库仑法测定腈纶聚合原料混合液中甲基丙烯磺酸钠的含量

本文首次提出了用库仑测定法测定腈聚合原料混合液中甲基丙烯磺酸钠的含量，解决了腈纶生产染色性能控制问题之一，方法简便，快速，测定回收率９８．４％～１０２％，变异系数小于０．４％（ｎ＝７）适用于生产流程质量控制分析。     

硫铵颜色灰黑氮含量偏低的原因分析

我公司采用饱和器法工艺生产硫铵，其晶体形状为针状、片状或粉末状，正常情况颜色为白色。当条件控制不当时，由于杂质影响往往带绿色、蓝色、灰色或暗黑色，氮含量下降为20．94％～20．99％，而GB535—1995规定硫铵氮含量优等品≥21．009／6，一等品≥21．00%。本文针对这一问题进行分析探讨，通过试验，找到了原因。加强监测后，达到了提高硫铵产品质量的目的。     

硝酸镉中铁铜锌铅的FAAS快速分析测试技术

运用FAAS快速分析硝酸镉中铁、铜、锌、铅含量,建立了铁、铜、锌、铅的共振线,灯电流,酸性介质等最佳实验条件．显示出该方法具有很好的灵敏度和材料重现性,具有方法步骤简单、操作容易、干扰少等特点．测定样品铁、铜、锌、铅含量的相对标准偏差均小于1．0％（n=10）．标准加入回收率均在97．0％～98．5％范围内．适用于硝酸镉中铁、铜、锌、铅的含量控制分析和样品系统分析．     

控制电位库仑法测定铁,铅,镉,镍,钴,锌,铬单元素标准溶液中的离子含量

进行了控制电位、支持电解质各上类等条件选择，使得测定背景电流小，标准偏差低于０．２％，。并对样品进行了均匀性，稳定性检验，溶液的有效期为二年     

钒渣中二氧化钛的容量法测定

本文报道钒渣中测定二氧化钛的硫酸高铈容量法，在盐酸－硫酸混酸介质中，控制磷酸浓度大于３．５ｍｏｌ／Ｌ，在用铝片还原Ｔｉ（Ⅳ）时可以消除大量钒的干扰，方法用于实际试样分析，结果较好。     

磷光寿命的研究及生物体内色氨酸的测定

研究了磷光寿命的特性及ｐＨ、溶剂极性、碘、铅、钡、铊等重原子对磷光寿命的影响。应用磷光寿命变化法，分析生物样品中色氨酸含量。小鼠体内，血、脑、心、肺、肝、脾、肾中游离色氨酸分别为８．９μｇ／ｍＬ，１７．３，５１．８，２９．１，２９．９，４６，６８．８μｇ／ｇ。其中，组织血脑中色氨酸含量与文献报道一致。     

氢化物电热原子吸收法测定人血清中的硒

应用氢化物电热原子化装置测定了血清中的硒。采用这种技术可减少试样的基体干扰，提高分析灵敏度，而且具有良好的线性关系。方法测定灵敏度为１．２μｇ／Ｌ（１％吸收），检出限０．４μｇ／Ｌ变异系数６．３％，具有血量少、成本低、方法简便、精度好等优点。     

火焰原子吸收光谱法连续测定陶瓷绝缘子镀液中的锌、铜、铁

采用火焰原子吸收光谱法进行镉镍电池陶瓷绝缘子镀液中锌、铜、铁含量的连续测定。在优化条件下．该方法灵敏度高，干扰小，选择性和重现性好，步骤简单，操作容易，分析周期短。测定结果的相对标准偏差均小于1．0％，加标回收率为97．0％～99．0％。该法适用于镉镍电池陶瓷绝缘子镀液中锌、铜、铁含量的现场控制分析和样品系统分析。     

罂粟碱的吸附伏安行为的研究

在ＮＨ３－ＮＨ４Ｃｌ底液中，罂粟碱在汞电极上有一一线性扫描还原峰，峰电位Ｅｐｃ＝－１．４４（ｖｓ．ｓａｔ．Ａｇ／ＡｇＣｌ）。该峰具有明显的吸附性。当ＰＡＰ浓度较小时，扫速较快，搅拌富集时间较长时，电极反应完全为吸附态的ＰＡＰ的还原所控制。     

C60微电极伏安法研究

自从1990年用电弧法成功地制备出宏观量的C60和C70以来，富勒烯的电化学研究有了迅速的发展．理论研究指出，在一个C60簇化合物中，有六个吡喃环烯单元，可分别得到一个电子使五元环芳香化，从而形成C（n＝1～6）阴离子．Haufler首先报导了C60可逆的两步单电子还原，之后一些作者陆续得到了三步、四步和五步单电子电还原过程．直到达1992年，在使用混合溶剂并控制低温-10℃至5℃和-88℃至60℃条件下，才得到了C60的六步电还原伏安图．富勒烯的微电极伏安法的研究极少见报导．杨汉西等用铂微电极得到了C60三步电还原的稳态伏安图．本文在…     

基于LabVIEW 7 Express的电导滴定虚拟仪器

将常规的电导率仪通过自制的调理电路连接计算机,在LabVIEW 7 Express平台上开发了电导滴定虚拟仪器,实现了电导滴定实验数据的自动记录和自动处理。将该虚拟仪器应用到多种电导滴定,实验结果的相对误差小于0.7%,大大地提高了实验结果的重现性和准确性。该虚拟仪器界面友好、操作简便,能实时绘出滴定曲线、自动处理数据及形成结果报告。     

Automated on-line HPLC-HRGC: Instrumental aspects and application for the determination of heroin metabolites in urine

A fully automated on-line HPLC-HRGC instrument is described. Samples are loaded into an HPLC autosampler. Pre-separation is carried out, automatically transferring the previously determined HPLC fraction to GC. Total HPLC fractions are introduced into GC, using the on-column or the loop-type interface, depending on the solvent evaporation technique applied. The HPLC column is automatically backflushed with a suitable solvent during GC analysis. The instrument was used for analyzing heroin metabolites, particularly morphine, in urine samples. Raw urine extracts were injected into HPLC and analyzed by GC using FID.     

An automated vapor-generation and data collection instrument for the evaluation of chemical microsensors

An instrument has been built which can generate up to twelve different vapors from bubbler or permeation tube sources. These vapors can be individually selected, diluted to concentrations typically in the range of 1 to 10 000 mg/m³ volume and delivered at a programmable flow rate to the system output. Mixtures of two vapors can also be easily generated. The system is fully automated using a small personal computer and permits completely unattended operation during elaborate vapor-exposure sequences. Parameters describing the vapor test conditions are automatically stored in the computer disk memory, along with the sensor responses to the test. This instrument has proved to be extremely valuable for rapidly testing prototype chemical sensors.     

Validating automated analytical instruments to meet regulatory and quality standard requirements

Analytical laboratories are more and more faced to meet official regulatory requirements as described in FDA and EPA good laboratory practice, good automated laboratory practice and good manufacturing practice regulations or to officially establish quality systems, such as specified in the ISO 9000 Series quality standards, in the ISO Guide 25 or in the EN 45001 guidelines. The impact on analytical instrumentation will be the requirement for stringent validation of analytical equipment and methods which increase the overall analysis costs. An overview is presented on the validation requirements using e.g. gas chromatography, high performance liquid chromatography, capillary electrophoresis and UV-visible spectroscopy and on the strategy to meet such needs at minimal extra costs with the help of an instrument vendor. It is recommended to use instrument hardware that has already built-in tools for self-verification and which is to be validated at the vendor's site. Performance testing in the user's laboratory is done using standard operating procedures as supplied with the instrument. If resources in the user's laboratory are limited, the performance verification is done by the vendor. Software and the entire computer system is validated prior to shipment at the vendor's site. Acceptance testing is done in the user's environment following the vendor recommendations. Analytical methods are validated automatically at the end of method development using a dedicated software. The software can be customized such that it can also be used for daily automated system suitability testing. Security and integrity of analytical data are ensured by saving the raw data together with instrument conditions and instrument log-books in check-sum protected binary register files for long-term archiving.     

基于LabVIEW 8.0的pH电位滴定虚拟仪器

运用离子选择性电极、调理电路、DAQ卡和计算机,构建了基于LabVIEW 8.0的电位滴定虚拟仪器,实现了电位滴定实验数据的自动记录和自动处理.将该虚拟仪器应用到乙酸等的电位滴定实验表明,实验结果相对标准偏差小于0.65%,提高了实验结果的重现性和准确性;且虚拟仪器界面友好、操作简便、实时绘出滴定曲线,自动处理数据及即时得到结果.     

低功耗便携式温度自动记录仪的设计

综合应用计算机技术、通信技术、数理统计和控制论的有关知识设计了能自动检测并记忆温度的仪器,该仪器具有掉电自动保护、低功耗、便携的特点,并具有智能性,能预测温度变化趋势,有超前警示和及时报警两种报警功能。     

Automatic control of the ion-illumination angle in a spark-source mass spectrometer

Automatic adjustment of only the spark-gap width in a spark-source mass spectrometer does not ensure that optimum conditions of electrode geometry are maintained with respect to the ion-optics system. A device has been developed which simultaneously maintains a constant gap width and also a more constant z-axis ion-illumination angle. This is the first development to utilize ion-optics parameters to adjust the sparking electrodes automatically. The system maintains the electrodes in an optimum configuration such that higher and more constant instrument sensitivity is maintained automatically. In addition, a significant improvement in the precision of instrumental response is demonstrated. It appears that relative isotopic abundances can be determined directly by the spark-source method which are comparable to those obtained in some cases by surface ionization or by electron bombardment. Results are given that support this contention.     

Trace analysis with automatic printout based on reaction rate measurements: determination of osmium

An instrument is described which measures reaction rates and converts the information to a voltage which is calibrated to read the concentration of the desired constituent. It is applied to the determination of trace amounts of osmium in solution, based upon catalysis of the Ce(IV)-As(III) reaction. The instrument is versatile, sensitive, and capable of high precision. After a short calibration procedure, it is necessary only to activate the instrument once between runs, and the concentration of sample is printed on tape automatically. Osmium is determined in the 1–60 p.p.b. range with relative standard deviations and accuracy of about 1%. At the lower end of the concentration range this corresponds to an error of about 2.5·10^-11 g of osmium. Measurement times range between 15 and 150 sec with average analysis times of 3–4 min per sample, including initial calibration and other manipulations.     

Rapid and accurate titrations with a convenient and compact automatic derivative spectrophotometric titrator

A convenient and compact automatic derivative spectrophotometric titrator is described which is suitable for automatically performing a wide variety of the well known color indicator titrations without any procedure modifications and usually with few, if any, pretitration considerations and instrument adjustments The results for many acid-base and oxidation-reduction titrations are presented to illustrate the general applicability and important characteristics of the instrument     

Rapid determination of aliphatic amines in water samples by pressure-assisted monolithic octadecylsilica capillary electrochromatography-mass spectrometry

A pressure-assisted capillary chromatography-mass spectrometry method based on the use of a monolithic octadecylsilica (ODS) capillary is proposed for the determination of aliphatic amines. A 25 mM citric acid buffer containing 10% methanol is used as running electrolyte. Separation is achieved by simultaneously applying a capillary electrophoresis (CE) voltage of 13 kV and an overimposed pressure of 8 bar. The use of pressure is required to ensure stable electrospray conditions. Analysis times are reduced by using a capillary column consisting of a 30 cm long monolithic silica capillary column bound with ODS and a fused-silica capillary column also 30 cm long. The proposed method was successfully applied to the determination of low-molecular-weight aliphatic amines in tap and river water. The analysis of real samples requires cleanup and preconcentration, which can be performed automatically by inserting a minicolumn in the replenishment system of the commercial instrument.