苯和甲苯差分吸收光谱方法的实验室测量研究

本文介绍了差分光学吸收光谱法(DOAS)测量大气污染气体浓度的基本原理。DOAS方法就是利用氙灯发出的紫外—可见光，经望远镜准直后再经过一段距离的传输，由望远镜来接收．在传输中，由于各种不同的分子在不同的波段对光有不同的吸收特征，使光谱具有了污染物的特征，再通过与光源发出的光进行比较，反演这些气体在大气中浓度．我们将DOAS方法应用在监测有机物上，在分析光谱的过程中，应用多项式拟合和最小二乘法，从而精确地从测量光谱中来反演出大气中污染气体的浓度．文中用DOAS方法测量了苯和甲苯的样品，并分析了结果，结果和理论吻合．可为环境中有机污染物监测提供可靠的方法。     

Monitoring of CdTe atomic layer epitaxy using in-situ spectroscopic ellipsometry

Atomic layer epitaxy or ALE has proven to be useful for the growth of epitaxial layers of high uniformity, good quality, and well-controlled thickness. In this study, we have carried out in-situ monitoring during the atmospheric pressure ALE of CdTe on GaAs (100) substrates using spectroscopic ellipsometry (SE). The susceptor temperature, reactant partial pressures, as well as the flow and flush duration for each precursor are crucial process variables for ALE growth. Growth was carried out for 20–25 cycles under different sets of these process conditions during the experiment and in-situ SE was used to verify the presence of layer-by-layer growth, which enabled the quick determination of the process window. We observed ALE growth of CdTe at 300°C, supporting the explanation that the growth of CdTe occurs via a surface catalyzed decomposition of the Te precursor di-isopropyltelluride (DIPTe). Investigation of ALE mode growth behavior for different susceptor temperatures and DIPTe flush times indicated that the growth was limited by competition between desorption and reaction of the adsorbed DIPTe species on the Cd terminated surface.     

森林火情监测预报研究

对现行的森林火情监测方法进行了分析比较。根据实际存在的难题，提出了料为产用的实施方案及应采取的技术措施，进行了实地试验，取得较好的效果。     

In‐line monitoring of UV photopolymerization with a quartz crystal resonator

An in‐line monitoring device using a quartz crystal resonator for thin film polymerization was proposed, and its performance has been evaluated by implementing in the UV polymerization of 2‐hydroxyethyl methacrylate with a photoinitiator of 1‐chloroanthraquinone. Because the variation of resonant resistance of the resonator is proportional to the square root of viscosity change that is closely related to the polymerization degree, the resistance can be used as a measure of the polymerization degree. The resistance measurements were compared with the outcome of instrumental analyses of polymerization degree using an FTIR spectrometer and a gel permeation chromatograph. The experimental results showed that the resistance measurements were consistent with the experimental outcome of the instrumental analyses, and this indicates the effectiveness of the proposed device. Owing to the simplicity and availability of the resonator system, its wide utilization in the monitoring of a variety of film polymerization processes, including photoresistor application, is expected. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 2428–2439, 2006     

Modeling of in situ monitored laser reflectance during MOCVD growth of HgCdTe

An effective way to in situ monitor the metalorganic chemical vapor deposition (MOCVD) of HgCdTe/CdTe/ZnTe on GaAs or GaAs/Si substrates is presented. Specular He-Ne laser reflectance was used to in situ monitor the growth rates, layer thickness, and morphology for each layer in the grown multilayer structure. In situ monitoring has enabled precise measurements of ZnTe nucleation and CdTe buffer layer thicknesses. Monitoring the constancy of reflectance during the thicker CdTe buffer growth where absorption in the CdTe reduces reflectance to just the surface component has led to optimum buffer growth ensuring good quality of subsequently grown HgCdTe. During the interdiffused multilayer process (IMP) HgCdTe growth, because multiple interfaces are present within the absorption length, a periodic reflectance signal is maintained throughout this growth cycle. A theoretical model was developed to extract IMP layer thicknesses from in situ recorded experimental data. For structures that required the growth of a larger band gap HgCdTe cap layer on top of a smaller band gap active layer, in situ monitored reflectance data allowed determination of alloy composition in the cap layer as well. Continuous monitoring of IMP parameters established the stability of growth conditions, translating into depth uniformity of the grown material, and allowed diagnosis of growth rate instabilities in terms of changes in the HgTe and CdTe parts of the IMP cycle. A unique advantage of in situ laser monitoring is the opportunity to perform “interactive” crystal growth, a development that is a key to real time MOCVD HgCdTe feedback growth control.     

用碘酸钾滴定法标定二氧化硫标准溶液

用KIO3滴定法标定SO2标准溶液,RSD≈0.10%,标定结果与标准法结果无显著性差异,相对误差<±0.3%。     

Hydrogen Oxidation on a Platinum Microelectrode: Effect of Carbon Monoxide Impurities

The kinetics of the hydrogen oxidation and the CO adsorption on a Pt (ultra)microelectrode is studied in a 0.5 M H₂SO₄ solution saturated with a mixture of gaseous H₂ and CO at partial CO pressures p _CO = 10–500 ppm. The balance between rates of diffusion and adsorption of CO at different adsorption times is studied. Studied is the effect of CO impurities in H₂ on steady-state polarization curves for the hydrogen ionization and nonsteady-state curves of the oxidation current decay with time at 0.02–0.05 V. Conditions under which in a certain time interval and at a certain CO concentration the slope of an I vs. t curve is proportional to p _CO are determined. The obtained dependence may be used when designing a technique for monitoring CO impurities in technical hydrogen.     

Identification of a chemical indicator of the rupture of 1,4-β-glycosidic bonds of cellulose in an oil-impregnated insulating paper system

In this study, headspace gas chromatography/mass spectrometry has been used to assess the volatile by-products generated by the ageing of oil-impregnated paper insulation of power transformers. Sealed-glass ampoules were used to age under oxidative conditions 0.5-g specimens of insulating paper in 9 mL of inhibited mineral oil in a temperature range of 60–120 °C and moisture of 0.5, 1 and 2% (w/w). A linear relationship between one of the oil-soluble degradation by-products, i.e. methanol, and the number of ruptured 1,4-β-glycosidic bonds of cellulose, regardless of the type of paper (ordinary Kraft or thermally-upgraded (TU) Kraft paper), was established for the first time in this field. Ageing at 130 °C of model compounds of the Kraft paper constituents (α-cellulose, hemicellulose and lignin) and two cellulosic breakdown by-products (D-(+)-glucose and 1,6-anhydro-β-d-glucopyranose) confirmed that the α-cellulose degradation was mostly responsible for the presence of this molecule in the system. Furthermore, additional 130 °C-tests with six different papers and pressboard samples under a tight control of initial moisture indicated that at least one molecule of methanol is formed for each rupture of 1,4-β-glucosidic bond of the molecular chains. Stability tests showed that the ageing indicator is stable under the oxygen and temperature conditions of open-breathing transformers. The presence of methanol was detected in 94% of oil samples collected from over than 900 in-service pieces of equipment, confirming the potential for this application. Lastly, the tests have shown that oil-oxidation by-products and TU-nitrogenous agents modify the methanol partitioning coefficients in the paper/oil/air system, which makes their study essential over a range of field conditions encountered by power transformers. Results are presented and discussed in comparison with 2-furfuraldehyde, which is the current reference in the domain.     

GC-MS法测定焦化厂气溶胶中多环芳烃

利用气相色谱-质谱(GC-MS),电子轰击离子化(EI)法测定焦化厂气溶胶中多环芳烃的含量。超声波抽提气溶胶样品,用GC-MS的选择离子监测(SIM)方式测定EPA提出的优先监测的16种多环芳烃的含量。该法的检出限为0.167pg·m~(-3),PAHs的回收率为85.1％～110.5％,相对标准偏差为4.62％～19.4％。应用该法测定气溶胶中PAHs获得满意的结果。     

Chemometric interpretation of pesticide occurence in soil samples from an intensive horticulture area in north Portugal

An extensive monitoring programme of pesticides was carried out in soil samples from an intensive horticulture area in north of Portugal, putting into practice the needs for increased control of soil quality as far as organic pollution is concerned. The area under investigation was additionally defined as vulnerable to nitrates due to local soil and aquifer characteristics, which might be extended to pesticides contamination. Five sampling sites were selected and soils analysed at three depths in eight sampling campaigns, for the period of 2 years. A stepwise multivariate statistical approach was selected to uncover most relevant patterns inside a complex environmental data matrix. Cluster analysis was applied both to group pesticides and samples, giving a primary and unsupervised overlook of privileged relationships. Clusters of persistent pesticides and selected herbicides were identified, whereas sample classes were also formed and disposed geographically. Thirty eight percent of analysed soils samples fell into one class characterized by low contamination (class 1 in cluster analysis), which is entirely representative of the sampling site no. 1. Afterwards, linear discriminant analysis was applied to identify those pesticides, which had a higher impact in the definition of classes. Finally, factor analysis using a five component model was implemented in order to bring to light the constitution and data variance explained by each of the five main principal components, as well as, their relation to pest management practices. A factor was identified (PC1 – 22% variance) composed of chlorinated pesticides, which was representative of one of the investigated sites indicating its high contamination status. Qualitative main findings and class average concentration values were obtained through this multivariate statistical approach.