Automated derivatization for on-line solid-phase extraction-gas chromatography; phenolic compounds

An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1–12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1–0.3 μg/1 range.     

Determination of anions in rainwater by capillary electrophoresis with conductivity detection

A routine method for the determination of chloride, nitrate and sulfate anions in rainwater by capillary electrophoresis was developed. The system uses an end-column non-suppressed conductivity detector. Linear calibration plots were generated from 0.050 to 20 mg/l, which is the range generally found in wet depositions. Accuracy and precision were evaluated by analyzing certified standards of simulated rainwater and environmental samples, or by comparing CE results with those obtained by IC, the reference technique for anion analysis in wet deposition. The reproducibility of the method was satisfactory except at the lower and upper limits of the analytical range. Sensitivity lay in the range of few μg/l.     

一种自制的蒸馏水器保护装置

本装置由检测、控制、执行、报警和电源五部分组成。检测部分采用了靠正常水位导通的两根信号线。当蒸馏水器在正常运行时遇停水,本装置可立即实现断电保护,同时发出声光报警,有效防止干烧,杜绝事故发生。本装置制作简便,元器件均为市售,成本低廉,性能可靠。     

简便快速的硫化氢测定法

本文提出了有一种简易快速测定剂来测定水样中的硫化氢的方法。该法的检出限为０．１ｍｇ／Ｌ，对１．０１ｍｇ／Ｌ的Ｈ２Ｓ样品７次测定的相对标准偏差＜４．１％，１ｈ能测定１２个样品。用本测定了几种水样中的Ｈ２Ｓ含量，回收率为８４％－１０５％。应用它可上标准法的４ｈ左右缩短到５ｍｉｎ；使分析成本降低９／１０；不需配制一系列分析试剂和仪器，只需一支小型塑料管和几片药片，便于渔业水质和环境水质的野外现场监测。     

Quantitative analysis of imazamox herbicide in environmental water samples by capillary electrophoresis electrospray ionization mass spectrometry

Capillary electrophoresis-mass spectrometry (CE-MS) with an electrospray ionization interface was applied for the quantitative analysis of imazamox pesticide in well water, potable water, and pond water. The detector response for imazamox was determined to be linear over the concentration range of 50-1 ng/ml. The limits of quantitation and detection of the method were determined to be 200 and 20 ng/l for imazamox compound in each type of water sample, respectively. The total sample preparation and CE-MS analysis time was under 2 h.     

Suppression of red cell diffusional water permeability by lipophilic solutes

The inhibitory effect of a series of neutral lipophilic solutes (methanol, ethanol, n-propanol, iso-propanol, n-butanol, iso-amylalcohol, n-hexanol, diethylether, nitrobenzene, and pyridine) on the diffusional water permeability (Pd, tot) of bovine erythrocyte membrane at 25 degrees C was studied in comparison to that of p-chloromercuri benzoate (pCMB). Permeability data were obtained by measuring the transmembrane diffusional water exchange time tau(exch) using an 1H-T2 NMR technique. Maximal inhibition by approximately 50% of Pd, tot was produced by 2 mM pCMB which completely blocked the membrane water channels in 20 min, hence suggesting the channel-to-lipid diffusional water permeability ratio of about 1:1. Furthermore, the maximal inhibitory effect of pCMB in combination with the lipophilic solutes was lower than that of pCMB alone. As pCMB does not interfere with the lipid bilayer, and provided that it blocks the water channels in solute presence as well, this confirms that the solutes induce an increase in the lipid-mediated background water permeability contribution (Pd, lipid) by the formation of aqueous leaks in the membrane hydrophobic barrier. However, faster but less efficient in permeability inhibition than pCMB (either alone or combined with solutes) were the lipophilic solutes alone. Taken together, the results indicate that the lipophilic solutes suppress the membrane total permeability Pd, tot by two opposing effects: a reduction of its channel-mediated part (Pd, channel) to the extent exceeding that of a simultaneous Pd, lipid increase. The inhibitory potency of the solutes tested appears to be correlated with their solubility in the membrane medium.     

光度法测定水样中铝

研究了铝与对乙酰基偶氮胂(ASApA)显色反应,在pH 4.7的HOAc-NaOAc缓冲溶液中,Al3+与ASApA显色形成1:2络合物,最大吸收波长位于612 nm,ε-8.19×103L·mol-1·cm-1,铝量在0～2.8μg·ml-1范围内遵守比耳定律,用于水样中铝的测定,结果满意。     

On-line determination of organophosphorus pesticides in water by solid-phase microextraction and gas chromatography with thermionic-selective detection

This paper describes the extraction of 49 organophosphorus pesti-cides (OPPs) from water samples using solid-phase microextraction (SPME). Three fibers, including a 15-μm XAD-coated fiber, a 85-μm polyacrylate-coated fiber, and a 30-μm polydimethylsilox-ane-coated fiber (PDMS), were evaluated here. The effects of stirring and the addition of NaCl to the sample were examined for the polyacrylate-coated fiber. The precision of the technique was examined for all three fibers and the extraction kinetics were investigated using the XAD- and polyacrylate-coated fibers. With some exceptions, the XAD- and polyacrylate-coated fibers performed better than the PDMS-coated fiber. The superiority of the XAD-nd polyacrylate-coated fiber. The superiority of the XAD- and polyacrylate-coated fibers over the PDMS-coated fibers can be attribuibuted to the aromatic functionalities of the XAD and the polar functionalities in the polyacrylate. The relatively high percent RSDs indicate that the SPME technique needs to be further refined before it can be used for anything other than screening. A more effective form of agitation than mechanical stirring may be neccessary to reduce variability and achieve a faster equilibrium between the sample and the SPME fiber.