叠层型串联ISE的电分析化学性能与Nernst倍增效应

设计了多元叠层型串联ISE,结构紧凑,组装简便,适用于微体积样液分析。对四元叠层型串联ISE的试验表明:与现行ISE比较,其线性响应斜率、测定精密度与灵敏度均增大4倍,但响应速度、选择性系数与检测下限不变。     

多元稀土薄膜的微量化学分析法(YSmLuCa)_3(FeGe)_5O_(12)原子比值

本法解决了薄膜取样问题,以及稀土与非稀土元素的分离和测定,从而确定了薄膜组份的原子比值。方法的准确度与精密度都达到要求,并可为非破坏性测定提供校对数据。本法也适用于其他类型的多元稀土薄膜的测定。     

多元稀土薄膜的微量化学分析法(YSmLuCa)3(FeGe)5O12原子比值

本法解决了薄膜取样问题,以及稀土与非稀土元素的分离和测定,从而确定了薄膜组份的原子比值。方法的准确度与精密度都达到要求,并可为非破坏性测定提供校对数据。本法也适用于其他类型的多元稀土薄膜的测定。     

流动注射-分光光度法测定水中氰化物

使用流动注射(FIA)-分光光度法测定水中的氰化物的含量,并与传统分光光度法的分析结果进行比对。实验证明流动注射(FIA)-分光光度法操作简便、线性好,灵敏度、精密度、准确度都能符合分析工作要求。检出限为0.2μg/L,适用于水中微量氰化物的检测。分析频率为每小时30个样品,特别适合大批样品的测定。     

应用二极管阵列串联荧光检测-高效液相色谱技术快速测定玩具材料中蒽油的4种成分

采用二极管阵列串联荧光检测-高效液相色谱法对玩具材料中蒽油的4种主要成分蒽、菲、芘、荧蒽进行了检测。样品用正己烷-丙酮溶液超声提取,硅胶小柱净化。方法的荧光检测线性范围为0.5～1000 μg/L,二极管阵列检测线性范围为0.5～1000 mg/L。加标回收、精密度试验表明4种成分的回收率为70.0%～120%,精密度为0.7%～8.8%。蒽、菲、芘、荧蒽的检出限分别为0.1、0.1、0.2、0.3 μg/L,定量限分别为0.4、0.2、0.5、0.8 μg/L。方法具有灵敏度高、检出限低的特点,适用于玩具材料中蒽油4种成分的快速定性、定量检测。     

热解析-裂解-气相色谱/质谱联用法测定电子电气产品中的多溴二苯醚

建立了热解析-裂解-气相色谱/质谱法测定电子电气中多溴二苯醚(PBDEs)的方法。采用气相色谱-质谱总离子流和选择离子流对PBDEs进行定性和定量测定。对热解析温度,热解析时间,热解析升温速率和附件初始温度进行了优化,并进行了线性关系、精密度等试验。本方法线性范围200~1000 mg/kg,相关系数为0.995,检出限为50 mg/kg,相对标准偏差小于15%。本方法可直接固体进样,简化了前处理步骤,适用于电子电气产品中PBDEs的测定,满足欧盟Ro HS指令限量的检测要求。     

气相色谱测定工作场所空气中二氟二氯甲烷

按照《工作场所有害物质监测方法》中的要求,提出了热解吸-气相色谱法测定工作场所空气中二氟二氯甲烷的方法,空气中的二氟二氯甲烷用活性碳吸附采样,随后在热解吸仪中使活性碳中的被测物质热解吸,并引入气相色谱中.以氢焰离子化检出器进行检测,二氟二氯甲烷浓度在0～2 000 mg·L-1之间呈线性,相关系数为0.998 7,方法的检出限为8.5×10-2 mg·L-1.在3种不同浓度水平(500,1 000,2 000 mg·L-1)进行方法的精密度试验,所得RSD值在2.0%～4.6%之间.根据试验数据算得每100 mg活性碳对二氟二氯甲烷的穿透容量为20 mg,对不同浓度的二氟二氯甲烷的热解吸效率均在90%以上,所提出的方法适用于工作场所空气中二氟二氯甲烷的现场监测.     

紫外可见分光光度法测定水中六价铬的线性范围

探讨紫外可见分光光度法测定水中六价铬的最佳线性范围。GB 7467–1987规定以二苯碳酰二肼为显色剂,用紫外可见分光光度法测定水中的六价铬,实践表明,在标准规定的浓度区间内,测量精密度和准确度不能达到标准要求。大量的实验数据表明此法测定水中六价铬的最佳线性范围为0.05～0.4μg/mL。     

热重量法分析石墨成分

研究了用热重分析仪进行石墨成分分析的方法，摸索了仪器的适宜分析条件，并对试验结果进行了讨论。针对仪器系统误差对挥发分测定的影响，采用一无线性回归对测量数据进行了校正。方法的精密度和准确度试验证明，用热重量法可有效地应用于日常检验工作。     

多道γ能谱仪应用于测定磷矿石中226Ra

应用GBT 2480多道γ能谱仪测定了磷矿石中226Ra的含量,对测定的工作奈件进行了试验并予以优化.用该仪器配备的谱测量软件MCA获得数据和谱分析软件Win Nal处理数据.试验结果表明,所获得的精密度和准确度数据符合国家标准规定的要求.     

A statistical evaluation of the Youden Matched-Pairs Procedure

AOAC INTERNATIONAL currently permits investigators to use the Youden Matched-Pairs Procedure to obtain estimates of the method performance indicators repeatability and reproducibility (S(r) and SR, respectively). This report explains the statistical model assumptions upon which the procedure is based, provides validity tests for several of these assumptions, explains conditions under which Youdens' "precision error" is not consistent with precision estimate S(r) or SR as defined by AOAC INTERNATIONAL, and indicates when precision estimates based on the procedure should be interpreted with caution or should not be used.     

水中氟化物国际标准检验方法的验证及其比较

介绍水中氟化物国际标准检验方法的验证结果,其中包括了干扰实验、标准曲线、准确度、精密度、检出限等.并将本方法测定结果与国标同类方法进行了比较.结果表明,该方法抗干扰性好,测量精度高,其标准曲线范围宽,点数设计合理,优于国标中的同类方法.应加以采纳和推广.     

Development,method validation and simultaneous quantification of eleven bioactive natural products from high-altitude medicinal plant by high-performance liquid chromatography

Herein, a novel, rapid, reliable, simple method validation and simultaneous quantification of 11 bioactive compounds (mostly xanthones) have been described. International Conference on Harmonization guidelines were used for the analytical method validation. Good linearity, repeatability, intra- and inter-day precision, accuracy and reliability were well-illuminated in the method validation procedure. The calibration curves showed a good linear relationship (r > 0.999) within test range. Precision was evaluated by intra- and inter-day tests with relative standard deviation <2.79% and accuracy validation recovery of 74.16%–91.84%. On quantification study, the validated method described the high content of bioactive xanthone derivatives, including 1-hydroxy-3, 5-dimethoxyxanthone ( 7 ), 2-(allyloxy)-8-hydroxy-1, 6-dimethoxyxanthone ( 6 ) 1, 7, 8-trihydroxy-3-methoxyxanthone ( 9 ) and Coxanthone E ( 5 ) in Codonopsis ovata, which is advantageous given the numerous pharmacological and biological effects associated with these compounds, which mostly exhibit anti-cancerous, antioxidant, anti-inflammatory, anti-mutagenic and anti-obesity effects. The bulk abundance of these compounds can also be used for further modification to produce better lead molecules for drug discovery with low toxicity and high potency. The proposed method makes it possible to simultaneously determine all bioactive compounds in one run and can be extended to marker-based standardization of herbal formulations in medicinal and pharmaceutical industries.     

Expert systems for method development and validation in HPLC

ESCA, Expert Systems Applied to Chemical Analysis, started its research in March 1987, with the aim of building prototype expert systems for HPLC method development. Results of this research have been published as the work has progressed. The project is now completed and this paper summarises some of the overall project conclusions. Seven different expert systems have been built which tackle problems throughout the process of method development, four stand-alone systems and three integrated systems. The object of ESCA was to evaluate the applicability of expert system technology to analytical chemistry and not all the systems were built for commercial uses. Many of the systems tackle problems specific to one or more of the partners and thus may not be useful outside this environment. However, the results of the work are still pertinent to analysts wishing to build their own systems. These results are described, however, the emphasis of the paper is on those systems developed for method validation.Method validation for HPLC is a complex task which requires many characteristics of the method to be tested, e.g. accuracy, precision, etc. The expert systems built within ESCA concern the validation of precision. Two systems were developed for repeatability testing and ruggedness testing. The method validation process can be divided into several discrete stages, these include: (1) The selection of the method feature to test, for instance which factors can influence the ruggedness of a method. (2) The definition of a test procedure, for instance an efficient statistical design. (3) The execution of experiments and the interpretation of results. (4) A diagnosis of any observed problem. This paper describes these two systems in some detail and summarises some of the results obtained from their evaluation. It concludes that expert systems can be useful in solving analytical problems and the integration of several expert systems can provide extremely powerful tools for the analyst.     

X射线荧光光谱法测定萤石中CaF2、CaCO3、S、Fe及SiO2

X射线荧光光谱法分析是目前快速分析方法之一,精密度受基体效应、均匀性、元素间干扰等影响。采用粉末压片法制备样品,用X射线荧光光谱法直接测定F、Ca元素,得出CaF_2及CaCO_3含量,并同时分析萤石中S、Fe、SiO_2的含量。精密度实验表明,待测元素的相对标准偏差均低于0.66%(RSD,n=10),能满足萤石中各元素的检测要求。     

Development and optimization of a stability indicating method on a monolithic reversed-phase column for Colchicum dry extract

This article presents a method developed on a monolithic reversed-phase column for separation of related alkaloids and degradation products from colchicine in dry extract preparations from Colchicum seeds. Optimization was performed using an optimization software with variation of the pH of the mobile phase and the percentage of organic modifier. This method permits for the first time a fast separation of all alkaloids including colchiceine without prior derivatization or complexation with excellent linearity, precision and low limits of quantitation which makes it a suitable method for stability testing of extracts or drug formulations containing extracts of Colchicum seeds.     

Direct Spectrographic Determination of In,La, Nb and Sr in Thorium Oxide

Abstract

A d.c. are emission spectrographic method is described for the determination of ppm levels of In, La, Nb and Sr in thorium oxide. The method permits determination of the above low and high volatile impurity elements in thoria using AgCl as carrier in an atmosphere of oxygen. The carrier-distillation technique reported makes possible the following range of estimations: In : 1–50 ppm; La, Nb : 10–500 ppm and Sr: 2–100 ppm. The method is simple and rapid and its precision ranges from 14% for In to 18% for Nb. Observations made on the choice of carrier and internal standard are presented.     

Performance of the elongation method with larger basis sets

The elongation method proposed by Imamura serves as a theoretical model for polymerization processes. It can now be used together with larger basis sets, Hartree–Fock and density functional methods from the Gaussian 94 package with direct self‐consistent field (SCF). This allows electronic structure calculation of elongating clusters with an efficiency superior to full cluster calculations and a precision superior to previous versions of our elongation method. Performance and accuracy compared with full cluster calculations on a regular polymer using the BLYP/6‐31G(d, p) method. Interaction energies of water and hydrogen fluoride polymers of increasing length are compared between HF, BLYP methods and 4‐31G, 6‐31G(d, p) basis sets: Diffuse and polarization functions have a large influence on the interaction energy on both polymers. Local density of states are calculated for different cluster lengths. They are in good agreement with full cluster calculations. ©1999 John Wiley & Sons, Inc. Int J Quant Chem 74: 35–47, 1999     

有机试剂的结构与性质研究(Ⅴ)——5-Br-PADAP的酸碱平衡及其在溶液中存在形式的研究

本文用分光光度法研究了2-[2-(5-溴-吡啶)偶氮]-5-二乙胺基酚(5-Br-PADAP)的酸碱平衡,实验测得的pH和A的数据,用最小二乘法处理得到了5-Br-PADAP在30％乙醇溶液中的离解常数:pK_a1=-0.12,PK_a2=1.66,pK_a3=12.30;并用HMO量子化学计算法确定了5-Br-PADAP在溶液中可能存在的各种形式.     

Über die anwendbarkeit der mikrotorsionswaage 1700 zur mikrogrammanalyse

The high precision of the Sartorius micro-balance 1700 with its load capacity of 2 g permits a weighing precision of ± 10 μg, which is the value of a half scale-division; by means of the classical “statistical weighing method”, an increased precision of ±1 μg is attainable. This accuracy is, in the investigated range, independent of the load up to 1.5 g.