ICP—AES测定钯—钡合金中常量钡

本文采用ＩＣＰ－ＡＥＳ法测定钯－钡合金中常量钡。考察了其体及无机酸的存在对钡发射线强度的影响，采用标准曲线法对含量分别为０．５９％和２６．０４％的两个试样进行了测定，结果满意。     

ICP-AES法同时测定合金工具钢中的Cr、Mo、V

采用盐酸－硫酸对以Cr,Mo,V为主要合金元素的工具钢试样进行消化，用ICP－AES法同时测定试样中Cr,Mo,V的含量。方法简便，结果满意。方法的加标回收率为95．5％－103．2％，相对标准偏差（n=9)为1．61％－6．64％。     

ICP－AES测定钯－钡合金中常量钡

本文采用ＩＣＰ－ＡＥＳ法测定钯－钡合金中常量钡。考察了基体及无机酸的存在对钡发射线强度的影响。采用标准曲线法对含量分别为０．５９％和２６．０４％的两个试样进行了测定，结果满意。     

电感耦合等离子体-原子发射光谱法测定贵金属-难熔金属涂布液中的铱和钌

报道了采用ＩＣＰ－ＡＥＳ法测定贵金属－难溶金属涂布液中铱和钌。考察了基体及无机酸对发射强度的影响。采用铬作为内标元素以提高方法的精密度。在优化条件下,对Ｉｒ１０,Ｉｒ２０两个试样进行了测定。其相对标准偏差（ｎ＝９）Ｉｒ为０．５８％～１．３６％,Ｒｕ为０．５４％～０．７６％;回收率Ｉｒ为９７％～１０３％、Ｒｕ为９６％～１０３％。     

催化动力学分析离子选择性电极法测定钌(Ⅲ)

本文采用ＩＯ离子选择性电极跟踪钌（Ⅲ）催化ＩＯ氧化甲基红反应，实现了动力学法测定痕量钌（Ⅲ）。测定线性范围为５．０×１０－１１～２．４×１０ｍｏｌ　Ｌ－，检出限为５．０×１０－１２ｍｏ１Ｌ－１。方法选择性好、灵敏度高，对载钌的４Ａ分子筛试样中钌含量测定结果满意，相对标准偏差小于８．４％，回收率在９６％～１０４％之间。同时对该反应体系的有关性质也进行了初步研究。     

鲜魔芋及其种植土壤中矿物元素的ICP-AES法测定

采用电感耦合等离子体原子发射光谱法（ICP－AES）测量了不同产区鲜魔芋球茎及其种植土壤中10种矿物元素的含量，并初步讨论其相关性；采用湿法消化处理样品并考察了不同元素测定的精密度、回收率；测定的相对标准偏差（RSD）均小于2％，回收率为95％－104％，结果可信度高。     

氢化物发生/原子吸收分光光度法测定食盐中铅

采用氢化物／原子吸收光谱法测定食盐中痕量铅，使用流动注射氢化物发生器，自动吸入试样和NaBH4溶液，空气／乙炔火焰加热石英管原子化器。对测定条件及共存元素的允许量进行了研究，采用K3[Fe(CN)6]作氧化剂。方法的灵敏度是0．28n/mL/1％吸收，检出限为0．10ng/mL，回收率在94％－102％之间，RSD为2．1％－5．3％。     

电感耦合等离子体原子发射光谱法测定中药方剂煎煮液中的微量元素

本文采用HNO3－H2O2对中药方剂煎煮液进行处理，拟定了电感耦合等离子体原子发射光谱法同时测定试样中12个微量元素的方法，选择了仪器的最佳工作条件，考察了基本效应的影响。在选定条件下，12个微量元素的检出限为0．10－5．0ng/g，相对标准偏差为0.10%-9.5%(n=10),加标回收率为85％－103％。该方法简单、快速，已用于大量样品的检测，分析结果满意。     

同位素稀释气相色谱-谱法快速测定酱油中3-氯-，2-二醇量

采用同位素稀释气相色谱－质谱联用（GC－MS）法，快速测定酱油中3－氯－1，2-丙二醇（3-MCPD）的含量。试样中加入3－氯－1，2-丙二醇的氘代同位素作为内标，经超声混匀后加入到自行填装的弗罗里硅土柱中，以乙醚洗脱，洗脱液经氮气吹干后在正己烷溶剂中进行衍生化，衍生化试剂采用七氟丁酰咪唑。GC-MS采用选择离子监测（SIM）模式进行定性定量分析。结果表明，本方法的添加回收率为95．0％－101．0％；相对标准偏差为3．2％～4．8％；检出限达到0．010mg／kg。本方法步骤简单，溶剂用量少，定性定量准确可靠。可快速测定酱油等调味品中3－氯－1，2-丙二醇的含量。     

固氮蓝藻分离富集石墨炉原子吸收光谱法测定痕量Cr（Ⅵ）／Cr（Ⅲ）

本文选取固氮蓝藻分离富集Ｃｒ（Ⅵ）／Ｃｒ（Ⅲ），用墨炉原子吸收光谱法测定。结果表明该方法对１０ｍＬ试样，测定Ｃｒ（Ⅵ）的检测限为０．１μｇ．Ｌ＾－１＇变异系数为３．２％，在０－４５μｇ．Ｌ＾－１范围内线性关系好；测定Ｃｒ（Ⅲ）的检测限为０．３μｇ．Ｌ＾－１、变异系数３．７％，在０－４０μｇ．Ｌ＾－１范围内线性关系好。方法选择性高、富集率高。测定矿泉水、海水及自来水中的铬，获得满意结果。     

Reduction of matrix effects and improvement of sensitivity during determination of two chloridazon degradation products in aqueous matrices by using UPLC-ESI-MS/MS

The development and validation of a sensitive and reliable detection method for the determination of two polar degradation products, desphenyl-chloridazon (DPC) and methyl-desphenyl-chloridazon (MDPC) in surface water, ground water and drinking water is presented. The method is based on direct large volume injection ultra-performance liquid chromatography electrospray tandem mass spectrometry. This simple but powerful analytical method for polar substances in the aquatic environment is usually hampered by varying matrix effects, depending on the nature of different water bodies. For the two examined degradation products, the matrix effects are particularly strong compared with other polar degradation products of pesticides. Therefore, matrix effects were studied thoroughly with the aim of minimising them and improving sensitivity during determination by postcolumn addition of ammonia solution as a modifier. An internal standard was used in order to compensate for remaining matrix effects. The calibration curve shows very good coefficients of correlation (0.9994 for DPC and 0.9999 for MDPC). Intraday precision values were lower than 5 % for DPC, 3 % for MDPC and the limits of detection were 10 ng/L for both substances. The method was successfully used in a national round robin test with a deviation between 3 and 8 % from target values. Finally, about 1,000 samples from different water bodies have been examined with this method in the Rhine and Ruhr region of North-Rhine-Westphalia (Germany) and in the European Union. Approximately 76 % of analysed samples contained measurable amounts of DPC at concentrations up to 8 μg/L while 53 % of the samples showed MDPC concentrations up to 2.3 μg/L.     

Determination of Sex Hormones in Antler Velvet by High Performance Liquid Chromatography Tandem Mass Spectrometry

Eighteen sex hormones in antler velvet were determined by high performance liquid chromatography tandem mass spectrometry.The solid phase extraction was applied to eliminating the matrix effect.The exp...     

ICP-MS 法测定高纯氧化铕中稀土杂质的研究

深入考察了ＩＣＰ－ＭＳ法测定高纯氧化铕时基体对稀土杂质测定的影响,研究了Ｐ５０７萃淋树脂分离大量基体Ｅｕ２Ｏ３的实验条件,建立了采用内标补偿直接测定大部分稀土杂质和经Ｐ５０７萃淋树脂分离基体后测定被干扰离子Ｔｍ相结合的高纯Ｅｕ２Ｏ３中稀土杂质的ＩＣＰ－ＭＳ分析方法。方法检出限为０．００５～０．０２１μｇ／Ｌ,加标回收率为８４％～１１２％。ＲＳＤ为１．４％～８．１％。本法适用于质量分数为９９．９９％～９９．９９９９％的高纯Ｅｕ２Ｏ３中稀土杂质的分析。     

ICP-AES法测定钛基钎料中的铍和钙

介绍了应用电感耦合等离子体发射光谱技术（ICP-AES），测定钛基钎料中Be和Ca的方法。研究了钛基钎料中基体及主量元素对铍和钙光谱干扰、基体效应情况，选定了铍和钙元素的分析线，研究了仪器工作参数对测量的影响。优化仪器工作条件，标准加入回收率为98％-102％，相对标准偏差〈3％，试验结果表明，方法可以满足钛基钎料的测定要求。     

Fully automated standard addition method for the quantification of 29 polar pesticide metabolites in different water bodies using LC-MS/MS

A reliable quantification by LC-ESI-MS/MS as the most suitable analytical method for polar substances in the aquatic environment is usually hampered by matrix effects from co-eluting compounds, which are unavoidably present in environmental samples. The standard addition method (SAM) is the most appropriate method to compensate matrix effects. However, when performed manually, this method is too labour- and time-intensive for routine analysis. In the present work, a fully automated SAM using a multi-purpose sample manager “Open Architecture UPLC®-MS/MS” (ultra-performance liquid chromatography tandem mass spectrometry) was developed for the sensitive and reliable determination of 29 polar pesticide metabolites in environmental samples. A four-point SAM was conducted parallel to direct-injection UPLC-ESI-MS/MS determination that was followed by a work flow to calculate the analyte concentrations including monitoring of required quality criteria. Several parameters regarding the SAM, chromatography and mass spectrometry conditions were optimised in order to obtain a fast as well as reliable analytical method. The matrix effects were examined by comparison of the SAM with an external calibration method. The accuracy of the SAM was investigated by recovery tests in samples of different catchment areas. The method detection limit was estimated to be between 1 and 10 ng/L for all metabolites by direct injection of a 10-μL sample. The relative standard deviation values were between 2 and 10 % at the end of calibration range (30 ng/L). About 200 samples from different water bodies were examined with this method in the Rhine and Ruhr region of North Rhine-Westphalia (Germany). Approximately 94 % of the analysed samples contained measurable amounts of metabolites. For most metabolites, low concentrations ≤0.10 μg/L were determined. Only for three metabolites were the concentrations in ground water significantly higher (up to 20 μg/L). In none of the examined drinking water samples were the health-related indication values (between 1 and 3 μg/L) for non-relevant metabolites exceeded.     

Determination of fat in leather by the use of supercritical fluid extraction combined with on-line piezoelectric detection.

Leather samples were prepared and characterized as 'in house' matrix standards for the determination of fat. The Soxhlet standard method was used to establish the reference fat content in every standard sample. Sample homogeneity and stability were examined under specific storing conditions. The materials were subsequently used as matrix standards for the determination of fat in leather samples, using supercritical fluid extraction (SFE) with on-line piezoelectric detection. Real samples were weighed in the extraction SFE thimble, previously loaded with 1 g of diatomaceous earth. A temperature of 45 degrees C and a CO2 fluid density of 0.85 g ml-1 were used for extraction. The linear calibration range thus achieved was 0.001-0.040% m/m total fat (related to the weight of the leather) and the relative standard deviation +/- 3% (n = 11; P = 0.05). The results were compared with those obtained with the Soxhlet method and no significant differences were found.     

电感耦合等离子体发射光谱(ICP-OES)法测定含稀土磷矿中钛

为了准确测定含稀土磷矿石中钛的含量,采用两种溶样方法对磷矿进行处理,用电感耦合等离子体发射光谱(ICP-OES)法对磷矿中钛进行测定。实验表明,不进行基体匹配的标准曲线法不适合磷矿中钛的分析,采用基体匹配的标准曲线法时又难以制得与其各组分含量相似的校准溶液。用能有效消除样品本身基体干扰的标准加入法进行测定,分析结果的相对标准偏差小于2.0%,碱熔法的加标回收率为98.48%,酸溶法的加标回收率为104.4%,检测结果可靠,适合于磷矿中钛的分析。     

电感耦合等离子体发射光谱法测定锌铝镁合金中铝、镁含量

采用基体匹配法绘制校准曲线和镧元素作内标校正来消除基体效应和仪器漂移的影响, 建立了电感耦合等离子体发射光谱仪测定锌铝镁合金中铝、镁元素的分析方法. 将方法应用于锌铝镁合金试样的测定, 结果的相对标准偏差(RSD)在0.86%~2.13%之间, 加标回收率为96.4%~99.6%. 并与化学分析方法进行了比对, 两种方法测定值吻合较好.     

ICP-OES法测定镍铬合金中Si，Mn，Fe，Ti，Al，Cu多种元素

建立了电感耦合等离子体发射光谱法测定镍铬合金中Si,Mn,Fe,Ti,Al,Cu元素含量的分析方法。确定了溶样方法和分析谱线,采用基体匹配消除干扰。对方法精密度和准确度进行实验,实验结果表明,各元素的相对标准偏差均小于3%,加标回收率在86.8%～106.9%,镍铬合金标准物质的各元素测定结果均与标准值一致。所建立的方法快速、准确,适用于镍铬合金中多元素同时测定。     

石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙

以甘露醇为基体改进剂,建立石墨炉原子吸收光谱法测定压水反应堆硼酸介质中钙含量的方法。考察基体改进剂用量、灰化温度、原子化温度、基体干扰以及共存离子干扰对测定结果的影响,确定最佳测定条件:以硼含量为1000 mg/kg的硼酸为背景基体,加入适量甘露醇,样品作酸化处理,灰化温度为1700℃,原子化温度为2450℃。钙含量在8~32 μg/kg范围内与光谱强度成良好的线性关系,相关系数为0.9996,方法检出限为1.79 μg/kg。对于硼基体含量为0~2500 mg/kg的样品,测定结果的相对标准偏差为0.5%~7.5%(n=6),相对误差不大于13.2%,加标回收率为93.9%~113.3%。该方法检测速度快,结果准确,能满足实际生产要求。