Analytical chemistry of chlorpyrifos and diuron in aquatic ecosystems

The chemistry and toxicology of chlorpyrifos and diuron are presented. These compounds represent the extremes of pesticide use both in terms of toxicity and chemistry. Methods used for their determination are reviewed with an emphasis on recent developments in sample preparation and quantification.     

Determination of mercury and organic mercury contents in Malaysian seafood

The contents of mercury and organic mercury in various types of seafood from various location in Malaysia were determined by neutron activation analysis. Total mercury was determined by instrumental neutron activation analysis (INAA) whilst organic mercury was determined by INAA after chemical separation. Samples were digested in acid media and into the solution was added copper ion and KBr to release organic mercury compound from sulphur component of the tissue. The organic mercury was then extracted into toluene and then treated with cysteine paper to convert the compound into sub-organo-mercury from. The paper was then transferred into polyethylene vials and irradiated in the MINT TRIGA Reactor. Analytical results of organic mercury in Indian mackerel (Rastrelliger kanagurta), Spanish mackerel (Scomberomurus commersoni), shrimp (Peneaus sp.), squid (Loligo sp.) and cockle (Anadara granosa) is in the range of 45%–94% of the total mercury.     

Determination of mercury and mercury compounds in air and other non-corrosive gases

Summary Mercury is adsorbed on cellulose powder and activated charcoal. The contents of the adsorber are burnt in the oxy-hydrogen flame, and the mercury determined by the flameless atomic absorption procedure. The method is applicable to mercury present as metallic vapour, organo mercurical compounds and particulate matter containing adsorbed mercury compounds. The combustion step eliminates all possible non-atomic absorption interferences in the measuring procedure and ensures quantitative recovery of the mercury from the adsorption material.Quantitative adsorption recovery over a wide range of flow rate from 2–200 l/h allows the use of small battery operated pumps for personal monitoring, or vacuum pumps for high speed and large volume sampling. The range of flow rate makes isokinetic sampling conditions possible.

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Bestimmung von Quecksilber und Quecksilberverbindungen in Luft und anderen nicht korrodierenden Gasen

Zusammenfassung Quecksilber wird an Cellulosepulver und Aktivkohle adsorbiert. Der Inhalt des Adsorbers wird in der Wasserstoff-Sauerstoff-Flamme verbrannt und das Quecksilber durch flammenlose Atomabsorption bestimmt. Die Methode erfa\t Quecksilber als Metalldampf, in Form von Organo-Quecksilberverbindungen sowie Quecksilberverbindungen, die an Staubpartikel adsorbiert sind. Die Verbrennung in der Wasserstoff-Sauerstoff-Flamme eliminiert Störungen durch nicht-atomare Absorption bei der AAS-Messung und garantiert die quantitative Erfassung des adsorbierten Quecksilbers.Die quantitative Adsorption über einen gro\en Bereich der Durchflu\geschwindigkeit von 2–200 l/h erlaubt batteriebetriebene Pumpen für die Quecksilbermessung am Mann, oder den Einsatz von Vakuumpumpen für die Probenahme bei hoher Durchflu\rate und gro\em Probenvolumen. Der gro\e Bereich der Durchflu\rate gestattet isokinetische Bedingungen für die Probenahme.

     

分光光度法测定矿渣中的汞

采用酚藏花红分光光度法测定矿渣中的微量汞,对反应条件进行了实验及优化,得最佳测定条件为:测定波长535 nm,H2SO4浓度为3.0 mol/L,NaBr浓度为0.02 mol/L,并且在室内漫射光条件下,溴汞酸-酚藏花红缔合物在溶剂中的稳定时间为120 min之内,汞含量在0～20μg/mL范围内服从比尔定律,检出限为1.09×10-3μg/mL。该条件下测得矿渣中的汞含量为2.5μg/g,加标回收率在97.95%～98.57%之间,测得其相对标准偏差(n=6)≤3.0%。该方法可用于矿渣中微量汞的测定。     

Determination of small amounts of mercury

A number of methods for the determination of trace amounts of mercury are reviewed with emphasis on sensitivity and ease of application.     

Determination of volatile mercury compounds in air with the coleman mercury analyzer system

A simple but very selective cold-vapour atomic absorption system is described for the determination of volatile mercury compounds at very low levels in ambient air. Three different absorbers are compared: activated charcoal, silver-coated sea sand and gold-coated sea sand. To eliminate interferences, a two-step desorption unit is used. After thermal desorption, the mercury is measured by using a modified MAS-50 spectrophotometer. The effects of flow rate and desorption temperature are discussed. The detection limit is 0.1 ng. Above 1 ng, the reproducibility is about 1%. Calibration is done by injection of elemental mercury vapour. The method with gold-coated sand absorbers is most satisfactory and is suitable for the analysis of ambient outdoor and indoor air. All likely volatile mercury compounds are absorbed, and a wide range of mercury concentrations can be determined. In routine application, one analysis takes about 3 min.     

Determination of total particulate mercury in air with the coleman mercury analyzer system

A simple and rapid cold-vapour atomic absorption system is described for the simultaneous determination of low ambient levels of particulate mercury and volatile mercury compounds. Of the different filters checked for particle collection, quartz fibre filters have the best properties. Sampling characteristics were considered with respect to efficiency, reproducibility and duration of sampling. The homogeneity of the solid mercury deposit on the filter was tested. Possible enrichment during sampling by absorption of volatile mercury compounds and possible mercury losses by volatilization of solid compounds were examined. After sampling the mercury is released by pyrolysis and collected on a gold-coated sand absorber. In order to avoid deactivation of the absorber by condensation of pyrolysis products or interference during the subsequent dcsorption and atomic absorption measurement of the collected mercury, a heated catalytic convertor and two specific absorbers for organic substances are inserted in the analysis line.     

Determination of mercury in urine of Mexican dentists

Mercury levels in the urine of Mexican dentists were determined by instrumental neutron activation analysis. A control group with no suspicion of contamination by mercury was also studied. Acid digestion was used for samples treatment and the presence of ²⁰³Hg was determined by gamma spectroscopy. The ranges of mercury concentration found in urine were: for the dentists group from 0.19 to 11.56 mg Hg/l, with a mean value of 3.16 mg Hg/l and standard deviation of 2.74 mg Hg/l, and for the control group from 0.03 to 0.05 mg Hg/l with a mean value of 0.04 mg Hg/l and standard deviation of 0.01 mg Hg/l. The mercury levels found in urine of dentists are associated with several exposure factors which appear to be positively correlated to its concentration, such as years of dental practice, amalgamation techniques, etc.     

Determination of mercury by radiochemical displacement

2–15 g of mercury has been determined by exchange with zinc in⁶⁵Zn labelled zinc sulphide. The influence of various ions which are likely to interfere in the determination of mercury has also been studied.     

Determination of mercury by atomic-absorption spectrophotometry

A flameless atomic-absorption system has been developed for the determination of low concentrations of mercury in gaseous, solid and liquid samples of organic and inorganic materials.     

固体进样直接测定法测定铜精矿中汞

建立了固体进样直接测定法测定铜精矿中汞含量的方法。铜精矿样品在测汞仪的分解炉中经300℃干燥和750℃高温热分解后,汞被催化分解为汞原子,于850℃齐化成金汞齐。汞蒸气被氧气流带入单波长光学吸收池,在波长253.7 nm处测量汞的吸光度,采用标准曲线法计算汞量。方法的线性范围分别为0~1.00,0~100μg/mL,线性相关系数为0.9999,检出限分别为0.10,0.04 ng/g。5个汞含量不同的铜精矿样品测定结果的相对标准偏差为2.14%~4.35%(n=11),样品加标回收率为92.00%~104.02%。采用该方法分别对2个铜精矿样品和铜精矿国际标准物质进行测定,测定结果与标准分析方法测定值和标准物质标示值基本一致。该方法简便、快速、准确,可以作为标准方法推广使用。     

Determination of trace amounts of mercury in rock samples

Summary A precise and accurate method is described for the measurement of ng quantities of mercury in inorganic samples such as rock, mineral ores and soil. The mercury is distilled from pulverized samples and collected on a silver gauze absorber. The mercury is then rapidly desorbed from the silver element using heat, and it is carried by gas entrainment into the measuring cell of an ultraviolet absorption analyzer. Readout of the mercury content can be made by measurement of peak heights on a strip chart recording, but more elegantly and accurately by the digital printout from a GC integrator. Calibration of the instrumental assembly, by injection of measured quantities of saturated mercury vapor, is simple, rapid and accurate.

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Zusammenfassung Eine genaue Methode zur Bestimmung von Nanogrammengen Quecksilber in anorganischem Material wie Gesteinen, Erzen und Bodenproben wurde beschrieben. Aus den gepulverten Proben wird das Hg abdestilliert und auf einem Silberdrahtnetz gesammelt. Dann wird es rasch durch Erwärmen desorbiert und mit einem Gasstrom in die Meßzelle eines UV-Ab-sorptionsgerätes geleitet. Die Ermittlung des Quecksilbergehaltes kann aus der Peakhöhe eines Schreibers, besser mit dem Digitalzähler eines GC-Integrators erfolgen. Die Eichung des Gerätes durch Einleiten gemessener Mengen von gesättigtem Quecksilberdampf ist einfach rasch und genau.

     

Determination of mercury by radiochemical displacement method

A radiochemical displacement method for the determination of micro amounts of Hg(II) has been developed. 65Zn was displaced from the Zn-1-(2-pyridylazo-2-naphthol) complex at pH 5 in borate buffers by Hg (II). 10-80 micrograms of mercury could be determined. Interference of various metal ions and methods for suppression have also been carried out.     

Determination of cobalt on surfactant-modified mercury electrodes

Cobalt ions can be determined in the presence of interfering matrix components such as zinc ions by applying adsorbed surfactants. The influence of different adsorption layers on the reduction processes of both ions was studied. Selective inhibition of the zinc signal was achieved even with an extremely large zinc(II) to cobalt(II) ratio in solutions such as zinc plating baths after modification of the mercury electrode with adsorbed tetrabutylammonium. The influence of additions of dimethylglyoxime and citrate and pH changes on the cobalt signal was investigated.     

Determination of phenylmercuric compounds and total mercury in paints

Summary A quick method has been developed for the analysis of phenylmercuric compounds and total mercury in paints.

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Zusammenfassung Es wird eine Methode zur schnellen Bestimmung von Phenylquecksilberverbindungen und Gesamtquecksilber in Anstrichmitteln beschrieben.