分光光度法研究铝制品对水样溶出铝含量的影响

采用分光光度法,在pH为3-4的酸度条件下,以二甲酚橙为显色剂,快速检测水样中微量铝的含量.研究了不同情况下不同铝制品对水样溶出铝含量的影响.结果表明:水样在铝制品中放置时间越长,从铝制品中溶解出的铝越多,而且薄的铝制品中溶出的铝要比铝合金锅中溶出的多;当在水中加入一定量的食盐后,由铝制品中溶解出的铝含量明显增多.本方法简便快速,灵敏度高,对样品测定的结果令人满意.     

Stability of low levels of perchlorate in drinking water and natural water samples

Perchlorate ion (ClO₄⁻) is an environmental contaminant of growing concern due to its potential human health effects, impact on aquatic and land animals, and widespread occurrence throughout the United States. The determination of perchlorate cannot normally be carried out in the field. As such, water samples for perchlorate analysis are often shipped to a central laboratory, where they may be stored for a significant period before analysis. The stability of perchlorate ion in various types of commonly encountered water samples has not been generally examined—the effect of such storage is thus not known. In the present study, the long-term stability of perchlorate ion in deionized water, tap water, ground water, and surface water was examined. Sample sets containing approximately 1000, 100, 1.0, and 0.5 μg l⁻¹ perchlorate ion in deionized water and also in local tap water were formulated. These samples were analyzed by ion chromatography for perchlorate ion concentration against freshly prepared standards every 24 h for the first 7 days, biweekly for the next 4 weeks, and periodically after that for a total of 400 or 610 days for the two lowest concentrations and a total of 428 or 638 days for the high concentrations. Ground and surface water samples containing perchlorate were collected, held and analyzed for perchlorate concentration periodically over at least 360 days. All samples except for the surface water samples were found to be stable for the duration of the study, allowing for holding times of at least 300 days for ground water samples and at least 90 days for surface water samples.     

固相微萃取研究进展

对固相微萃取的发展背景，应用及其研究进展作了综述。引用文献 145篇。     

微波消解ICP-AES法测定玩具塑料中镉

采用微波加压消解溶样，ICP-AES法测定玩具塑料中镉含量，选择最佳工作条件，方法简便、快速、可靠。适用于各类玩具塑料中镉含量的分析。     

Flow injection in-valve-mini-column pretreatment combined with ion chromatography for cadmium, lead and zinc determination

A flow injection (FI) in-valve-mini-column packed with Chelex-100 resin is proposed for on-line sample pretreatment for some metal ions, namely, Cd(II), Pb(II) and Zn(II), prior to simultaneous determination using ion chromatography (IC). A solution containing a mixture of the cations was first passed through the in-valve-mini-column, followed by on-line elution. The eluate was then flowed further to an injection valve and was injected into an ion chromatograph. Conditions of the system were optimized. A single standard calibration was possible. The recoveries of cations were found to be in the range of 95–105%. The developed method was applied to the accurate analysis of zinc ore samples.     

A method for calibration and validation subset partitioning

This paper proposes a new method to divide a pool of samples into calibration and validation subsets for multivariate modelling. The proposed method is of value for analytical applications involving complex matrices, in which the composition variability of real samples cannot be easily reproduced by optimized experimental designs. A stepwise procedure is employed to select samples according to their differences in both x (instrumental responses) and y (predicted parameter) spaces. The proposed technique is illustrated in a case study involving the prediction of three quality parameters (specific mass and distillation temperatures at which 10 and 90% of the sample has evaporated) of diesel by NIR spectrometry and PLS modelling. For comparison, PLS models are also constructed by full cross-validation, as well as by using the Kennard-Stone and random sampling methods for calibration and validation subset partitioning. The obtained models are compared in terms of prediction performance by employing an independent set of samples not used for calibration or validation. The results of F-tests at 95% confidence level reveal that the proposed technique may be an advantageous alternative to the other three strategies.     

Air sampling of aromatic hydrocarbons in the presence of ozone by solid-phase microextraction

Effects of ozone on air sampling of standard gas mixtures of aromatic hydrocarbons were tested using solid-phase microextraction (SPME). Standard concentrations of ozone ranging from 10 ppb (v/v) to 6400 ppm (v/v) were generated using an in-house built ozone generator based on corona discharge. Effects of temperature, discharge voltage, and oxygen flow on the ozone generation were tested. The working dc voltage had the greatest effect on generated ozone concentration and was proportional to the ozone concentration. Generation temperature and oxygen flow rate were inversely proportional to ozone concentrations. Produced ozone was mixed with standard benzene, toluene, ethylbenzene, and xylenes (BTEX) gas at less than 100 ppb (v/v). Air samples were collected with poly(dimethylsiloxane) (PDMS) 100 microm SPME fibers and analyzed by gas chromatography (GC)-flame ionization detection (FID) and GC-MS. Significant reductions of BTEX concentrations were observed. In addition, some products of BTEX-ozone-oxygen reactions were identified. SPME worked well as a rapid sampler for BTEX and BTEX-ozone-oxygen reaction products. No significant deterioration of the PDMS coating and no significant reduction of absorption capacity were observed after repeated exposure to ozone.     

Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for simultaneous determination of chloramphenicol and thiamphenicol in honey

Dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography-variable wavelength detector (HPLC-VWD) was developed for extraction and determination of chloramphenicol (CAP) and thiamphenicol (THA) in honey. In this extraction method, 1.0 mL of acetonitrile (as dispersive solvent) containing 30 μL 1,1,2,2-tetrachloroethane (as extraction solution) was rapidly injected by syringe into a 5.00-mL water sample containing the analytes, thereby forming a cloudy solution. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by HPLC-VWD. Some important parameters, such as the nature and volume of extraction solvent and dispersive solvent, extraction time, sample solution pH, sample volume and salt effect were investigated and optimized. Under the optimum extraction condition, the method yields a linear calibration curve in the concentration range from 3 to 2000 μg kg⁻¹ for target analytes. The enrichment factors for CAP and THA were 68.2 and 87.9, and the limits of detection (S/N = 3) were 0.6 and 0.1 μg kg⁻¹, respectively. The relative standard deviations (RSDs) for the extraction of 10 μg kg⁻¹ of CAP and THA were 4.3% and 6.2% (n = 6). The main advantages of DLLME-HPLC method are simplicity of operation, rapidity, low cost, high enrichment factor, high recovery, good repeatability and extraction solvent volume at microliter level. Honey samples were successfully analyzed using the proposed method.     

Analytical methods applied to the determination of pesticide residues in foods of animal origin. A review of the past two decades

Pesticides are widely used in agriculture and can be transferred to animals in a number of ways. Consequently, reliable analytical methods are required to determine pesticide residues in foods of animal origin. The present review covers published methods and research articles (1990-2010) in which pesticide residues have been extracted from meat and meat products, milk and dairy products, fish and seafood, and eggs, then cleaned up, and isolated by chromatographic techniques to be identified and quantified by various detection methods. Recovery rates, quantification limits, the matrix effect and related parameters have all been considered. Lastly, future developments in this field are outlined.     

碳纳米管在样品前处理中的应用

碳纳米管是一维碳基纳米材料,具有独特的管状结构、良好的化学稳定性、热稳定性和高比表面积.近年来,碳纳米管在有机小分子、金属离子和生物大分子分离富集方面得到了广泛的应用.本文综述了碳纳米管及功能化碳纳米管在固相萃取、固相微萃取、中空纤维膜保护固相微萃取和液膜萃取等样品前处理技术中的应用.