Crystallization and X‐ray structure of 3,3’,4‐trichlorobiphenyl (PCB 35)∗

A method for the preparation of single crystals of PCB 35 suitable for single crystal X‐ray structure determination was developed. This method has already been proven suitable for 2,4'‐dichlorobiphenyl and may prove useful for other PCBs or related compounds. The crystals of PCB 35 are orthorhombic, spacegroup P2₁22₁ (a= 10.665(8), 6 = 3.825(3), c= 14.086(9) Å) and the structure was refined to R = 0.094 for 156 unique observed reflections and 43 parameters. Although the crystals were of poor quality, the structure determination unequivocally confirmed the substitution pattern of the biphenyl moiety by Cl atoms inferred previously from spectroscopic methods. The dihedral angle between the planes of the two phenyl rings is 33(2)°.     

高效液相色谱-荧光检测法同时测定畜禽粪便中4种磺胺类药物残留

建立了高效液相色谱-荧光检测法测定畜禽粪便中4种磺胺药物(磺胺甲基嘧啶(SM1)、磺胺氯哒嗪(SCP)、磺胺邻二甲氧嘧啶(SDM’)、磺胺喹噁啉(SQ))的方法.样品用25 mL甲醇提取3次,合并提取液,浓缩干燥,用0.1 mol.L-1的HCL溶解残渣,经荧光胺衍生化后,用反相C18柱为分离柱,以乙腈∶0.5%乙酸=40∶60(V/V)为流动相进行洗脱,20 min内分离4种药物.在0.05—5.00μg.mL-1范围内,4种磺胺类药物的峰面积与质量浓度的线性关系良好(R2≥0.999),SM1、SCP、SDM’、SQ的定量限(LOQ)分别为2.3、6.3、4.3和9.6μg.kg-1;添加水平为50、100、1000μg.kg-1时,SM1、SCP、SDM’、SQ的回收率分别为74.91%—81.82%、78.45%—91.43%和86.10%—92.88%,RSD小于8.82%.     

Effects of temperature variation on TSD in turtle (C. picta) populations

We formulate a two-sex model of temperature-dependent sex determination (TSD) for a freshwater turtle (C. picta) population. The aim is to understand how environmental temperature variations and nest heat conduction properties affect the long term dynamics of the population. This is a key to understanding how global temperature changes may affect their survival. With stochastic inputs of ambient temperature and solar radiation, the model uses the heat equation to determine the temperature in the egg layer in the nest; in turn, this determines the sex ratio in the egg clutch using a variable degree-day model. Finally, a nonlinear Leslie type, stage-based, two-sex model, is used to determine the long term male and female populations. A two-sex model is required because of different development rates for males and females. The model is flexible enough to enable other researchers to examine the effects of temperature variation variations on other species with TSD, e.g., crocodilians, reptilians, as well as other turtle species. It can be adapted to study effects of nest location, soil type, rain events, different incubation periods, and density effects, for example, the dependence of the mating function on the ratio of males to females and each’s contribution to the sex of hatchlings. Modifications can be easily made to fit a specific life history traits. The model is a beginning step in understanding the long term, high fitness shown by many reptile species with TSD, and it may suggest to experimentalists what data may be relevant to these issues; it can also be useful to wildlife managers in developing strategies for intervention if needed. Among the principal findings are that temperature variability and detailed nest heat conduction properties may buffer projected negative effects on a population.     

The relentless progress of commodity exchanges in the establishment of primary commodity prices

A continuously expanding group of commodities are being priced on commodity exchanges. This paper explains the causes to the increasing preference of exchanges as pricing instruments. It also provides the detail of the shift in the 1970s and 1980s from producer determined prices to prices set by commodity exchanges for three major commodities—aluminum, nickel and petroleum.     

高锰酸盐指数测定的影响因素研究

采用正交实验设计法L9(34)考察高锰酸盐指数测定的影响因素,确定各因素的主次关系及最佳测定条件。结果表明,高锰酸钾浓度对高锰酸盐指数测定的影响程度最大,其次是加热时间及滴定时间,影响较小的是溶液的酸度。在最佳测定条件下:1+3硫酸、加热8min、60s内滴定、高锰酸钾浓度为0.0100mol/L,加标回收率为101%。     

含油污泥油含量测定方法

根据“相似易溶”原理,采用重量法和索氏抽提-紫外吸收光度法对含油污泥的油含量测定进行了研究,利用差重和含有芳香族化合物的石油及其产品在紫外区的吸收波长特性,采用了毒性较小的正己烷、石油醚或混合庚烷等作为萃取荆。根据试验结果可知,重量法具有药荆使用量少、标准偏差小（1.48％）,结果准确等特点;紫外吸收光度法具有操作简便、数据重现性好等优点,适于芳烃含量较高的含油泥油含量的测定。     

土壤中矿物油含量测定方法研究

建立了土壤中矿物油含量的分析方法。采集的土壤鲜样,采用无水硫酸钠进行化学干燥。用四氯化碳提取土壤中的油类物质,采用硅酸镁去除提取液中的动植物油等极性化合物后,使用红外分光测油仪测定提取液中的矿物油含量。此方法具有良好的线性关系,相关系数在0.9999以上。测定下限为1.85 mg/l,测定上限为100 mg/l,测量范围为9 mg/kg～500 mg/kg,方法的灵敏度为1.05。试剂空白加标回收率56%～83%,实际样品加标回收率在69%～74%之间。该法简便快速,灵敏准确,具有广泛的应用前景。     

环境样品中汞形态分析技术的进展

汞的毒性、环境行为、生物有效性不仅跟其浓度有关,还决定于其化学形态,因此汞的形态分析在环境科学中具有重要意义。样品前处理几乎是汞形态分析研究中不可或缺的步骤,而色谱和光谱/质谱联用技术是目前普遍采用的分离检测方法。文章对近十年来这些方面的研究进展进行了综述,主要包括样品的前处理方法如酸/碱溶剂萃取、微波辅助萃取、固相萃取、固相微萃取、单滴微萃取、分散液液微萃取等,以及色谱(液相色谱、气相色谱)和毛细管电泳与光谱/质谱(紫外可见光谱、原子吸收光谱、原子荧光光谱、等离子体质谱等)的联用技术在汞化合物形态分析中的应用情况。最后提出今后应重点研究建立高效、简便的前处理方法,发展高分离度、高灵敏度、高速度的分离检测联用技术,以便更好地对汞的形态进行分析监测。     

矿井通风系统稳定性定量判定方法研究

稳定的矿井通风系统是实现矿井安全高效生产的前提,但是随着采掘工作面的推进,通风网络结构的变化,巷道的冒顶变形等,通风系统的稳定性也随之变化.基于矿井通风系统稳定性的重要性、非线性和时变性,运用Lyapounov(李雅普诺夫)稳定性理论和灵敏度,提出了定量分析判定矿井通风系统稳定性的方法.方法以Lyapounov稳定性分...     

预浓缩-GC/MS测定空气中的27种ODS和HFCs

优化预浓缩仪二级冷阱温度和柱温箱初始温度,建立了预浓缩-气相色谱 /质谱联用(GC/MS)技术测定空气中27种消耗臭氧层物(ODS)和氢氟烃(HFCs)的分析方法。结果表明,27种ODS和HFCs峰形良好,分离度较好,校准曲线相对响应因子标准偏差为1.7%~15.9%,方法检出限为0.016~0.172 μg/m³。空白加标样品连续测定6次的相对标准偏差为0.9%~13.4%,回收率为70.4%~116%。基体加标样品连续测定6次的相对标准偏差为1.0%~7.8%,回收率为94.3%~108%。实验楼周边的环境空气以及实验室内部工作环境空气均检出不同浓度的ODS和HFCs,该方法适用于空气中ODS和HFCs的测定。