示扫描量热法（ＤＳＣ）及透射电镜（ＴＥＭ）的研究结果表明，共混物两组分均具有同种（负）电荷时，仍表现明显的增容作用．     

一种新型的ICP-AES用低功率微波热雾化系统

热雾化法自问世以来 [1 ,2 ] ,就以其较高的雾化效率及传输效率受到学者们的普遍重视 .最近 Bordera等[3] 提出了一种新的热雾化系统 (该系统采用聚焦微波炉作热雾化系统中液体样品的热源 ,即微波热雾化系统 ,简称 MWTN) ,同时还考察了实验变量对雾滴粒径分布的影响 ,并预期 MWTN具有较高的雾化效率 .本文所提出的热雾化系统与 Bordera等所建立的 MWTN系统在原理上虽然相同 ,但由于采用了新的微波器件 ,所需功率大大降低 ,因此 ,是一种新的低功率 MWTN系统 .在本实验中 ,我们对酸的浓度、载气流量、样品提升量等参数对 Mg的发射强度…     

New developments in thermospray sample introduction for atomic spectrometry

The status of thermospray sample introduction for analytical atomic spectrometry was last reviewed in 1992. In this review, we summarize developments in this field since that time, including investigations of aerosol generation processes, noise diagnosis and control with inductively coupled plasma-atomic emission or mass spectrometry (ICP-AES/MS), high flow thermospray, the use of dual-stage desolvation systems based on membrane dryers, and the utilization of thermospray with axially viewed ICP-AES. Since a major advantage of methods based on thermospray is improved limits of detection, the emphasis for applications of thermospray with ICP spectrometries remains focused on environmental sample types, particularly with ICP-MS. Relatedly, the use of thermospray as a means for the direct speciation of Se is also under development.     

Use of a multi-tube Nafion® membrane dryer for desolvation with thermospray sample introduction to inductively coupled plasma-atomic emission spectrometry

A multi-tube Nafion^® membrane dryer used as a part of a desolvation system in conjunction with thermospray nebulization was optimized and characterized with inductively coupled plasma-atomic emission spectrometry (ICP-AES). Either argon or nitrogen could be used as the sweep gas, and optimum conditions were found to be at low temperature and low sweep gas flow rate. Analyte sensitivity was not significantly affected by placing the membrane between the plasma and the nebulizer, although about 20% of the analyte entering the dryer is lost within the dryer. A dual role of the membrane dryer was demonstrated. As a secondary step within the desolvation system, it enabled a high desolvation efficiency of 99.94% for aerosols from 1% (v/v) nitric acid. Plasma solvent load could be reduced to 0.9 mg min⁻¹ with a tap water cooled condenser combined with the membrane dryer, compared to 21 mg min⁻¹ with the normal chilled condenser desolvation system. Meanwhile, the membrane was also found to act as a pulse dampener, eliminating the plasma pulsation in the central channel caused by thermospray nebulization and thus improving the analytical performance of the system. The average relative standard deviations (RSD) with the optimized membrane/thermospray system were 0.83% and 0.60% for the background and analyte signals, respectively, which were reduced by a factor of 1.9 and 2.7 for the background and analyte signals, respectively, compared to thermospray without the membrane desolvation, and were essentially identical to those obtained with pneumatic nebulization sample introduction. The improvements in detection limits with the membrane/thermospray system were 1.2–3.0 times with an average factor of 1.8 compared to thermospray without the membrane dryer, and 18–68 times with an average factor of 39 compared to the standard pneumatic nebulization sample introduction system without a desolvation unit. The detection limits for Mn, Mg, Cr and Cd with the present thermospray/membrane system were comparable to those reported for pneumatic nebulization ICP mass spectrometry.     

Utility of solution electrochemistry mass spectrometry for investigating the formation and detection of biologically important conjugates of acetaminophen

On-line formation and detection of glutathione and cysteine conjugates of acetaminophen were accomplished by the interfacing of a coulometric electrochemical cell with a thermospray mass spectrometer in a flow-injection experiment using a liquid chromatographic pump. Formation of the conjugates occurred only after acetaminophen was oxidized electrochemically by a two-electron transfer to N-acetyl-p-benzoquinoneimine and reacted in a mixing tee with either glutathione or cysteine. The newly formed conjugate was detected by thermospray mass spectrometry by observing the [M + H]+ ion for the acetaminophen-glutathione conjugate at m/z 457, or the [M + H]+ ion for the acetaminophen cysteine conjugate at m/z 271. Both the glutathione and cysteine conjugates produced a common fragment ion at m/z 184. The on-line reaction of glutathione and electrochemically generated N-acetyl-p-benzoquinoneimine was monitored at varying pH. At pH 8.5 the ion intensity for the acetaminophen-glutathione conjugate was greater than at lower pH, indicating that lower proton concentration enhanced the reaction of glutathione with N-acetyl-p-benzoquinoneimine. This on-line electrochemical-thermospray mass spectrometric method demonstrated that acetaminophen conjugates may be formed and detected in the time frame of 1 s.     

Characterization of aerosols generated by thermospray nebulization for atomic spectroscopy

The performance of an inductively coupled plasma (ICP) for atomic emission spectroscopy (AES) is strongly dependent upon the sample introduction system. The Thermospray Vaporizer has recently been shown to yield enhanced sensitivity compared to conventional pneumatic nebulizers when used as a sample introduction source for the ICP. This report is a study of the properties of the aerosols produced by the thermospray. Aerosol particle diameter distributions have been related to droplet size distribution and nebulization efficiencies as a function of the relevant variables of the nebulization system. The results help explain high emission intensities and lower detection limits achieved using the thermospray. The higher efficiencies with thermospray, compared to conventional pneumatic nebulization, also makes the thermospray a prime candidate for sample introduction into molecular gas ICPs.     

Liquid chromatography-thermospray mass spectrometry of DNA adducts formed with mitomycin C, porfiromycin and thiotepa

High-performance liquid chromatography (HPLC) and thermospray mass spectrometry were combined for the analysis of DNA adducts formed from the interaction of the anticancer drugs mitomycin C, porfiromycin and thiotepa with calf thymus DNA. The adducts formed from reaction of mitomycin C and porfiromycin with DNA were separated from unmodified nucleosides by HPLC on a C18 column and identified by thermospray mass spectrometry. Thiotepa DNA adducts readily depurinated from DNA and were chromatographed and identified by thermospray liquid chromatography-mass spectrometry as the modified bases without the ribose moiety attached. The utility of thermospray mass spectrometry for the identification of microgram quantities of nucleoside adducts and depurinated base adducts of these anticancer drugs was demonstrated.     

热喷雾作为电感耦合等离子体原子发射光谱的进样技术

设计并建立了热喷雾器及其去溶装置。用热喷雾作为电感耦合等离子体原子发射光谱的进样技术，并对其性能作了系统研究。与气动雾化器比较，对２３个元素检出限的改善为５￣２０倍。     

Application of an HPLC-FTIR modified thermospray interface for analysis of dye samples.

Previously, we developed a reversed-phase HPLC method compatible to high performance liquid chromatography diffuse reflectance Fourier-transform infrared (HPLC-FTIR) thermospray interface for the analysis of dyes. Dye separation achieved with a mixed-mode (SCX-ODS) column using a small gradient (90 to 80% water with acetic acid) and pH 3.25; 10 to 20% acetonitrile was considered to be suitable for HPLC-FTIR. A constant-voltage setting for the thermospray temperature (227 degrees C) was successfully used for this gradient condition. The HPLC-separated components deposited as a series of concentrated spots on a moving tape were scanned by specially developed HPLC-FTIR software. Excellent repeatability of the thermospray deposition FTIR chromatograms and IR spectra was obtained. The interface-derived spectra of the separated components of formulated and purified reactive dyes were compared and differences in spectral features were observed.     

Evaluation of an automated thermospray liquid chromatography-mass spectrometry system for quantitative use in bioanalytical chemistry.

An automated thermospray liquid chromatography-mass spectrometry system is described, including an autosampler and a gradient liquid chromatography system controlled from the mass spectrometer data system. The performance and reliability of the equipment during unattended operation were evaluated by repeated injections of standard solutions of some antiasthmatic drugs, using deuterium-labelled analogues as internal standards. High sensitivity and reproducibility were achieved during a 19-hour run, incorporating gradient elution and a total of 54 injections. The relative standard deviation of the peak area measurement of the internal standards was in the range of 6.5-8.2%. The corticosteroid budesonide can be routinely measured in plasma down to 0.1 nmol/l. Direct injection of a small plasma volume into the thermospray liquid chromatography-mass spectrometry system could be used to monitor drug plasma levels during a toxicity study in dogs.     

Thermospray nebulizer as sample introduction technique for microwave plasma torch atomic emission spectrometry

A thermospray nebulizer was used as a sample introduction device for microwave plasma torch (MPT) atomic emission spectrometry (AES). Experimental parameters, including the power supplied to the MPT, the flow rates of support and carrier gases, the observation height, the sample uptake rate, the thermospray working temperature, the temperature of the aerosol spray chamber and cooling water were optimized. Under optimum conditions, the relative standard deviation (RSD) of 10 measurements for 21 elements is in the range 0.3–2.0%. The detection limits were improved in comparison with the ultrasonic nebulizer as sample introduction technique for MPT–AES. The inclusion of 20% methanol into the MPT showed there is no effect on the stability of MPT discharge. The technique can thus be held to have the potential for interface to reverse-phase HPLC systems.