火焰原子吸收光谱法间接测定非金属材料中氯

报道了火焰原子吸收光谱法（ＦＡＡＳ）间接测定非金属材料中氯的方法，采用ＡｇＣｌ沉淀，测定剩余Ａｇ~＋间接求出氯含量。方法的特征浓度为０．０１４ｍｇ／Ｌ（１％吸收），检出限为０．０３２ｍｇ／Ｌ（３），测定下限为０．１１ｍｇ／Ｌ，相对标准偏差（ＲＳＤ）为１．５％～１０％，样品加标准回收率在９１．４％－１０５％之间。     

鲁米诺-双氧水-铬(Ⅲ)化学发光体系测定化探样品中痕量砷

用鲁米诺－双氧水－铬（Ⅲ）化学发光体系结合巯基棉对Ａｓ（Ⅲ）的富集分离，建立了快速的测定化探样品中痕量砷的新方法，检测线性范围为１．０×１０－４～１．０×１０１ｍｇ／Ｌ，检出限为３．４×１０－５ｍｇ／Ｌ。用于实际化探样品测定，相对标准偏差为５．５％～９．０％。     

偏最小二乘催化极谱法同时测定铂,钯,铑

应用Ｍ２７３Ａ电化学系统中的线性扫描技术，确定了０．７５ｍｏｌ／ＬＨ２ＳＯ４－１．５％ＮＨ４Ｃｌ－２．８ｍｍｏｌ／Ｌ（ＣＨ２）６Ｎ４－０．００２５％Ｎ２Ｈ４．Ｈ２ＳＯ４为偏最小二乘极谱法同时测定Ｐｔ、Ｐｄ、Ｒｈ的最佳极谱体系。Ｐｔ、Ｐｄ、Ｒｈ的线性范围为３．２ｍｇ／Ｌ、０－１５．０ｍｇ／Ｌ和０－１．０ｍｇ／Ｌ。模拟样品及实际样品的回收率在９０．３－１０７．７％之间。     

用离子色谱法测定环境样品中甲酸、乙酸、草酸

用离子色谱法分析环境样品中甲酸、乙酸、草酸,操作简便,灵敏度较好,线性范围宽。甲酸、乙酸、草酸的检出限分别为０．０２ｍｇ／Ｌ、０．１０ｍｇ／Ｌ、０．０４ｍｇ／Ｌ;样品加标回收率分别为９３％～１０６％、９４％～１０８％、９２％～１０８％;相对标准偏差分别为１．２％、２．４％、２．７％;工作曲线的线性范围分别为０．００～３０ｍｇ／Ｌ、０．００～３０ｍｇ／Ｌ、０．００～５０ｍｇ／Ｌ。该法可用于酸雨、大气     

反相高效液相色谱法测定雷公藤提取物中雷公藤甲素含量

应用反相高效液相色谱法检测了雷公藤提取物中雷公藤甲素的含量。样品经洗脱提取后,以Ｃ１８化学键合硅胶为固定相,乙腈－水（４０∶６０,Ｖ／Ｖ）为流动相,用２１０ｎｍ波长定量检测。测定结果表明,雷公藤甲素浓度在０．２５～４．００ｍｇ／Ｌ范围内线性良好,最低进样检测浓度为０．１ｍｇ／Ｌ。批内（ｎ＝５）及批间（ｎ＝５）测定相对标准偏差分别为１．９％～６．５％和２．７％～７．８％,回收率为８９．８％～９２．０％。     

铜（Ⅰ）—苯骈三氮唑络合吸附波的极谱研究与应用

本文在０．６ｍｏｌ／Ｌ ＮＨ３－ＮＨ４Ｃｌ缓冲溶液（ｐＨ＝９．８）中，Ｃｕ（Ⅱ）在滴汞电极上还原生成Ｃｕ（Ⅰ），可与苯骈三氮唑（ＢＴＡ）络合，产生一灵敏的络合吸附波，Ｅｐ＝－０．７３Ｖ（ｕｓ，ＳＣＥ）。苯骈三氮唑的浓度在０．４０－１０．０ｍｇ／Ｌ范围内与极谱波峰高呈线性关系，检测下限为０．４０ｍｇ／Ｌ，相对标准偏差为１．４％－３．２％；回收率为９７．５％－１０１．５％。     

流动注射—二极管阵列检测分光光度法同时测定铅和镉

建立流动注射－电荷耦合器件二极管阵理分光光度法装置，研究了以ｍｅｓｏ－四（４－三甲铵苯基）卟啉为显色剂同时测定铅和镉的方法，镉和铅测定的线性范围为０～２．０ｍｇ／Ｌ和０～２．５ｍｇ／Ｌ镉的检出限为０．０１４ｍｇ／Ｌ，铅为０．０１５ｍｇ／Ｌ。进样频率为６０次／ｈ，对合成样品和陶瓷食具容器浸泡液中铅和镉进行了同时测定，获得满意的结果，样品的平均标准加入回收率为１００．９％，相对标准偏差小于８．８％。     

抑制动力学分析法测定痕量铈

１引言研究了铈（Ⅲ）阻抑Ｈ２Ｏ２氧化水杨基荧光酮（ＳＡＦ）褪色的反应。反应对铈（Ⅲ）为一级反应，表观活化能为２８．７５ｋＪ／ｍｏｌ。据此建立了测定痕量铈的动力学分析法。测定条件为：ＳＡＦ：４．０ｘ１０－５ｍｏｌ／Ｌ，Ｈ２Ｏ２：０．０１０％，ＮａＯＨ：２．０ｘ１０－２ｍｏｌ／Ｌ，５０℃。线性范围０．０４～０．４４ｍｇ／Ｌ，检测限为０．０２ｍｇ／Ｌ。当溶液中的铈含量为０．１６ｍｇ／Ｌ时，３～８倍量的轻稀土，５～１１倍量的重稀土及同倍量铀和钍不干扰测定。２实验部分２．１试剂和仪器铈（Ⅲ）标准溶液：２０…     

硅胶管采样—液相色谱法测定空气中的氯氰菊酯

本文报道空气中氯氰菊酯的高效液相色谱测定方法，空气样品用硅胶管采样，经甲醇洗脱后用ＨｙｐｏｒｓｉｌＯＤＳ柱分离，紫外检测器检测，在本法的测定条件下，最低检测浓度为０．０４ｍｇ／ｍ＾３，当氯氰菊酯浓度范围为０～２５．０ｍｇ／Ｌ时，呈线性响应关系，相对标准偏差为２．４％～８．４％，本法的解吸效率为９６．８％～１００．３％，采样效率为１００％，氯氰菊酯在硅胶管中可稳定７ｄ。     

高效液相色谱法测定人血清中鬼臼乙叉甙浓度

建立了测定血清中鬼臼乙叉甙浓度的反相高效液相色谱方法。血清样品以乙酸乙酯提取,加表鬼臼毒噻吩糖甙作内标,以甲醇∶水（５５∶４５）为流动相,紫外２５４ｎｍ检测,最低检测浓度０．１ｍｇ／Ｌ,在药物浓度为０．５～５０ｍｇ／Ｌ范围内有良好的线性关系,Ｙ＝０．０１６０＋０．０３４０Ｘ,ｒ＝０．９９９１,回收率达９５．０％。日内、日间精密度分别为４．１６％和４．７６％（ｎ＝５）。用所建立的方法测定了患者的血清浓度,结果表明,方法简便、灵敏。     

双柱串联–便携式气相色谱法测定室内空气中苯系物

建立双柱串联–便携式气相色谱测法定室内空气中苯系物的方法。利用仪器内部自带的Tenax吸附剂在0.5 L/min流量下采集空气样品100 s,然后仪器迅速升温至400℃左右,对吸附剂进行热解吸进样,以微亚离子检测器(MAID)对室内空气中7种苯系物进行测定。结果表明,色谱条件为MXT–200/MXT–WAX金属毛细管柱串联色谱柱,柱温90℃,柱压103 425 Pa时,分离效果最好,且运行时间短。各组分在19.26~306.7μg/m~3范围内与色谱峰面积的平方根线性关系良好,相关系数r大于0.995。方法检出限为6.40~15.9μg/m~3,空白加标回收率为92%~114%,测定结果的相对标准偏差为6.1%~13.7%(n=6)。采用双柱串联便携式气相色谱法测定室内空气中苯系物具有快速、准确、方便等优点。     

气相色谱法测定环境空气中的微量丙烯腈

 建立了测定环境空气中丙烯腈的Tenax GC吸附-热解吸气相色谱法。方法的回收率为85.6%～105.4%,RSD为4.5%～6.2%。当采样体积为2 L时,最低检测限为0.01 mg/m3 。     

环境空气中痕量硝基苯测定方法研究

建立了Tenax富集-气相色谱仪测定环境空气中痕量硝基苯的方法。用Tenax采样管吸附环境空气中的痕量硝基苯,用1.0mL石油醚淋洗解析吸附的硝基苯,用气相色谱-电子捕获检测器进行检测,外标法定量,线性相关系数为0.9992,平均回收率为95.9%～97.1%,RSD不大于5.2%(n=5)。按采样10L计算,检出限为0.0002mg/m3,经实际样品测定完全能满足环境空气中痕量硝基苯监测的要求。     

Multi-adsorbent preconcentration/focusing module for portable-GC/microsensor-array analysis of complex vapor mixtures

A small multi-adsorbent preconcentration/focusing module for a portable GC with microsensor-array detector designed to determine complex mixtures of volatile and semi-volatile organic compounds encountered in indoor working environments is described. Candidate adsorbents were assessed on the basis of analyte thermal-desorption bandwidth and efficiency, chromatographic peak shape, and breakthrough volume against mixtures of organic compounds ranging over four orders of magnitude in vapor pressure. A capillary packed with just 12.3 mg of adsorbent material comprising Carbopack B (8 mg), Carbopack X (2.5 mg) and Carboxen 1000 (1.8 mg) provided the best tradeoff in operating variables, while maintaining sufficient capacity for a 1 L air sample containing a mixture of up to 43 compounds, each at 100 parts-per-billion, at an ambient relative humidity of up to 100%. On-column focusing and temperature programming were used to enhance chromatographic separations, and detection limits as low as 100 parts-per-trillion were achieved for a 1 L air sample using an integrated array of polymer-coated surface-acoustic-wave (SAW) sensors. Implications for field analysis of indoor air quality are emphasized.     

Development of a gas chromatography-mass spectrometry method for the determination of household insecticides in indoor air

This work presents a GC-MS method for the determination of 17 household insecticides and acaricides in indoor air. Air samples were collected with a sampling train which consisted of a glass fibre filter and two polyurethane foam plugs, followed by a high-volume air pump. Filters and plugs were analysed separately. The overall recoveries ranged from 85 to 109% (4-11% RSD). Minimum method detection limits between 0.1 and 5 ng/m3 were determined.     

Tenax采样管富集气相色谱-质谱法测定空气中的痕量酚类化合物

建立了Tenax采样管富集气相色谱-质谱测定空气中痕量酚类化合物的方法。用Tenax采样管吸附环境空气中的痕量酚类化合物,用甲醇淋洗解吸酚类化合物,洗脱液加入萘-D8作为内标,利用气相色谱-选择离子监测质谱(GC-MS/SIM)进行检测,内标法定量。该方法定性、定量准确,线性响应良好,回归曲线的线性相关系数均大于0.999,平均回收率为92.4%～102%,测定干扰小,检测灵敏度高,按采样10 L计算,空气中最低检测浓度可达0.001 mg/m3。用于实际样品测定,完全能满足环境空气中痕量酚类化合物监测的要求。     

活性氧化铝柱-气相色谱法测定工作场所空气中“四烯”的方法研究

采用活性氧化铝柱-气相色谱法对作业场所空气中乙烯、丙烯、丁烯、丁二烯进行活性炭采样,热解吸后进样分析。活性炭管对"四烯"的吸附性良好,测定结果的相对标准偏差为0.37%～2.08%;乙烯、丙烯、丁烯、丁二烯检出限分别为0.0010、0.000520、.00083、0.0003 mg/L;样品的平均解吸效率为93.7%～98.59%;样品的平均采样效率为93.9%～99.1%;乙烯、丙烯、丁烯、丁二烯穿透容量分别为9.58、.87、.4、7.1 mg;样品在室温下放置7 d,其平均样品损失率不大于5.58%,在4～10℃环境放置10 d,其平均样品损失率不大于7.11%,空气中乙烷对本方法无干扰。该法可满足职业卫生检测的要求。     

Trace determination of airborne polyfluorinated iodine alkanes using multisorbent thermal desorption/gas chromatography/high resolution mass spectrometry

A novel gas chromatography/high resolution mass spectrometry method coupled with multisorbent thermal desorption cartridges has been developed for the determination of volatile neutral polyfluorinated iodine alkanes (PFIs) in airborne samples. It allows, for the first time, simultaneous analysis of four mono-iodized perfluorinated alkanes, three diiodized perfluorinated alkanes and four mono-iodized polyfluorinated telomers in ambient air samples. 3.75 L air sample was passed through a sorbent tube packed with 150 mg of Tenax TA and 200 mg of Carbograph 1TD for analyte adsorption. Important factors during the analysis procedures, such as safe sampling volume, air sampling rate, analyte desorption and transfer strategies, were optimized and good thermal desorption efficiencies were obtained. The method detection limit (MDL) concentration ranged from 0.04 pg/L for 1H,1H,2H,2H-perfluorododecyl iodide to 1.2 pg/L for perfluorohexyl iodide, and instrument response of a seven-point calibration was linear in the range of 10–1000 pg. Travel spike recoveries ranged from 83% to 116%. Small variabilities of less than 36% were obtained near the MDLs and the differences between triplicates were even smaller (2.1–7.3%) at 200 pg spiked level. The method was successfully applied to analyze ambient air samples collected near a point source, and five PFIs were identified (10.8–85.0 pg/L), with none of the analytes detectable at the background site.     

石墨炉原子吸收光谱法测定工作场所空气中铬及其化合物

于工作场所采用微孔滤膜采样夹以5L.min-1流量采集空气样品15min,用石墨炉原子吸收光谱法测定其中铬的含量。选择灰化温度为1 300℃,原子化温度为2 400℃。铬的质量浓度在5mg.L-1以内与其吸光度呈线性关系,检出限(3s/k)为6.81×10-4 mg.m-3。应用此法分析了采集的空气样品,加标回收率在98.8%～100.7%之间,相对标准偏差(n=6)在2.2%～2.4%之间。