Interlaboratory comparisons between results from testing metallurgical products for precious metal content

Problems verifying the accuracy of analyses of non-standardized materials for precious metal (PM) content have arisen at the Norilsky Nickel plant, which is a major producer of nickel, copper, and PMs in Russia. Because of the unavailability of certified reference samples for direct accuracy verification, a program of interlaboratory comparisons (ILC) was developed. This program was based on testing three semi-products of the PM production process for PM content. On program completion, a total of 826 results in 98 runs had been obtained. For each run, the calculated mean value of PM concentration was taken to be the reference value. The results obtained by Norilsky Nickel were in agreement with the reference values within the standard deviations calculated for the values. The quality of results yielded with the ILC program, as assessed via the Z-criterion, is regarded as satisfactory.Presented at the Second International Conference on Metrology – Trends and Applications in Calibration and Testing Laboratories, November 4–6, 2003, Eilat, Israel.     

Structure of the Polymer Obtained from Bisphenol-A and Cl 2 P(O)CH 3

Using the step-by-step build-up approach, the possible conformations of compound PhOP(O)(Me)OPh(Me) 2 Ph were constructed and geometrically optimized. Among the obtained structures 32 conformations belonging to low, comparable energy levels were used to construct the most stable dimers and tetramers of the title polymer. The results allowed us to estimate the geometrical structure of the polymer.     

Darstellung,Kristallstruktur und Normalkoordinatenanalyse der bindungsisomeren Pentachlororhodanoosmate(IV)

Preparation, Crystal Structure and Normal Coordinate Analysis of Linkage Isomeric Pentachlororhodanoosmates(IV) By treatment of [OsCl₅I]^2? with (SCN)₂ in dichloromethane the linkage isomers [OsCl₅(NCS)]^2? and [OsCl₅(SCN)]^2? are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The X-ray structure determination on single crystals of (Ph₄As)₂[OsCl₅(NCS)] (monoclinic, space group P2₁/a, a = 18.872(2), b = 11.6024(2), c = 22.786(1), β = 109.057(1)°, Z = 4) and (Ph₄As)₂[OsCl₅(SCN)] (monoclinic, space group P2₁/a, a = 19.057(2), b = 11.306(2), c = 22.612(1), β = 106.64(2)°, Z = 4) reveals the complete ordering of the complex anions. The thiocyanate group is located above one of the Cl ligands of the equatorial plane with the Os? N? C angle of 166.1° for N bonding and the Os? S? C angle of 109.9° for S bonding. The IR and Raman spectra of both linkage isomers known from literature are assigned by normal coordinate analysis based on the general valence force field using the molecular parameters of the X-ray determination. The valence force constants are f_d(OsN) = 1,81 and f_d(OsS) = 1,32 mdyn/Å. Taking into account increments of the trans influence a good adjustment between observed and calculated frequencies is achieved.     

The effect of capillary column diameter on the performance of thermal conductivity detectors

The concentration sensitivity of a thermal conductivity detector (TCD) depends, among other factors, on the amount of sample mixture in the detector's sensing cell. Since the cell volume has to be appropriately matched with column diameter, it makes the concentration sensitivity of a TCD dependent on column diameter and, therefore, on the speed of gas chromatography. Through reduction of column diameter, higher speed tends to lead to a reduction in the concentration sensitivity of the cell. The factor which the most directly affects the concentration sensitivity of a TCD cell is the heat power conducted through the cell. The higher the power, the greater the sensitivity. The limit of detection of a TCD depends on the concentration-sensitivity of its cell and on the level of statistical errors in the measurement. The errors increase with increasing analysis speed. As the column diameter is reduced, the errors cause additional worsening (on top of the decrease in concentration sensitivity) of the detection limit, dynamic range, and other performance characteristics of the TCD.     

加味异功散对脾虚小白鼠全血Zn、Fe的影响

探讨加味异功能健脾补血的生化机理、对脾虚治疗组、脾虚组和对照组小白鼠全血Zn、Fe含量进行动态观测。结果显示，加味异功散明显提高脾虚治疗组小鼠全血Zn、Fe含量。     

微量元素与妊娠及围产医学的关系

为探讨微量元素与妊娠及围产医学的关系，取４９例正常孕产妇和５１例异常孕产妇的头发进行微量元素检测．结果表明，异常孕产妇中妊娠高血压综合征组发锌均值（１０４±１７．５４）×１０－６明显低于正常组（１６８±２２．１２）×１０－６，而发铜均值（１３．３±０．７８）×１０－６明显高于正常组（１１．３±０．９４）×１０－６，不明原因流产组发锌（１１５±１０．３２）×１０－６，发铜（９．０３±１．０３）×１０－６两项均值明显低于正常组，羊膜早破组仅发铜均值（７．５９±１．９７）×１０－６低于正常组；畸胎组则锌、铜、铁、钙均值都低于正常组．经统计学处理均有显著性差异（Ｐ＜０．０５或产＜０．０１）     

原子吸收法在有机分析中的应用（Ⅴ）─甘草及其制品中甘草酸分析法的研究

原子吸收法在有机分析中的应用（Ⅴ）─甘草及其制品中甘草酸分析法的研究郎惠云，谢志海，赵怡（西北大学化学系西安，７１００６９）关键词原子吸收法，有机分析，甘草酸现代医药研究证明，甘草草药理作用的活性成分为甘草甜素或甘草酸，其定量测定方法国内外虽有报导￣...     

Synthese et Etude Structurale D'acides Alkylphosphoniques a Longue Chaine Hydrocarbonee

Long-chain dialkyl alkylphosphonates were synthesized by radical addition of dialkyl hydrogenphosphonates onto alkenes in presence of di(t-butyl) peroxide. This synthetic route leads to high yields between 94 and 97%. We performed chemical modifications of these phosphonates in order to obtain acidic derivatives. The structure of these compounds was characterized by NMR analyses and mass spectroscopy. We also studied their thermal behaviour and various crystalline phases were put in evidence by differential scanning calorimetry and optical microscopy. The thermal stability of these compounds was compared by thermogravimetric analyses.     

In-house validation for analytical methods and quality control for risk evaluation of chlordecone in food

Chlordecone was used until 1993 as a pesticide in the banana plantation of Martinique and Guadeloupe (French Antilles) against the root borer. This organochlorine pesticide was lipophilic, remnant, and toxic for human beings with both acute and chronic effects. Chlordecone was strongly absorbed and stored in soil and weakly decomposed in environment. Surveys conducted in 2001 revealed its presence in soil, rivers, and domestic food products. Local food (fruits and vegetables, cattle, poultry, and fish) was growing on soils, widely contaminated by chlordecone, used in the past as banana plantations. In 2003, French Administration asked for a risk evaluation for the Antilles population. The French Agency for Food Safety, proposed a Provisional Tolerable Daily Intake of 0.0005?mg?kg^?1?b.w.?day^?1, and an Acute Reference Dose of 0.01?mg?kg^?1?b.w.?day^?1, based on a toxicological risk assessment. The French National Reference Laboratory for pesticides has carried out two analytical methods, one for food of animal origin and another for food of fruit and vegetable origin. These methods were validated in the reference laboratory and dispatched to 13 laboratories for a proficiency test before the launch of two studies on Martinique and Guadeloupe food. About 900 samples from Martinique were sent to the network of laboratories for analysis of chlordecone. Performance parameters obtained through the proficiency test were briefly reported. The quality control test proposed in this study was discussed to shed light on the true variability achievable by intra-laboratory and inter-laboratory analysis. The limits of conventional quality-control procedures were discussed, and a process was proposed in order to get better confidence in analytical results.