Development and validation of methods for the trace determination of phthalates in sludge and vegetables

A routine method which is simple, quick and precise has been set up and validated for phthalate analysis in environmental samples (tomato plants and sewage sludges). Six phthalates have been studied simultaneously: dimethylphthalate, diethylphthalate, di-n-butylphthalate, n-butylbenzylphthalate, di-2-ethyl-hexyl phthalate (DEHP) and di-n-octylphthalate. Optimization of sample, solvent extraction uses a Soxtec apparatus and extract purification with an a solid-phase extraction cartridge allows between 90 and 110% recovery of phthalates. Precise, sensitive and selective identification and quantifying of analytes is by GC-MS in the single ion monitoring mode. This protocol allows analytes with concentrations as low as 10 microg/kg dry matter (DM) to be determined from small (1-2 g DM) samples. This analytical method has been applied to the phthalate transfer study for agricultural recycling of sludges, where phthalate bioavailability has been studied in aquiculture using two types of experiments. Tomatoes have been grown in containers where the trace organics have been directly introduced as pure substances, and in a second experiment under the same growth conditions, sewage sludge has replaced the pure substances. Transfer of these trace organics has been followed into the various parts of the tomato plant and in general only the DEHP is worthy of note although its percentage transfer remains very low even in an experiment designed to maximize this.     

超临界流体萃取仪器的研制

本文报道了以国产原配件为基础，成功地研制了分析规模的超临界流体萃取仪器、并对仪器性能进行了全面考察，仪器性能稳定，重现性良好（ＲＳＤ＜３．１％），定量线性关系可靠，可满足定量萃取的要求。     

The detection of formaldehyde in textiles using interdigitated microelectrode array diffusion layer titration with electrogenerated hypobromite

An interdigitated microelectrode array (IDA) was applied to the determination of formaldehyde released from textiles produced in industry. The proposed method is based on formaldehyde reaction with hypobromite which is formed in weakly basic media by control current electrooxidation of bromide on the generator segment of the IDA array. The unreacted hypobromite diffuses through the gap between individually polarisable IDA segments and it is amperometrically detected on the collector segment of the IDA. The efficiency of this nonconvective transfer process in the absence of formaldehyde was substantially higher (78%) in comparison with that when using the rotating ring disc electrode. The influence of the added formaldehyde on the transfer process can be utilised to develop a simple and sensitive analytical procedure for formaldehyde detection with a detection limit of 4×10⁻⁶ mol dm⁻³.     

Ion-exchange method for separation and concentration of platinum and palladium for analysis of environmental samples by inductively coupled plasma atomic emission spectrometry

An ion-exchange procedure is proposed for determination of Pt and Pd in environmental samples, using a Dowex 1-X10 anion-exchange resin. Pt and Pd were separated from the matrix elements in the sample by selective retention on the column as anionic chloro complexes and subsequent elution by circulated thiourea at 60 °C. The eluent, containing Pt and Pd was analyzed by inductively coupled plasma (ICP) atomic emission spectrometry (AES). Average recoveries of 98% and detection limit of 15 ng/g for both metals were achieved. Analysis of Pt and Pd concentrations in road dust, sampled from several sites in Germany was performed. The comparison of the obtained data with the concentrations of Pt and Pd in the same samples, determined by ICP-MS showed a very good agreement.     

Monitoring nitrite with optical sensing films

A new, low-cost nitrite sensor was developed by immobilizing a direct indicator dye in an optical sensing film for food and environmental monitoring. This sensor was fabricated by binding Safranine O to a cellulose acetate film that had previously been subjected to an exhaustive base hydrolysis. The membrane has good durability (>12 months) and a short response time (<8 s). Nitrite can be determined for the range of 0.005-2.00 μg ml⁻¹ with 3δ detection limits of 0.001 μg ml⁻¹. The method is easy to perform and uses acetylcellulose as a carrier. The reagents used for the activity of the cellulose support are inexpensive, non-toxic and widely available.     

The European Eco-Management and Audit Scheme Accreditation – an overview

 Environmental quality is still deteriorating in the EU and worldwide despite all the Directives and Regulations in this field over the past 20 years. The European Community has devised a new approach to this problem with the introduction of the Eco-Management and Audit Scheme Regulation. This Regulation provides industry with an opportunity to demonstrate that it can achieve continuous improvement in its environmental performance through a voluntary scheme which is not based on the traditional command and control mechanisms of Directives. This paper gives an overview of the steps involved in implementing the European Eco-Management and Audit Scheme and the role of accreditation in supporting the scheme.     

Simultaneous determination of traces of heavy metals by solid-phase spectrophotometry

A coupling sensitive solid phase spectrophotometric (SPS) procedure for determination of traces of heavy metals (Me-SPS) and multicomponent analysis by multiple linear regressions (MA), a simple methodology for simultaneous determination of metals in mixtures was inaugurated. The Me-SPS procedure is based on sorption of heavy metals on PAN-resin and direct absorbance measurements of colour product Me-PAN sorbed on a solid carrier in a 1-mm cell. This methodology (Me-SPS-MA) was checked by simultaneous determination of metals in synthetic mixtures with different compositions and contents of metals important in pharmaceutical practice: Zn, Pb, Cd, Cu, Co, and Ni. Good agreement between experimental and theoretical amounts of heavy metals is obtained from the recovery test (78.3–110.0%). The proposed method enables determination of particular metal ion at the ng mL⁻¹ level and it was successfully applied to the determination impurities from heavy metal traces in pharmaceutical substances (Cu in ascorbic acid, Pb in glucose, and Zn in insulin). The proposed procedure could be possible contribution to the development of pharmacopoeial methodology for a heavy metals test.     

微量元素锌在治疗Bell麻痹中的作用

为探讨急性早期应用补锌和综合疗法治疗Bell麻痹 ,将 1 5 8例Bell麻痹患者 ,随机分成两组 :(1 )补锌组 (补锌 +综合疗法 ) ;(2 )对照组 (单纯综合疗法 )。对其进行了观察对比治疗 ,同时检测了所有患者治疗前后自身对照发锌值 ,还对所有患者进行了定位诊断、面神经电反应测试、并对面肌功能进行评分。结果表明 ,对定位诊断其病变在D段、面肌功能评分在 1 1分以下、面神经无电反应患者 ,即使给予早期综合治疗 ,效果仍较差 ,而早期给予补锌加综合治疗效果优于对照组 ,其它段内患者治疗次数和治愈天数也均优于对照组。可见微量元素锌在发挥免疫应答、免疫调控中的重要作用     

Automated at-line solid-phase extraction-gas chromatographic analysis of micropollutants in water using the PrepStation

A fully automated at-line solid-phase extraction-gas chromatography procedure has been developed for the analysis of aqueous samples using the PrepStation. The sample extract is transferred from the sample preparation module to the gas chromatograph via an autosampler vial. With flame-ionization detection, limits of determination (S/N=10) of 0.05–0.13 μg/l were obtained for the analysis of HPLC-grade water when modifying the PrepStation by: (i) increasing the sample volume to 50 ml, (ii) increasing the injection volume up to 50 μl, and (iii) decreasing the desorption volume to 300 μl. The HP autosampler had to be modified to enable the automated “at-once” on-column injection of up to 50 μl of sample extract. The amount of packing material in the original cartridge had to be reduced to effect the decrease of the desorption volume. The total set-up did not require any further optimization after having set up the method once. The analytical characteristics of the organonitrogen and organophosphorus test analytes, i.e. recoveries (typically 75–105%), repeatability (2–8%) and linearity (0.09–3.0 μg/l) were satisfactory. The potential of the system was demonstrated by determining triazines and organophosphorus pesticides in river Rhine water at the 0.6 μg/l level using flame-ionization and mass-selective detection. No practical problems were observed during the analysis of more than 100 river water samples.     

Boundary scan test,test methodology,and fault modeling

The test technique called boundary scan test (BST) offers new opportunities in testing but confronts users with new problems too. The implementation of BST in a chip has become an IEEE standard and users on board level are the next group to begin thinking about using the new possibilities. This article addresses some of the questions about changes in board-level testing and fault diagnosis. The fault model itself is also affected by using BST. Trivial items are extended with more sophisticated details in order to complete the fault model. Finally, BST appears to be a test technique that offers a high degree of detectability on board level, but for diagnosis, some additional effort has to be made.