Analysis of sulfur-containing compounds in crude oils by comprehensive two-dimensional gas chromatography with sulfur chemiluminescence detection

This paper reports an analytical method for separating, identifying, and quantifying sulfur-containing compounds in crude oil fraction (IBP-360degreesC) samples based on comprehensive two-dimensional gas chromatography coupled with a sulfur chemiluminescence detector. Various sulfur-containing compounds and their groups were analyzed with one direct injection. 3620 peaks were detected including 1722 thiols/thioethers/ disulfides/1-ring thiophenes, 953 benzothiophenes, 704 dibenzothiophenes, and 241 benzonaphthothiophenes. The target sulfur compounds and their groups were identified based on the group separation feature and structured retention of comprehensive two-dimensional gas chromatography as well as standard substances. The quantitative analysis of major sulfur-containing compounds and total sulfur was based on the linear response of the sulfur chemiluminescence detector using the internal standard method. The sulfur contents of target sulfur compounds and their groups in 4 crude oil fractions were also determined. The recoveries for standard sulfur-containing compounds were in the range of 90-102%. The quantitative result of total sulfur in the Oman crude oil fraction sample was compared with those from ASTM D 4294 standard method (total S by X-ray fluorescence spectrometry), the relative deviation (RD%) was 4.2% and the precision of the method satisfactory.

长白山北坡植物群落复杂性的海拔梯度变化(英文)

应用梯度格局法在长白山北坡海拔700m-2600m的坡面上每100 m海拔设置一样地,共计20块样地,通过对同一群落各样方间的相异性测定,对各海拔植物群落的复杂性进行了分析。结果表明,以主林层乔木种的二元数据计算的结果,除亚高山岳桦林外,其它各海拔群落的样方间均表现出较高的相异性,特别是低海拔的阔叶红松林平均相异系数达0.74,明显高于其它植被类型;暗针叶林各群落间差异不大,相对而言1400 m群落样方间的相异性略高于其它群落,表现出过渡性群落树种组成的复杂性;岳桦林树种组成简单,样[(\267\275\274\344\322\262\261\355\317\326\263\366\275\317\270\337\265\304\\317\340\313\306\320\324\241\243)-0.1(\322\324\271\340\304\276\326\326\265\304\266\376\324\252\312\375\276\335\\274\306\313\343\265\304\310\272)]落内的相异性,虽低海拔的阔叶红松林总体上高于其它群落,但差异趋势并不像乔木种那么明显。以各草本植物与所有植物种的二元数据计算的各海拔群落内样方间的相异性,表现出非常相近的趋势,群落内样方间草本植物及所有植物种均以阔叶红松林及高山冻原差异最大,暗针叶林基本稳定于比较相近的水平。图3表1参8。

Investigation of thermodynamic properties of Co2O3 powder

The isobaric molar heat capacities of powder of Co2O3 were determined by an adiabatic calorimeter in the temperature range from 78 to 350 K. No phase transition takes place in this temperature range. The relationship of C-p,C-m with thermodynamic temperature T was established as C-p,C-m = -5 x 10(-6)T(3) + 0.0026T(2) + 0.0325T + 4.2592 (J K-1 mol(-1)), fitting coefficient R-2 = 0.9996. According to this relationship and the relationships between thermodynamic functions, the thermodynamic functions of powder of C2O3 were derived with 298.15 K as reference temperature. Thermal decomposition of Co2O3 powder was studied through thermogravimetry (TG). The possible mechanism of the thermal decomposition reaction was suggested according to the TG result. (C) 2003 Elsevier Science B.V. All rights reserved.

放牧和封育条件下科尔沁沙地小叶锦鸡儿群落土壤种子库特征

以科尔沁沙地小叶锦鸡儿群落为研究对象,对比分析了放牧干扰和不同封育年限下土壤种子库特征。结果表明:①放牧和封育样地土壤种子库均以一年生植物为主,物种丰富度没有明显差异;②放牧样地土壤种子库密度为(3 475±519)粒/m2,封育6年和封育12年样地土壤种子库密度分别为(20 241±1 714)粒/m2和(28 777±3 946)粒/m2,显著高于放牧样地;③Shannon-W iener多样性指数、S impson多样性指数和P ielou均匀度指数在放牧样地分别为1.36,0.68和0.56,并随着封育年限的增加而降低;④放牧和封育样地土壤种子库主要分布于0~2 cm的土壤表层,封育样地各层的种子库密度均显著高于放牧样地;⑤放牧和封育样地土壤种子库均为聚集分布,但放牧样地种子库的空间异质性高于封育样地。

Molecularly imprinted monolithic stationary phases for liquid chromatographic separation of enantiomers and diastereomers

The method for preparation of molecularly imprinted monolithic stationary phase has been improved to achieve liquid chromatographic separation of enantiomers and diastereomers. By adopting low polar porogenic solvents of toluene and dodecanol and optimal polymerization conditions, the molecularly imprinted monolithic stationary phases with good flow-through properties and high resolution were prepared. Enantiomers of amino acid derivatives and diastereomers of cinchona alkaloids were completely resolved using the monolithic stationary phases. The influence of porogenic composition, monomer-template ratio and polymerization conditions on the chromatographic performance was investigated. Some chromatographic conditions such as the composition of the mobile phase and the temperature were characterized. Scanning electron microscopy showed that the molecularly imprinted monolithic stationary phase has a large through-pore structure to allow the mobile phase to flow through the column at very low backpressure. Accelerated separations of enantiomers and diastereomers were therefore achieved at elevated flow rates. Finally, the chiral recognition performance of the prepared stationary phase in aqueous media was investigated. Hydrophobic interaction, and ionic and/or hydrogen bonding interactions were proposed to be responsible for the recognition mechanism. (C) 2002 Elsevier Science B.V. All rights reserved.

海洋光合细菌Rx菌株的分离鉴定与生物学特性研究

　从大连金州区海湾养虾池底分离获得光合细菌Rx菌株的初筛菌株,并对其纯培养物进行了形态特征、培养特征、生理生化特征以及DNA中G+C摩尔百分比等生物学特性分析。结果表明,Rx菌株为革兰氏阴性菌,大小为(0.5～0.7)μm×(1.0～1.2)μm,单极生鞭毛,光合内膜为泡囊状,繁殖方式为二分分裂生殖;Rx菌株的纯培养物含细菌叶绿素a和球状素型类胡萝卜素,光照厌氧和黑暗好氧条件均能生长;Rx菌株生长盐度为5～100g/kg,生长pH为5.8～8.4;Rx菌株不能利用硫化物为电子供体,其生长受高浓度硫化物的抑制;能利用谷氨酸而不能利用柠檬酸钠、酒石酸为有机碳源或电子供体;盐酸硫胺素(t)、生物素(b)、p-对氨基苯甲酸(p-ABA)、烟酸(n)为Rx菌株生长的必需因子;Rx菌株DNA的G+C摩尔百分比为64.18%。根据以上特征,并参照《常见细菌系统鉴定手册》(2002)和《伯杰氏细菌系统学手册》第3卷(1989),将Rx菌株鉴定为小红卵菌属广海小红卵菌(Rhodovulumeuryhalinum)。

Affinity membrane chromatography for the analysis and purification of proteins

Affinity chromatography is unique among separation methods as it is the only technique that permits the purification of proteins based on biological functions rather than individual physical or chemical properties. The high specificity of affinity chromatography is due to the strong interaction between the ligand and the proteins of interest. Membrane separation allows the processing of a large amount of sample in a relatively short time owing to its structure, which provides a system with rapid reaction kinetics. The integration of membrane and affinity chromatography provides a number of advantages over traditional affinity chromatography with porous-bead packed columns, especially with regard to time and recovery of activity. This review gives detailed descriptions of materials used as membrane substrates, preparation of basic membranes, coupling of affinity ligands to membrane supports, and categories of affinity membrane cartridges. It also summarizes the applications of cellulose/glycidyl methacrylate composite membranes for proteins separation developed in our laboratory. (C) 2001 Elsevier Science B.V. All rights reserved.

缓/控释氮素肥料对土壤生物学活性的影响

采用盆栽试验方法,研究施用不同种缓/控释氮素肥料对玉米苗期土壤脲酶、硝酸还原酶活性、微生物生物量碳和氮的影响。结果表明:在玉米苗期,施用脲酶抑制剂(NBPT)涂层大颗粒尿素、硝化抑制剂(DCD)与NBPT混合涂层大颗粒尿素肥料对脲酶活性有显著的抑制作用,脲酶活性为48～50mgNH3-N·kg-1土·24h-1;施用DCD与NBPT混合涂层大颗粒尿素肥料,硝酸还原酶活性最高,为1.43μgN·g-1土·24h-1,施用含有NBPT肥料对硝酸还原酶活性没有显著影响。玉米苗期施用NBPT涂层尿素肥料微生物量碳、氮含量最高,分别为241和57mg·kg-1土,NBPT对土壤微生物量没有产生负面影响。施用不同种缓/控释氮素肥料微生物量氮变化与微生物量碳一致,施用DCD与NBPT混合涂层大颗粒尿素肥料微生物量氮与对照无显著差别,为50mg·kg-1土。施用DCD与NBPT混合涂层大颗粒尿素肥料,玉米苗期微生物固持氮素能力没有受到影响,同种膜材料包膜NBPT/DCD涂层尿素制成的控释氮肥,对土壤生物学活性影响明显强于直接包膜大颗粒尿素制成的控释氮肥的作用效果。不同种缓/控释肥料玉米苗期土壤生物学活性差异表明,丙烯酸树脂包膜尿素制成的控释氮肥,对氮素或抑制剂的控释效果显著好于醋酸酯淀粉包膜尿素制成的控释氮肥。

Transient state of chiral recognition in a binary mixture of cyclodextrins in capillary electrophoresis

The transient state (as the defined point where no enantioseparation is obtained in a dual chiral selector system) of chiral recognition of aminoglutethimide in a binary mixture of neutral cyclodextrins (CDs) was studied by capillary electrophoresis (CE). The following three dual selector systems were used: alpha-cyclodextrin (alpha-CD) and beta-cyclodextrin (beta-CD); alpha-CD and heptakis(di-O-methyl-beta-cyclodextrin) (DM-beta-CD); alpha-CD and heptakis(tri-O-methyl-beta-cyclodextrin) (TM-beta-CD). The S-(-) enantiomer of the analyte was more strongly retained in the presence of either alpha-CD or TM-beta-CD at pH 2.5, 100 mM phosphate buffer, while the R-(+) enantiomer was more strongly retained in the presence of either P-CD or DM-P-CD. In the more simple case, the elution order is invariably kept if the enantiomers have the same elution order in either one of the two hosts of the binary mixture. In contrast, the elution order may be switched by varying the concentration ratio of two hosts that produce opposite elution order for this particular analyte. In such a dual selector system, the enantioselectivity will disappear at the transient state at a certain ratio of host,:host, Moreover, the migration times of the two enantiomers with host, alone (diluted in buffer) is approximately equal to the migration times at the corresponding concentration of host, alone (diluted in buffer), where the ratio of concentrations of host,:host, is the same as in the binary mixture at the transient state. As found by nuclear magnetic resonance experiments, the analyte is forming a 1:1 complex with either one of the CDs applied. From this finding, a theoretical model based on the mobility difference of the two enantiomers was derived that was used to simulate the transient state. (C) 2000 Elsevier Science B.V. All rights reserved.