一种消毒样品的电喷雾质谱分析

从《禁止化学武器公约》1997年4月正式生效以来,化学核查方法研究不断深入,从鉴定化学战剂原体逐步向降解、消毒等相关化学品方向发展,且扩展到复杂的环境基质样品。为了确保各缔约国履约,对于已被"禁止化学武器组织"(简称OPCW)指定和正在寻求指定的实验室,每年至少要参加一次水平考试,分析公约附表化学品及它们的前体和降解产物,并取得优异的成绩,只有这样,才有资格分析真实样品(从被怀疑的产品或者储藏地点或者是从宣布使用过化学武器的环境中采集的)。本文样品是OPCW组织的第十四次水平考试的"消毒"废液样品D及其空白对照DB,采用液相色谱-电喷雾质谱联用技术(HPLC-ESI-MS)对样品进行定性检测,结合其他分析方法,结果与配样清单完全一致,见表1。     

PIXE法分析共聚物中痕量氯

四氟乙烯和全氟4-甲基-3,6-二氧杂-△~7辛基磺酰氟在溶剂氟里昂-113(F-113)中进行自由基引发聚合反应时,共聚物(T-O)是否有链转移,可以通过测定所得共聚物中的含氯量来得以证实。我们首次应用质子X萤光分析法(PIXE)进行分析。结果表明,共聚物中含氯量小于1ppm,F-113溶剂并未发生链转移。同时,我们测定了已证明有F-113参与链转移反应的F_(40)试样,含氯量高达700ppm。     

疏松砂岩油藏深部稳砂体系配方设计与应用

针对油藏充填砂的治理,研制了一种新型的防膨抑砂剂NTW-1。室内性能评价表明,防膨抑砂剂具有防膨和抑砂能力,其效果分别优于目前常用的其它抑砂剂或粘土稳定剂的平均水平10.5%和65.6%,同时现场使用简便、成本较低。根据油藏出砂机理,提出了“深部稳砂”新观点,以合成的防膨抑砂剂NTW-1为基础,研究了“深部稳砂”新体系配方,现场应用表明,与常规措施相比,该体系增强了充填砂与骨架砂间的结合力,阻止了深部充填砂的运移,缩小了出砂空间,防砂成功率和有效期分别提高了8.8%和37.3%,单井增油平均提高了46.2%。     

Magnetic Suspension Balance For Simultaneous Measurement of a Sample and the Density of the Measuring Fluid

This paper deals with gravimetric measurements of adsorption equilibria of gases on the surface of porous solids with a new type of magnetic suspension balance. Items discussed include the measurement of adsorption data at high pressure and temperature as well as the simultaneous measurement of adsorption and the density of the adsorptive gas using only one magnetic suspension balance. This revised version was published online in August 2006 with corrections to the Cover Date.     

Analysis of some medicinal plants in South-western Nigeria using PIXE

Summary Analysis of thirteen medicinal plants of various biological activities commonly used in South-western Nigeria was carried out using PIXE technique. Nine of these plants are anti-cancer while four are antimicrobial. PIXE measurements were carried out using collimated proton beams delivered by the 2. 5 MV AN 2000 Van de Graaff accelerator at the Istituto Nazionale di Fisica Nucleare (INFN), (LNL) Legnaro, (Padova), Italy. The results showed the presence of twenty three different elements in the plants and none of them contains any toxic heavy metals. Only Chenopodium ambrosioides showed detectable levels of selenium which is considered important in cancer prevention.     

Pyrolysis Kinetics of Phenols from Lignite Semicoking Tar

The features of pyrolysis of phenols from lignite semicoking tar were studied. The activation energy and order of the reactions of accumulation of methane, hydrogen, carbon monoxide and dioxide, naphthalene and its methyl homologs, phenols, and isomeric cresols and dimethylphenols were determined.     

农业样品分析

本文是本刊“农业样品分析”第三篇定期评述，对１９９４年４月至１９９８年６月（着重于近两年）国内农业测试分析的进展作了评述，包括分子光谱、原子光谱、色谱、电化学、电泳分析，共引用文献６７５篇。     

深共熔溶剂同步提取红景天中红景天苷和酪醇

采用深共熔溶剂(Deep eutectic solvents, DESs)法同步提取红景天中红景天苷和酪醇. 首先, 通过对氢键供体(HBD)、 氢键受体(HBA)及二者摩尔比和DESs含水量等因素的设计优化, 获得了同步提取红景天苷和酪醇的最佳DES为乙二醇-乙酰丙酸(摩尔比为1∶1), 含水质量分数为40%, 记为LAEG-40. 然后, 以LAEG-40作提取溶剂, 对提取方法、 料液比、 提取温度及提取时间等因素进行优化, 获得了最佳提取条件: 采用150 r/min搅拌速率提取, 料液比为1∶12.5(g/mL), 提取温度60 ℃, 提取时间65 min. 在此条件下LAEG-40对红景天苷的提取率可达(18.1268±0.1667) mg/g, 酪醇提取率可达(1.5608±0.0240) mg/g. 而在相同条件下, 以水和乙醇作为提取溶剂, 红景天苷提取率分别为(15.1221±0.1342)和(16.3425±0.0897) mg/g, 酪醇提取率分别为(1.1120±0.0389)和(1.1923±0.0423) mg/g, 可见LAEG-40的提取效果明显高于传统溶剂. 研究结果表明, LAEG-40是一种绿色、 高效的红景天苷和酪醇同步提取溶剂, 可用于替代传统溶剂.     

Applications of Deep Eutectic Solvents in Sample Preparation and Extraction of Organic Molecules

The use of deep eutectic solvents (DES) is on the rise worldwide because of the astounding properties they offer, such as simplicity of synthesis and utilization, low-cost, and environmental friendliness, which can, without a doubt, replace conventional solvents used in heaps. In this review, the focus will be on the usage of DES in extracting a substantial variety of organic compounds from different sample matrices, which not only exhibit great results but surpass the analytical performance of conventional solvents. Moreover, the properties of the most commonly used DES will be summarized.     

Evaluation of thick target PIXE analyses with a minicomputer

Thick target particle-induced X-ray emission (TTPIXE) spectrometry has been increasingly used for multielement and trace element analyses. The theoretical background and a formalism are presented for their evaluation by means of a minicomputer. Numerical results are given and compared with the experimental ones. The advantage of the program is shown by a special experimental example.     

因子分析—吸光光度法同时测定钢样中的钼和钨

本文研究了因子分析－吸光光度法同时测定钼和钨的最佳条件，并测定了合金钢实际试样中此两元素的含量，结果令人满意。     

双波长分光光度法同时测定贵金属冶金物料中铱,铑的研究

本文利用铱、铑与溴化亚锡和2-巯基苯并噻唑的显色反应,建立了同时测定铱、铑的双波长分光光度法。铱的测定用等吸收波长法(λ_2=415nm,λ_1=523nm);铑的测定用倍率系数法(λ_2~′=476nm,λ_1~′=460nm,K=2.20)。铱、铑的含量在工作曲线浓度(100μg/10ml)范围内以1:8或8:1共存互不干扰。方法简便快速,结果准确。用于实际物料分析,结果满意。     

PIXE eleemental analysis of erythrocyte and blood plasma samples from human pregnancies

Elemental concentrations of P, S, Cl, K, Ca, Fe, Ni, Cu, Zn, Br, Rb have been determined in erythrocyte and blood plasma samples from normal and diabetic human pregnancies. Average values, the dependence of the concentrations on the time during gestation period, the correlation coefficients for pairs of elements as well as for the same elements in plasma and erythrocyte samples are given. A marked difference appeared in a number of cases between normal and diabetic pregancies.     

Analysis of archaeological artefacts: PIXE, XRF or ICP-MS?

Elemental analysis of ancient artefacts is of considerable benefit to the field of Archaeology and of general interest to earth scientists. Several techniques are currently available for this purpose, and in this paper the capabilities of PIXE (Particle Induced X-ray Emission), XRF (X-ray Fluorescence) and ICP-MS (Inductively Coupled Plasma - Mass Spectrometry) were evaluated to establish which of these instrumental methods was best suited especially for routine on-line usage. The elements of interest discussed in this paper are useful in archaeological provenance studies.     

Analysis of geological standards with PIXE and PIGE technioues applications to volcanic rocks

Geological standards are analyzed using PIXE and PIGE techniques. The concentrations of up to 26 elements are determined and compared with those obtained by other methods. PIXE and PIGE techniques are also applied to different volcanic rock samples. Their sensitivity, accuracy, and speed of data collection and reduction, are of great interest in the study of volcanic phenomena.     

PIXE analysis of human stones: Comparison with data from ICP-AES

25 human stone samples previously analyzed by inductively coupled plasma atomic emission spectroscopy /ICP-AES/ and the IAEA Animal Bone Standard Reference Material were used to evaluate trace element analysis by PIXE. Bombardment with 4 MeV protons was used for the determination of Mn, Fe, Cu, Pb, Br, Rb, Sr as well as Ca. PIXE and ICP-AES data gave correlation factors better than 0.97 for the elements Ca, Fe, Zn, Sr and Pb.     

PIXE and PIGE analysis of pre-colonial pottery from Patanal - MS,Brazil

Summary The purpose of this study was to investigate by PIXE and PIGE the pottery from two archaeological sites located near the Brazil-Bolivia border in Pantanal, an area of natural preservation. The region was inhabited by ancient Amerindian tribes long before the Latin America colonization period and a deep understanding of their environment, cultural attributes and interconnections can only be achieved based on the study of archaeological findings. Multivariate statistical procedures were used to determine similarities and correlations between the analyzed samples and to indicate possible sources of raw material provenience. The results showed that traces of Cr, Cu and Ti and Na/Si and Mg/Si counting ratios were important to distinguish sherds from the archaeological sites MS-CP-71 and MS-CP-61.     

电堆集-非水毛细管电泳分离测定甘草次酸和阿魏酸的研究

建立了电堆集富集-非水毛细管电泳(NACE)同时分离测定甘草中甘草酸和阿魏酸的新方法.系统研究了电压、非水溶剂、乙酸钠浓度、氢氧化钠浓度、样品溶剂等因素对电堆集和分离效果的影响,确立了分离和富集的最佳条件.以甲醇-乙腈(体积比4 : 6)为非水介质,30 mmol·L-1乙酸钠-2.5 mmol·L-1氢氧化钠为背景电解质;分离电压-20 kV,检测波长254 nm.在优化条件下,甘草次酸在0.80 ～12.80 mg·L-1(r＝0.999 6),阿魏酸在0.77 ～45.60 mg·L-1(r＝0.999 6)质量浓度范围内线性关系良好,回收率分别为97% ～102%,98% ～102%;甘草次酸检出限为0.069 mg·L-1,阿魏酸检出限为0.087 mg·L-1,RSD均不大于4.6%.