Analysis of organic acids in wines by Fourier-transform infrared spectroscopy

Fourier-transform infrared (FTIR) spectroscopy has been a major point of development in many wine laboratories in recent years. It enables almost instant analysis of several properties of wine, usually with very good precision and accurate results. Nevertheless, validation procedures should not be forgotten and should be fully performed. Recovery experiments were performed by spiking wine samples with different amounts of organic acids (tartaric, malic, lactic, acetic and citric—the most prominent in wines). After FTIR analysis of the total acidity and of each organic acid concentration, recoveries were calculated. For total acidity recovery results were, in general, good and very close to 100% (64–111%). On the other hand, for individual organic acid concentrations, the recovery results were lower than 100% (11–73%) for all spiking additions. These results could be explained by spectroscopic interferences between the organic acids. Because they have similar infrared spectra, it is not easy to distinguish between them and, therefore, to achieve accurate calibration. When total acidity, with a different infrared spectrum from the other abundant compounds in the wine, was taken as a single property the recovery results were acceptable.     

Analysis of Seven Herbicides by Gas-Liquid Chromatography

Simutaneous analysis of seven commonly used herbicides, 2,4-D methyl ester, 2,4-D methyl ester, 2,4,5-T methyl ester, silvex methyl ester, ramrod, CIPC and DEF, by gas-liquid chromatography with an electron capture detector was attempted. Two packed columns (which are generally used for the analysis of chlorinated pesticides) and two chemically bonded fused silica capillary columns were used for the analysis. When the packed columns were used, ramrod always interfered with the analysis of 2,4-D methyl ester and/or silvex methyl ester. Complete separation with reasonable analysis time can be achieved using one of the chemically bonded fused silica capillary columns.     

BCEIA 2001学术报告会论文作者调查研究

对BCEIA2001学术报告会论文作者问卷调查资料进行统计分析，我国从事分析测试科研活动的人员以青年人为主，且具有高学历、高职称的特点；分析测试领域的科研活动主要集中在北京、湖北、辽宁、广东、上海等省市；分析测试领域的研究主要涉及分析测试物质的成份、结构以及提高分析测试质量；当前分析测试领域的研究热点在化学／化工、环保、生物技术、卫星／临床、制药等领域；分析测试领域研究工作的资金主要来源于各种基金的支持。     

A new adsorbent for trace level organic contaminants

Summary A preliminary study has been carried out to evaluate a new adsorbent, Thermosorb, for trace level organic contaminants. For this purpose, a comparison was made with a well-characterized adsorbent, Tenax GC, using a prepared aqueous solution of trace organic components. In addition, a comparison was made of chromatograms of air contaminants obtained using both of these adsorbents, under equivalent conditions. The results clearly indicated the potential of this thermally stable, inorganic adsorbent for many trace organic substances of environmental interest.     

Analytical techniques for cyanide in blood and published blood cyanide concentrations from healthy subjects and fire victims

Hydrogen cyanide can be produced by the pyrolysis of man-made polymers. Cyanide has been measured in the blood of healthy adults as well as the blood of fire survivors and fatalities. In healthy subjects the blood cyanide concentration of smokers is higher than that of non-smokers. Fire survivors and fatalities have been found to have higher cyanide levels than of control groups and the levels from fire fatalities are often higher than survivors. Blood concentrations quoted as normal, toxic or fatal are highly variable in the literature. Many studies have been performed to measure the blood cyanide levels in control subjects as well as those who have been exposed to fire but the values found differ. The values for control subjects can vary from none detected to 19 μmol dm⁻³ while those for fire survivors range from not detected to 150 μmol dm⁻³ and fatalities range from not detected to 284 μmol dm⁻³. Analytical techniques and published data are critically reviewed.Many of the existing antidotes for cyanide poisoning are highly toxic themselves and should ideally be administered at doses proportional to the amount of cyanide a patient has received to avoid compounding damage done by cyanide intoxication. For this reason, a rapid, accurate bedside assay of blood cyanide concentration that differentiates between bound and free cyanide would represent a leap forward in the clinical management of cyanide poisoning.     

Double pulse laser-induced breakdown spectroscopy of explosives: Initial study towards improved discrimination

Detecting trace explosive residues at standoff distances in real-time is a difficult problem. One method ideally suited for real-time standoff detection is laser-induced breakdown spectroscopy (LIBS). However, atmospheric oxygen and nitrogen contributes to the LIBS signal from the oxygen- and nitrogen-containing explosive compounds, complicating the discrimination of explosives from other organic materials. While bathing the sample in an inert gas will remove atmospheric oxygen and nitrogen interference, it cannot practically be applied for standoff LIBS. Alternatively, we have investigated the potential of double pulse LIBS to improve the discrimination of explosives by diminishing the contribution of atmospheric oxygen and nitrogen to the LIBS signal. These initial studies compare the close-contact (< 1 m) LIBS spectra of explosives using single pulse LIBS in argon with double pulse LIBS in atmosphere. We have demonstrated improved discrimination of an explosive and an organic interferent using double pulse LIBS to reduce the air entrained in the analytical plasma.     

Darstellung,Kristallstruktur und spektroskopische Eigenschaften der Clusteranionen [(Mo6Br)X]2− mit Xa = F,Cl, Br,I

Synthesis, Crystal Structure and Spectroscopic Properties of the Cluster Anions [(Mo₆Br )X ]^2? with X^a = F, Cl, Br, I The tetrabutylammonium (TBA), tetraphenylphosphonium (TPP) and tetraphenylarsonium (TPAs) salts of the octa-μ₃-bromo-hexahalogeno-octahedro-hexamolybdate(2?) anions [(Mo₆Br)X]^2? (X^a = F, Cl, Br, I) are synthesized from solutions of the free acids H₂[(Mo₆Br)X] · 8 H₂O with X^a = Cl, Br, I. The crystal structures show systematic stretchings in the Mo? Mo bond length and a slight compression of the Brⁱ₈ cube in the F^a to I^a series. The cations do not change much. The i.r. and Raman spectra show at 10 K almost constant frequencies of the (Mo₆Brⁱ₈) cluster vibrations, whereas all modes with X^a ligand contribution are characteristically shifted. The most important bands are assigned by polarization measurements and the force constants are derived from normal coordinate analysis. The ⁹⁵Mo nmr signals are shifted to lower field with increasing electronegativity of the X^a ligands. The fluorine compound shows a sharp ¹⁹F nmr singlet at ?184.5 ppm.     

Multivariate analysis of non-homogeneous peaks in liquid chromatography

Summary The effects of concentration, separation and spectral similarity as factors influencing the accuracy of iterative target testing factor analysis (ITT-FA) are investigated for three component systems by the application of analysis of variance (ANOVAR). ANOVAR is applied over a range of peak separations to map the changing effects of the three factors with increasing overlap. Two error responses were measured and analysed, (a) Relative cluster error (RCE) a measure of the error over all peaks in a cluster and (b) Relative peak error (RPE) the error of an individual peak. Multicomponent analysis (MCA) a method requiringa priori spectral information, is used as a referee method for ITT-FA.