气相色谱法测定海洋沉积物中十氯酮残留

研究了提取溶剂效率、毛细管柱极性、净化条件及共溶出干扰物等因素对十氯酮测定的影响;对比了加速溶剂提取及超声波提取方式,考察了DB-17、DB-1701与DB-5毛细管柱分离度,及不同比例甲醇/正己烷混合溶液作为定容溶液的分析结果。建立了加速溶剂萃取,H2SO4净化分离,DB-5毛细管柱电子捕获检测器(ECD)-气相色谱法(GC)测定海洋沉积物介质中有机氯农药类持久性有机污染物十氯酮残留分析方法。将5 g沉积物干样与3 g活化铜粉及3 g无水Na2SO4混匀后,采用二氯甲烷-丙酮(1∶1,V/V)进行加速溶剂萃取;萃取液浓缩后,用H2SO4净化,以1%甲醇-正己烷混合溶液定容后,采用DB-5非极性毛细管柱,及配备电子捕获检测器气相色谱测定十氯酮含量。本方法采用外标法进行定量分析,在0.005～0.1 mg/L浓度范围内,线性相关系数为0.9989;加标回收率为75%～98%;相对标准偏差为3.7%～9.6%(n=6);检出限为0.12 ng/g。     

Analytical and kinetic study of the aqueous hydrolysis of four organophosphorus and two carbamate pesticides

The hydrolysis of six selected pesticides has been studied in aqueous solution. Four organophosphorus pesticides (disulfoton, isofenfos, isazofos and profenfos) and two N-methylcarbamate derivatives (oxamyl and ethiofencarb) were selected. Hydrolysis was performed in purified buffered water at different pH in the range 7.0–10.0 (ionic strength?=?2.5?mM, T?=?25°C). At pH?=?8.0, isofenfos and disulfoton (t _1/2?≈?4 years, t _1/2?≈?1 year, resp.) were found to be far more stable than isazofos (t _1/2?≈?5 months), ethiofencarb and profenofos (t _1/2<1 month), themselves more stable than oxamyl (t _1/2?≈?1 day). As expected, a strong dependence on pH was observed for all pesticides: the rate of degradation increased when the pH increased. Degradation products were identified by GC–MS and/or LC–MS. Possible structures are presented in the article.     

Determination of dissolved and particle-bound PCB congeners at ultra-trace concentrations in water

Adsorption of 10 PCB congeners in aqueous solutions on glass-fibre filters taken from different boxes but of the same type were not significantly different. The standard deviations using filters from the same box were below 10% at concentration levels of 4.1?ng?L^?1. At this level, the adsorption of dissolved PCB at the filters was in the range of 5–20% depending on the congener. This led to a procedure for determination of dissolved and particle-bound congener in authentic landfill leachate, which included correction for adsorption losses. The procedure was based on filtration through glass-fibre filters, followed by trapping of the PCB in the eluate on solid-phase extraction (SPE) disks. After separate supercritical fluid (SFE) extractions, with carbon dioxide, of the filters as well as of the SPE disks, the extracts were analysed on a two-column capillary GC-ECD system. Corrections for congener adsorption on glass-fibre filters were made, from which corrected distribution constants between particle-bound and dissolved PCB congener in the water phase could be obtained for authentic landfill leachate. These values (10⁴–10⁵) agreed well with those obtained by others.     

二甲基亚砜对乙酸气相色谱保留时间的影响及其机理

通过气相色谱、红外光谱分析和量子化学计算,探究溶于二甲基亚砜（DMSO）中乙酸保留时间发生波动的原因。 结果显示,乙酸保留时间变化与DMSO体积等量递增呈线性关系,R²=0.99301;根据红外光谱分析得出,DMSO和乙酸之间生成了氢键,以DMSO-乙酸分子的形式通过色谱柱;根据Gaussian09程序计算结果,DMSO电子密度大的部分给予电子,与乙酸之间形成了氢键,而DMSO电子密度小的部分容易获得电子与具有强偶极矩的色谱柱固定液聚乙二醇产生作用力,吸附在固定液上。因此,在上述一系列复杂的分子间作用力的共同影响下,乙酸保留时间发生了波动,且随着溶剂DMSO体积比增加,乙酸保留时间不断延长。     

物理化学混合式教学设计与实践——以“单组分系统相变热力学”为例*

以“单组分系统相变热力学”为例介绍了物理化学混合式教学设计与教学实践。围绕课程教学目标,在课前、课中、课后的每一个教学环节中践行课程教学理念,通过“问题+案例”方式突出物理化学基本方法的应用性、普适性与前沿性,让学生在教学过程中获取原理、体验探究、发展思维、生成智慧。教学评价结果显示,绝大部分学生对混合式教学模式给予了积极的评价。     

Progress of Jinping Underground laboratory for Nuclear Astrophysics (JUNA)

Jinping Underground laboratory for Nuclear Astrophysics(JUNA) will take the advantage of the ultra-low background of CJPL lab and high current accelerator based on an ECR source and a highly sensitive detector to directly study for the first time a number of crucial reactions occurring at their relevant stellar energies during the evolution of hydrostatic stars. In its first phase, JUNA aims at the direct measurements of~(25)Mg(p,γ)~(26)Al,~(19)F(p,α)~(16)O,~(13)C(α,n)~(16)O and ~(12)C(α,γ)~(16)O reactions. The experimental setup,which includes an accelerator system with high stability and high intensity, a detector system, and a shielding material with low background, will be established during the above research. The current progress of JUNA will be given.     

Multi-Center Vector Field Methods for Wave Equations

We develop the method of vector-fields to further study Dispersive Wave Equations. Radial vector fields are used to get a-priori estimates such as the Morawetz estimate on solutions of Dispersive Wave Equations. A key to such estimates is the repulsiveness or nontrapping conditions on the flow corresponding to the wave equation. Thus this method is limited to potential perturbations which are repulsive, that is the radial derivative pointing away from the origin. In this work, we generalize this method to include potentials which are repulsive relative to a line in space (in three or higher dimensions), among other cases. This method is based on constructing multi-centered vector fields as multipliers, cancellation lemmas and energy localization.     

Measurement of the muon capture rate in hydrogen gas and determination of the proton's pseudoscalar coupling gP

The rate of nuclear muon capture by the proton has been measured using a new technique based on a time projection chamber operating in ultraclean, deuterium-depleted hydrogen gas, which is key to avoiding uncertainties from muonic molecule formation. The capture rate from the hyperfine singlet ground state of the microp atom was obtained from the difference between the micro(-) disappearance rate in hydrogen and the world average for the micro(+) decay rate, yielding Lambda(S)=725.0+/-17.4 s(-1), from which the induced pseudoscalar coupling of the nucleon, g(P)(q(2)=-0.88m(2)(micro))=7.3+/-1.1, is extracted.     

Geoneutrinos

Academician M.A. Markov in the 1960s first proposed detecting the electron antineutrino in the reaction of inverse beta decay on a proton to study the processes inside the Earth. The radioactive isotopes ²³⁸U, ²³²Th, and ⁴⁰K present in our planet decay with radiation of neutrinos (antineutrinos). Neutrinos that are produced reach the Earth’s surface practically without absorption and carry information about the internal structure of the planet. However, because of the smallness of the antineutrino fluxes and interaction cross sections with matter, antineutrinos of geological origin were first registered in only two experiments (Borexino and Kamland) in recent years. The experimental observation of antineutrinos from the isotope decays in the depths of the Earth is the only way to study the radiation in our planetary interior.