离子色谱法同时测定水中六种阳离子

研究了用抑制电导离子色谱法一次进样同时测定水中Li^ ,Na^ , NH4^ ,Mg^2 ,Ca^2 的色谱法条件，相对标准偏差小于0．5％，加标回收率在97．5％－104．0％。在水质分析中运用t检验法，比较了用钙、镁离子浓度计算和传统方法测定的总硬度之间是否存在显著性差异。     

Concentration and clean-up of trace hydrocarbons from atmospheric particulate matter

Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen (near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges (Supelclean ^tm LC-Silica SPE tubes and Sep-Pak^? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially important when aliphatic hydrocarbons concentrations are lower than 1 μg mL⁻¹. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples.     

Enhanced chromatographic resolution of amine enantiomers as carbobenzyloxy derivatives in high-performance liquid chromatography and supercritical fluid chromatography

The carbobenzyloxy (cbz) protecting group is evaluated for it's potential to enhance the resolution of chiral amine enantiomers using high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC). A series of cbz derivatives of commercially available racemates was prepared and analyzed by enantioselective chromatography using a variety of mobile phases and polysaccharide and Pirkle-type chiral stationary phases (CSPs). The cbz-derivatized product consistently demonstrated enhanced chiral resolution under HPLC and SFC conditions. Improved selectivity and resolution combined with an automated preparative HPLC or SFC system can lead to the rapid generation of highly purified enantiomers of desirable starting materials, intermediates or final products.     

A method for the determination of histamine in wine by HPLC with precolumn derivatization with phenylisothiocyanate

Summary A method for determining histamine in wine by precolumn derivatization with PITC (phenylisothiocyanate) with reversed-phase HPLC and UV detection is reported. Histamine can be determined together with the 24 amino acids within 40 min, or separately in a shorter time (less than 4 min) if a prior solid phase extraction clean-up is used.     

XPS,AFM, ATR and TPD evidence for terraced,dihydrogen terminated, 1×1 (100) silicon

Heating (100) silicon at high temperature (say, higher than 850 °C) in H₂, cooling to 670–700 °C in the same ambient, and quenching to room temperature in N₂ results in environmentally robust, terraced 1 × 1 (100) SiH₂. Evidence for this conclusion is based on angle‐resolved x‐ray photoelectron spectroscopy, atomic force microscopy, infrared absorption spectroscopy in the attenuated total reflection mode, thermal programmed desorption, and reflection high‐energy electron diffraction. Copyright © 2005 John Wiley & Sons, Ltd.     

Fe-Ni-B-O纳米合金的合成及其催化制氢性能的研究

Preparation and catalytic performance of Fe-Ni-B-O nano-alloy having crystal-palpus structure has been studied. Black powder was synthesized by reducing mixture solution of Fe²⁺, Ni²⁺ with KBH₄ as reducing agent and polyethylene glycol as dispersant. Fe-Ni-B-O nano-alloy of crystal-palpus structure was obtained after hydrogen reduction of black powder. TEM shows that crystal-palpus length is 200～400 nm, diameter is 2～4 nm. The analytic results indicate that the total content of Fe and Ni is 86.6%, B is 5.08%. The alloy exhibits excellent catalytic performance. Hydrogen generation rate can approach 100% especially when pH is 8.     

溴原子取代对二茂铁液晶化合物介晶性的影响

二茂铁液晶因其独特的稳定性和易于衍生化受到研究人员的青睐[1- 8] 。我们曾经报道过一类单取代二茂铁液晶的合成与介晶性[9] 。这里我们报道另外一类二茂铁单取代液晶 ,并对分子的长度、溴原子取代对介晶性的影响进行探讨。合成路线如下 :1　实验部分ＢｒｕｃｋｅｒＡＣＥ -2 0 0ｓｐｅｃｔｒｏｍｅｔｅｒ,ＣＤＣｌ3作溶剂。ＮｉｃｏｌｅｔＭａｇｎａ-ＩＲ 5 0 0Ｓｐｅｃｔｒｏｍｅｔｅｒ,ＳｅｒｉｅｓⅡ ,ＫＢｒ压片。ＷＲＳ -ＩＡ ,ＣａｒｌｏＥｒｂａ 1 1 0ｂ。Ｐｅｒｋｉｎ -Ｅｌｍｅｒ 7Ｓｅｒｉｅｓ热分析仪 ,分温速度 1 0℃ /ｍｉ…     

Headspace Solid-phase Microextraction–Gas Chromatographic–Mass Spectrometric Analysis of the Essential Oils of Two Traditional Chinese Medicines, Angelica pubescens and Angelica sinensis

Angelica pubescens and Angelica sinensis belong to the Umbelliferae family and both are used as traditional Chinese medicines. In the present study, headspace solid-phase microextraction (HS-SPME) with gas chromatography-mass spectrometry (GC-MS) was used for the analysis of the volatile constituents present in their roots. Eighty-seven compounds in Angelica pubescens and thirty-six compounds in Angelica sinensis were identified by GC-MS. Their relative contents were calculated by the peak area ratio. HS-SPME was compared to steam distillation (SD) by analyzing the volatile constituents of Angelica sinensis root. A good agreement between results obtained with both techniques was found. As a conclusion, HS-SPME is a powerful tool for determining the volatile constituents present in the TCMs.     

Synthesis of Some Allyl-β-Cyclodextrin Derivatives and their Properties as Capillary GC Stationary Phases

Summary Three -Cyclodextrin derivatives (-CDs) were synthesized by substituting the 2,6-OH groups of -CD with allyl groups and the 3-OH groups with three different acyl groups (valeryl, heptanonyl, octanoyl). The chromatographic properties of these -CDs as stationary phases for capillary gas chromatography (CGC) were studied. The test results showed that the three -CDs possessed good coating properties and that the capillary columns coated with them exhibited high column efficiency. These -CDs can separate not only the disubstituted benzene isomers but also some racemic compounds.     

Thermal decomposition of struvite

Struvite (NH₄MgPO₄·6H₂O) is a mineral often found in urinary tracts and kidneys. Thermal decomposition using slow low heating shows that the 'kidney' stone can be decomposed at temperatures below 40°C. At this temperature both ammonia and water are evolved. If more rapid heating is employed the decomposition occurs at around 80°C. The implication of this work rests with the use of low slow heat for the decomposition of the kidney stones. This revised version was published online in July 2006 with corrections to the Cover Date.