Spectrophotometric determination of ferbam (iron(III) dimethyldithiocarbamate) in commercial sample and wheat grains using 4,7-diphenyl-1,10-phenanthroline after extraction into mesityl oxide

A procedure has been developed for the determination of iron(III) dimethyldithiocarbamate by converting it into iron(II)-bathophenanthroline complex, which is then extracted into mesityl oxide in the presence of potassium perchlorate. The absorbance is then measured at 534 nm against a reagent blank. Beer's law is obeyed over the concentration range 0.5-20 microg ml(-1) in the final solution. The method is sensitive, highly selective and can be used for the determination of ferbam in a commercial sample, and in mixtures with various dithiocarbamates (ziram, zineb, maneb, etc.) and in wheat grains.     

Preparation of a highly sensitive enzyme electrode using gold nanoparticles for measurement of pesticides at the ppt level

A highly sensitive enzyme electrode was prepared based on gold nanoparticles for measurement of pesticides. Gold nanoparticles of 25-30 nm were synthesized on a glassy carbon electrode by double-pulse technique while the coverage was controlled by applied potential and time. The gold nanoparticles were modified to form a self-assembled monolayer, followed by covalent binding of tyrosinase. The TYR-AuNP-GC electrode was compared with bare GC, AuNP-GC, and modified AuNP-GC and TYR-Au (plate type) electrodes in terms of cyclic voltammetry. The voltammograms well represent the sensitivity of enzymatic oxidation of catechol, substrates for the enzyme activity. The prepared electrode integrated into a continuous flow system and was tested to detect pesticides, such as 2,4-D, atrazine, and ziram. Under the optimized conditions of the flow system, the electrode performed reasonably according to the inhibition mechanism in the concentration range of 0.001-0.5 ng mL(-1). The enhanced performance was attributed to the favored microenvironment for the enzyme activity provided by SAM on gold nanoparticles.     

Extractive Spectrofluorometric Determination of Quinalphos Using Fluorescein in Environmental Samples

A simple, sensitive, convenient and low cost spectrofluorometric technique for determination of quinalphos is described. Quinalphos is decomposed with sodium ethoxide. Resultant sodium diethyl thiophosphate (Na-DETP) is extracted with a cationic fluorescein as ion pair complex into 1-chloro-2-nitrobenzene. The fluorescence of the ion pair, fluorescein-DETP is measured at 530 nm after excitation at 490 nm. This technique is applicable for the determination of quinalphos in water, food grains and vegetable samples up to ng level with Amberlite XAD-4.     

Advances in the determination of inorganic ions in potable waters by ion chromatography

Ion chromatography (IC) is now a well-established methodology for the analysis of ionic species. The technique is applicable to the determination of a wide range of solutes in many sample types, although the determination of inorganic ions in potable waters continues to be the most widely used application of ion chromatography. Many standardization and regulatory bodies, such as the American Society for Testing and Materials (ASTM), International Organization for Standardization (ISO), and US Environmental Protection Agency (EPA), have approved methods of analysis based upon IC, most of which have been published within the last decade. Recent developments in the field of IC, such as the use of higher capacity columns, larger loop injections, more complex sample preparation and detection schemes, have been incorporated into these new approved methods. These advances allow the determination of environmentally significant contaminants, such as common inorganic anions, bromate, perchlorate and chromate, at trace levels in potable waters using ion chromatography.     

水中硫化物突发性污染事故应急监测方法研究

水中硫化物不稳定,最好是现场即时测定。本文旨在研究现场快速测定水中的硫化物。本研究运用比色分析的朗伯-比尔定律和真空工艺设计,将复杂繁琐的实验室测试方法和操作程序有机的融合在测试管中。该测试管具有快速、简便和价格低廉等特点,测定范围0.1～10mg/L。     

8-羟基喹哪啶固相萃取光度法测定生物样品中的钴

研究了8-羟基喹哪啶与钴的显色反应,在pH为8.0的氯化铵—氨水缓冲介质中,乳化剂-OP存在下,8-羟基喹哪啶与钴反应生成3∶1稳定的蓝紫色配合物,该配合物可被Waters Plus-C18固相萃取小柱萃取富集,小柱上富集的配合物用乙醇为洗脱剂洗脱后用光度法测定,在乙醇介质中,配合物最大吸收波长λmax为595 nm,ε为7.82×103L.mol-1.cm-1。钴含量在0.1~5.0 mg/L内符合比耳定律,方法用于生物样品中痕量钴的测定,结果令人满意。     

Determination of ethanolamine,ethylene glycol and triethylene glycol by ion chromatography for laboratory and field biodegradation studies

The determination of alkanolamines and glycols in groundwater and subsurface environments is essential for environmental assessment, remediation and monitoring for selected industrial sites. Monoethanolamine (MEA), ammonium, sodium, magnesium and calcium detection was performed using cation exchange chromatography (IC) with suppressed conductivity detection. Acetate, chloride, nitrite, nitrate, phosphate, sulfate and oxalate were monitored employing anion exchange chromatography with suppressed conductivity. Detection of ethylene glycol (MEG) and triethylene glycol (TEG) and ethanol was carried out using ion exclusion chromatography with pulsed amperometric detection. Effective determination of MEA, MEG and TEG in complex groundwater matrices without compound transformation offered improved monitoring capabilities. This study presents robust analytical tools for MEA, MEG and TEG determination in biodegradation studies. Using ion chromatography offered significant advantages for the analyses of groundwater samples and laboratory bioreactor monitoring.     

Interlaboratory comparability of copper complexation capacity determination in natural waters

The results of a test of interlaboratory comparability for the determination of copper complexation capacity and copper-ligand complex formation constant are presented. Eight water samples comprising, six natural waters, a synthetic ligand solution and a blank solution were analysed by seven laboratories using their own methods of complexation titration. Given the wide variation that might have been possible, relatively good comparability was demonstrated amongst the variety of methods for determining copper complexation capacity. The complexation capacity data largely satisfied the predefined criterion of agreement to within 50%. This provides support for the use of metal speciation criteria in the regulation of copper in the environment. Data for the determination of complex formation constants were of poorer comparability, ranging between 10(7) and 10(12) for the same water.     

Comparison study of five analytical methods for the fractionation and subsequent determination of aluminium in natural water samples

Five methods for aluminium fractionation used in different laboratories in Norway and Finland were compared using six control, 75 soil water and 10 lake water samples. Different fractionation principles [cation exchange, formation of the Pyrocatechol Violet (PCV) or quinolin-8-ol (oxine) complex], types of cation exchanger [Amberlite (Na/H) or Bond Elut (H)], reaction time (from 2.3 s), flow systems (flow injection analysis or segmented flow) and determination principles (molecular absorption spectrometry or ICP-AES) were tested. Determination of the 'labile' fraction was strongly dependent on the method used and the largest differences were observed between the ICP-AES method with cation exchange (Bond Elut H form) and the 'quickly reacting' method (oxine, 2.3 s). Different flow systems, both using cation exchange and determination of the PCV complex but with different reaction times and an extra acidification step, resulted in large differences in the 'reactive' and 'non-labile' fractions determined. However, the determination of the labile fraction gave similar results with both these methods. The two different types of cation exchanger used (with and without pH buffering and with different counter ions) in the ICP-AES methods resulted in differences, mainly because of a smaller 'non-labile' fraction in the non-buffered system. The two flow injection systems (oxine and PCV complexation) showed common trends, which may be connected with the short reaction times used. Comparison with theoretical equilibrium calculations using the model ALCHEMI suggested that the best correlation for the determination of the 'labile' fraction were obtained with the ICP-AES method with an Amberlite column.     

催化分光光度法测定环境样品中微量碘

本文介绍一个简单而灵敏的催化分光光度法,用于测定环境样品中微量碘,本法系基于亚硝酸根存在时微量碘离子催化还原硫氰酸铁络含物,并以分光光度计测量该红色络合物的减弱强度,在一定温度时,该络合物的分解速度正比于磺的含量.在给定的实验条件下,磺离子的浓度在0.001-0.024毫克/升之间服从比尔定律. 本法已成功地应用于天然水、土壤、海底泥和海生物中微量磺的测定,结果良好.     

Biofilms coating Schoenoplectus californicus as indicators of water quality in the Río de la Plata Estuary (Argentina)

N-ethyl-3-carbazolecarboxaldehyde-3-thio- semicarbazone (ECCT) as an new analytical reagent used for the development of a highly sensitive extractive spectrophotometric method for the determination of copper(II). The ECCT forms a greenish-yellow colored 1:1 (M:L) complex with copper(II) at pH 3.0, which is well extracted into n-butanol and shows maximum absorbance at 380nm. The color of the complex is stable for more than forty eight hours. The system obey Beer's law in the range 0.4–3.6 with 2.243 × 10⁴lmol⁻¹cm⁻¹, 2.83 × 10^-3μgcm⁻² molar absorptivity and Sandell's sensitivity respectively. The regression coefficient is 0.412 with 0.99 correlation coefficient. The precision and accuracy of the method was checked by finding the relative standard deviation (0.422%). This developed method has been successfully employed for the determination of copper(II) in environmental and pharmaceutical samples. The method is evaluated by analyzing samples from the bureau of analyzed samples (BCS 233, 266, 216/1, 207 and 179) and by inter comparison of experimental values using AAS.     

Spectrophotometric determination of platinum(IV) in alloys, complexes, environmental, and pharmaceutical samples using 4-[N,N-(diethyl)amino] benzaldehyde thiosemicarbazone

4-[N,N-(Diethyl)amino] benzaldehyde thiosemicarbazone (DEABT) is proposed as an analytical reagent for the spectrophotometric determination of platinum(IV). The DEABT forms 1:2 yellow complex with Pt(IV), which is sparingly soluble in water and completely soluble in water–ethanol–DMF medium. The Pt(IV)–DEABT complex shows maximum absorbance at 405 nm. Beer’s law is valid up to 7.80 μg cm^???3, and optimum concentration range for the determination of platinum(IV) is 0.48–7.02 μg cm^???3. The molar absorptivity and Sandell’s sensitivity of the method are found to be 1.755 × 10⁴ dm³ mol^???1 cm^???1 and 0.0012 μg cm^???2, respectively. The relative error and coefficient of variation (n?=?6) for the method does not exceed ±0.43% and 0.35%, respectively. Since the method tolerates a number of metal ions commonly associated with platinum, it can be employed for the determination of platinum in environmental samples, pharmaceutical samples, alloys, catalysts, and complexes. The method is rapid as the Pt(IV)–DEABT complex is soluble in water–ethanol–DMF medium and not requiring any time consuming extraction method for the complex.     

Simultaneous Determination of O- and P- Nitrophenol by First Derivative Spectrophotometry

A simple method by first derivative spectrophotometry is proposed for the simultaneous determination of o-nitrophenol and p-nitrophenol. The analytes were separated from samples by liquid-liquid extraction (pH = 7.4) as tetrabutylammonium ion pairs into the 1,2-dichloroethane organic phase and subsequently the extracts were evaluated directly by derivative spectrophotometry. Simultaneous determination of both analytes could be carried out using the zero-crossing and the graphical methods for o-nitrophenol and p-nitrophenol, respectively. The determination ranges were found to be between 0.115 to 3.00 ppm and 0.130 to 3.00 ppm for o-nitrophenol and p-nitrophenol, respectively. The relative standard deviations were in all instances less than 2.0%. The proposed method was applied to the determination of these compounds in fruit juices.     

饮用水源水中水合肼测定的注意事项及解决方法

对国标法( GB/T 5750.8-2006)中的二甲氨基苯甲醛分光光度法测定饮用水源水中水合肼进行了深入研究,同时指出了水合肼测定全过程中应注意的问题及解决方法.指出在标准分析方法基础上,选用合格的最新生产的分析纯以上的试剂,现场调节水样酸度至1 mol/L,正确进行浑浊带色干扰因素校正消除,利用氨基磺酸去除亚硝酸盐...     

The sensitive and selective determination of aluminium by spectrofluorimetric detection after complexation with N-o-vanillidine-2-amino-p-cresol

A simple, easy to use and selective spectrofluorimetric method for the determination of trace levels of aluminium has been developed. A new Schiff base, N-o-vanillidine-2-amino-p-cresol (OVAC), has been synthesized and its fluorescence activity with aluminium investigated. Based on this chelation reaction, a spectrofluorimetric method has been developed for the determination of aluminium in samples buffered at pH 4.0 using acetic acid-sodium acetate. The chelation reaction between Al(iii) and N-o-vanillidine-2-amino-p-cresol was very fast, requiring only 20 min at room temperature to complex completely. The excitation and emission wavelengths were 423.0 and 553.0 nm, respectively, at which the OVAC-Al complex gave the maximum fluorescence intensity at pH 4.0 in a 50% ethanol-50% water medium. The interference from fluoride ions was minimized by the addition of Be(2+). Other ions were found not to interfere at the concentrations likely to be found in natural waters. Under these conditions, the calibration plot was linear up to 1000 microg L(-1) (r = 0.999). The limit of detection (3sigma) for the determination of Al(iii) was 0.19 microg L(-1) and the precision for multiple determinations of 3 ng mL(-1) Al(iii) prepared in ultra-pure water was found to be 0.29% (n = 16). The Schiff base ligand could be used to determine ultra-trace aluminium from natural waters. Analysis of environmental certified reference materials showed good agreement with the certified values. The procedure was found to be equally applicable to both fresh water and saline solutions (including sea water) using either normal external calibration or the standard additions method.     

土壤中多氯联苯简化计算定量方法研究

针对含有两种或两种以上Aroclor多氯联苯混合物的样品,研究其简便易行的定性、定量方法。将复杂样品中的多氯联苯分别折算成Aroclor 1016、1242、1260含量,在定性的同时予以定量。3种不同组分混合样品的加标回收率分别为68.2%～80.6%、67.9%～74.2%、67.1%～76.8%,实际土壤样品的测定结果与已有研究结果相吻合。方法缺点为无法识别和计算各Aroclor之间的准确比例,可用于应急监测复杂组分样品中多氯联苯的测定。     

水中汞监测存在的问题与解决办法

利用中日合作 (JICA)项目资金 ,对测定地表水中汞存在的主要问题 ,如水样的保存和处理 ,水样的消解 ,测汞的冷原子吸收法和原子荧光法等进行了研究。通过对 33个环境监测站的样品考核 ,发现测定结果与标准值相比 ,偏高的数据达 75 %以上。提出了用 1%H2 SO4 和 0 1%K2 Cr2 O7保存水样最好 ;高锰酸钾 -过硫酸钾消解法适用于消解含有机物、悬浮物和组成复杂的废水样 ,高锰酸钾 -硫酸消解法适用于消解被有机物轻度污染的废水 ,溴酸钾 -溴化钾消解法适用于消解地表水和含较少有机物的生活污水及工业废水。研究表明 :尤以硫酸 -高锰酸钾 -过硫酸钾消解体系消解地表水和废水效果良好。对冷原子吸收法和原子荧光法中影响汞测定的因素 ,如空白值高、干扰物的消除、载气种类和流量、反应瓶体积和气液比以及反应时间等提出了详尽的解决方法     

Ecological mapping: A framework for delimiting forest management units

Ecological mapping attempts to objectively and spatially delimit and represent the natural organization and structure of the landscape. It offers nested levels of resolution, based upon a regionalization process, and provides an ecological basis for planning activities that may impact upon the environment.The essential principles of ecological mapping, as applied by the Quebec Ministry of Environment and Wildlife, are summarized. A methodological mapping approach is proposed for the determination of significant land portions for forest management using an ecological map at a scale of 1:50 000. At this scale, two nested levels of perception are expressed: 1) the topographic complex, and 2) the topographic entity. The topographic entity can be further subdivided into working units based upon operational criteria oriented to forest management. Within each nested level from topographic complex to working unit, there is a corresponding increase in the amount of detailed information available. Ecological mapping undertaken at 1:50 000 scale can provide a reliable and robust tool for planning forest management activities. In most cases, major ecological variations can be expressed and mapped at this scale; however, a greater degree of generalization must be accepted in the planning process when working at this scale rather than at larger scales.     

灰霾天气城市空气污染程度判据指标体系建立的探讨

灰霾天气加重空气污染程度,是空气污染呈现区域性、复合型污染的重要天气污染现象,对视觉空气质量以及人体健康造成很大影响与危害.针对灰霾天气下城市空气污染加重程度判据系统建立,对灰霾天气下空气污染程度评估方法及建立污染程度与能见度量化相关关系进行了初步探讨.     

超声提取-离子色谱法测定常见土壤中的高氯酸盐

建立了测定土壤中高氯酸盐的离子色谱法,通过前处理条件优化和色谱条件优化形成准确高效的测定方法,并采集实际土壤样品进行实验验证。称取 1.00 g土壤样品,用20 mL超纯水混合均匀,超声提取40 min,离心后采用水系微孔滤膜过滤的前处理方式,土壤中高氯酸盐的加标回收率最稳定;在淋洗液浓度和流速都满足测定条件的前提下,为了缩短高氯酸盐的保留时间,避免复杂基质干扰,延长淋洗液发生器的使用寿命以及保护色谱柱,选择淋洗液浓度为40 mmol/L,流速为1.0 mL/min。在优化条件下,高氯酸盐的方法检出限为0.04 mg/kg。实际样品加标中高氯酸盐的相对标准偏差为1.9%~8.8%,加标回收率为91.0%~106%,结果表明离子色谱法测定土壤中高氯酸盐简单、灵敏、快速。