An optimized gas chromatographic determination of priority pollutant phenols

Priority pollutant phenols are determined by gas chromatography on an SE-30 WCOT column using hydrogen carrier and flame ionization detection with dual internal standards. Linear responses over ranges ca. 12–125 ng per component are achieved and detection limits at or below 1 ng are obtained. Carrier flow and temperature program are optimized to maintain baseline resolution while affording an analysis time of less than 15 minutes.     

Powdered activated carbons as effective phases for bar adsorptive micro-extraction (BAμE) to monitor levels of triazinic herbicides in environmental water matrices

Bar adsorptive micro-extraction using three powdered activated carbons (ACs) as adsorbent phases followed by liquid desorption and high performance liquid chromatography with diode array detection (BAμE(ACs)-LD/HPLC-DAD), was developed to monitor triazinic herbicides (atrazine, simazine and terbutylazine) in environmental water matrices. ACs used present apparent surface areas around 1000 m² g⁻¹ with an important mesoporous volume and distinct surface chemistry characteristics (pH_PZC ranging from 6.5 to 10.4). The textural and surface chemistry properties of the ACs adsorbent phases were correlated with the analytical data for a better understanding of the overall enrichment process. Assays performed on 10 mL water samples spiked at the 10.0 μg L⁻¹ levels under optimized experimental conditions yielded recoveries around 100% for the three herbicides under study. The analytical performance showed good precision (RSD < 15.0%), convenient detection limits (≈0.1 μg L⁻¹) and suitable linearity (1.0-12.0 μg L⁻¹) with good correlation coefficients (r² > 0.9914). By using the standard addition method, the application of the present method on real water matrices, such as surface water and wastewater, allowed very good performances at the trace level. The proposed methodology proved to be a suitable sorptive extraction alternative for the analysis of priority pollutants with polar characteristics, showing to be easy to implement, reliable, sensitive and requiring a low sample volume to monitor triazinic compounds in water matrices.     

粘度国家基准装置测量结果的不确定度

分析粘度国家基准装置测量结果不确定度的来源并进行评定。影响粘度国家基准装置测量不确定度的主要因素有温度、时间、表面张力、空气浮力以及动能修正等。根据2002年粘度国家基准量值复测的结果，以及改造后新基准装置和辅助设备的状态，计算得粘度国家基准装测量结果的扩展不确定度为0.038%-0.4%。     

Application of Internal Standard for Micro Extraction– Spectrophotometric Determination of Bismuth in Pharmaceutical Formulations

 A micro extraction – spectrophotometric procedure is developed for the determination of bismuth in pharmaceutical formulations. The procedure is based on the extraction of tetraiodobismuthate(III) ion paired with benzyltributylammonium cation into chloroform. The application of Nile Blue as internal standard (IS) enabled good analytical performance for micro-scale analysis. The ratio between the absorbances measured at 491 nm (bismuth complex) and at 632 nm (IS) was taken as the analytical signal. The procedure was carried out in Eppendorf tubes, lowering significantly the use of reagents and the volume of organic solvent. In the calibration range up to 60 mgċl⁻¹, the linear regression coefficient was 0.9999, the CV for 15 mgċl⁻¹ and for 50 mgċl⁻¹ Bi were 1.6% and 0.7% respectively. The results obtained in the analysis of pharmaceutical formulations were in good agreement with the results of EDTA titration method. Received November 25, 1999. Revision February 14, 2000.     

A specific standard for quality in fundamental research

 The specific standard described here constitutes the heart of the quality system set up by the Commissariat à l'Energie Atomique – French Atomic Energy Commission – for its main "Fundamental Research" entity, the Directorate for the Sciences of Matter. It is a coherent standard (set of shared rules and provisions laid out in a clear fashion) designed, in the first instance, to provide those taking part in research, including the hierarchy, with the means to satisfy their requirements in the field of quality. And, secondly, to create the conditions for recognition of this action by third parties, which all research entities must nowadays convince of their trustworthiness (supervisory ministries, research partners, industrial companies, etc.). This standard places particular emphasis on the preponderant roles of initiative and freedom in fundamental research, which are a prerequisite for creativity, innovation and, last but not least, the motivation of personnel.     

ICP-AES内标法测定分子筛的组成

首次通过ICP-AES仪研究了分子筛化学组成全分析的方法，采用HNO3-HF混合酸密闭溶样，用H3BO3配合F^-，分别采用内标法和基体消除法消除基体效应．将研究结果与经典方法比较表明：采用本文研究的分析方法，结果准确可靠，符合分析要求，尤其对杂原子分子筛以及金属氧化物修饰的分子筛的组成分析具有应用价值．     

Modular Breath Analyzer (MBA): Introduction of a Breath Analyzer Platform Based on an Innovative and Unique,Modular eNose Concept for Breath Diagnostics and Utilization of Calibration Transfer Methods in Breath Analysis Studies

Exhaled breath analysis for early disease detection may provide a convenient method for painless and non-invasive diagnosis. In this work, a novel, compact and easy-to-use breath analyzer platform with a modular sensing chamber and direct breath sampling unit is presented. The developed analyzer system comprises a compact, low volume, temperature-controlled sensing chamber in three modules that can host any type of resistive gas sensor arrays. Furthermore, in this study three modular breath analyzers are explicitly tested for reproducibility in a real-life breath analysis experiment with several calibration transfer (CT) techniques using transfer samples from the experiment. The experiment consists of classifying breath samples from 15 subjects before and after eating a specific meal using three instruments. We investigate the possibility to transfer calibration models across instruments using transfer samples from the experiment under study, since representative samples of human breath at some conditions are difficult to simulate in a laboratory. For example, exhaled breath from subjects suffering from a disease for which the biomarkers are mostly unknown. Results show that many transfer samples of all the classes under study (in our case meal/no meal) are needed, although some CT methods present reasonably good results with only one class.     

气相色谱法测定广藿香油中百秋李醇含量

建立了气相色谱仪测定广藿香油中百秋李醇含量的方法。用毛细管色谱柱DB-5MS（30m×O．32mm．0．25μm）,正十八烷为内标,氢火焰离子化检测器进行检测,内标法定量。百秋李醇含量在0．2-2．0mg／mL范围内,百秋李醇峰面积和内标物峰面积之比与百秋李醇质量浓度呈良好的线性关系,相关系数r=0．9997。方法的检出限为1μg／mL,加标回收率为90．0％～100．6％,测定结果的相对标准偏差为1．22％（n=6）。研究表明,本法简便、快速、测定结果准确可靠,精密度优于外标法。     

The solubilization of alcohols in micellar solutions

The specific conductivities of dodecyldimethylbenzylammonium bromide (C12BBr) have been determined in aqueous butanol and aqueous benzyl alcohol solutions in the temperature range of 5-40°C. From these data the temperature dependent critical micelle concentration (cmc) was determined. The molar fraction of alcohol in the micelle was estimated using the theory suggested by Motomura et al. for surfactant binary mixtures. The thermal properties such as standard Gibbs free energy, enthalpy and entropy of solubilization of alcohols in the micelles were estimated for the phase separation model. The change in heat capacity upon solubilization of alcohol in the micelle has been estimated form the above properties. This revised version was published online in July 2006 with corrections to the Cover Date.