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摘 要:采用微波消解-石墨炉原子吸收光谱法分析测定食用菌中总砷。取可食部分的食用菌粉碎均匀,采用微波消解对样品进行消解,将消解液于140℃赶酸至0.5mL ,用超纯水转移定容至25mL。以0.1%的硝酸钯为基体改进剂,塞曼扣背景,用石墨炉原子吸收光谱法测定总砷。方法检出限为0.4μg/L,线性范围为0~30 μg/L,线性相关系数(r)大于0.998,采用精密度考察方法重现性,不同浓度水平的RSD%均小于6.6%;三个浓度水平的加标回收率为80.6% ~ 103.9%,有证标准物质测定结果符合要求。实验结果表明,方法操作简便、灵敏、准确,适合食用菌中总砷的测定。对砷形态复杂的野生食用菌,微波消解后可直接采用石墨炉原子吸收光谱法测定总砷。 相似文献
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本文就日本遗弃在华化学武器销毁残渣元素分布进行了分类分析,并对残渣样品的砷形态进行检测。结果表明,黄剂及红剂销毁残渣样品中主要元素均为铁、铜、砷、钛、铅等,其中砷元素占比较大且危害最深。进一步对样品进行分析结果显示,残渣中砷形态主要为Fe-结合态、Ca-结合态、残渣态等。该实验结果为销毁残渣的二次处理提供了必要的技术支撑,在敦促日方改进销毁技术方面具有重要的现实意义。 相似文献
4.
《Journal of separation science》2018,41(7):1524-1531
Nanoliter high‐performance liquid chromatography shows low consumption of solvents and samples, offering one of the best choices for arsenic speciation in precious samples in combination with inuctively coupled plasma mass spectrometry. A systematic investigation on coupling nanoliter high‐performance liquid chromatography to inductively coupled plasma mass spectrometry from instrument design to injected sample volume and mobile phase was performed in this study. Nanoflow mobile phase was delivered by flow splitting using a conventional high‐pressure pump with reuse of mobile phase waste. Dead volume was minimized to 60 nL for the sheathless interface based on the previously developed nanonebulizer. Capillary columns for nanoliter high‐performance liquid chromatography were found to be sensitive to sample loading volume. An apparent difference was also found between the mobile phases for nanoliter and conventional high‐performance liquid chromatography. Baseline separation of arsenite, arsenate, monomethylarsenic, and dimethylarsenic was achieved within 11 min on a 15 cm C18 capillary column and within 12 min on a 25 cm strong anion exchange column. Detection limits of 0.9–1.8 μg/L were obtained with precisions variable in the range of 1.6–4.2%. A good agreement between determined and certified values of a certified reference material of human urine (GBW 09115) validated its accuracy along with good recoveries (87–102%). 相似文献
5.
AbstractAccurate identification and quantification of trace elements and their species in cells is an important prerequisite for the exploration of their physiological function and related mechanisms of process involving trace elements/species in human body. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful analytical instrument for trace elements detection, while it still suffers from insufficient limits of detection, interference from complex cell matrix, and incompatible sample consumption in cells analysis. Microfluidic chips which possess advantages of low sample/reagent consumption, rapid analysis speed and high spatial resolution provide perfect miniaturized and integrated platforms for cell analysis. In this article, microfluidic chip-ICP-MS techniques for trace elements and their species analysis in cells were reviewed. Both chip-based pretreatment techniques (e.g., magnetic solid phase microextraction (MSPME), monolithic capillary microextraction (MCME), liquid phase microextraction (LPME)) including chip-based array microextraction techniques for trace elements and their species analysis and droplet chip for single cell analysis were introduced. The newly developed methods of microfluidic chips in combination with ICP-MS for trace elements and their species analysis in small numbers of cells and even single cell were critically discussed, including chip-based MSPME/MCME/LPME-(electrothermal vaporization-ICP-)MS, on-line chip-based array MSPME/MCME-ICP-MS, on-line chip-based array MSPME-high performance liquid chromatography-ICP-MS and online droplet chip-time-resolved ICP-MS. These methodologies were demonstrated with high sensitivity, high throughput, good matrix resistance and low sample/reagent consumption, contributing to the quantification of trace elements/species in cells and even single cells. Relevant 20 references are included herein, and the development trend of microfluidic chip-ICP-MS techniques for cells analysis is prospected. 相似文献
6.
Shilin Jiang Dr. Yalan Liu Dr. Lin Wang Prof. Zhifang Chai Prof. Wei-Qun Shi 《Chemistry (Weinheim an der Bergstrasse, Germany)》2022,28(60):e202201145
The coordination chemistry of f-block elements (lanthanide and actinide) in molten salts has become a resounding topic in view of its great importance to the research and development (R&D) of molten salt reactors and pyroprocessing. In this Review article, a general overview of the coordination chemistry of f-block elements in molten salts is provided including past achievements and recent advances. Particular emphases are placed on the oxidation state, speciation, and solution structure of f-block metal ions in molten salts, as well as their relationships with the salt composition. Furthermore, this review briefly discusses the spectroscopic and theoretical methods that complement each other in revealing the coordination properties. 相似文献
7.
Dr. Oliver Hegen Jens Braese Prof. Dr. Alexey Y. Timoshkin Prof. Dr. Manfred Scheer 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(2):485-489
A new class of neutral bidentate ligands with pnictogenyl-functional sites has been obtained. The reaction of tmeda⋅(BH2I)2 ( 1 , tmeda=tetramethylethylendiamine) with different phosphanides yields the corresponding bidentate phosphanylboranes tmeda⋅(BH2PH2)2 ( 2 a ), tmeda⋅(BH2PPh2)2 ( 2 b ), and tmeda⋅(BH2tBuPH)2 ( 2 c ). This reaction strategy could be further extended to synthesize the first bidentate arsanylborane tmeda⋅(BH2AsPh2)2 ( 3 ). Depending on the substituents on the phosphorus, these compounds form different AuI complexes, to build either polymeric tmeda⋅(BH2PH2AuCl)2 ( 4 a ), or monomeric tmeda⋅(BH2PPh2AuCl)2 ( 4 b ) products. These compounds form also neutral oligomeric group 13/15 chain-like molecules by coordination to a boron moiety such as tmeda⋅(BH2PH2BH3)2 ( 5 a ) and tmeda⋅(BH2AsPh2BH3)2 ( 5 b ). DFT calculations provide insight into the differences between the syntheses of mono- and bidentate pnictogenylboranes. 相似文献
8.
建立氢化物发生–原子吸收光谱法联用测定铅粉中痕量砷、锑的方法。试样用稀硝酸溶解,用5%抗坏血酸溶液作为砷(Ⅴ)、锑(Ⅴ)的预还原剂,5%的硫脲溶液作为其它元素的掩蔽剂,选用1%硼氢化钠溶液作为还原剂,氢化物反应在10%盐酸介质中进行。在优化的试验条件下,砷、锑的质量浓度在0~20 ng/m L范围内与吸光度线性相关,相关系数r2分别为砷0.999 6,锑0.993 8,方法的检出限分别为砷0.40 ng/m L,锑0.75 ng/m L。砷、锑测定结果的相对标准偏差分别为4.96%,6.27%(n=6),铅粉样品加标回收率分别为砷87.6%,锑79.3%。该方法准确可靠,可用于测定铅粉中痕量砷、锑。 相似文献
9.
On the Ambiphilic Reactivity of Geometrically Constrained Phosphorus(III) and Arsenic(III) Compounds: Insights into Their Interaction with Ionic Substrates 下载免费PDF全文
Thomas P. Robinson Siu‐Kwan Lo Daniel De Rosa Simon Aldridge Jose M. Goicoechea 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(44):15712-15724
The ambiphilic nature of geometrically constrained Group 15 complexes bearing the N,N‐bis(3,5‐di‐tert‐butyl‐2‐phenolate)amide pincer ligand (ONO3?) is explored. Despite their differing reactivity towards nucleophilic substrates with polarised element–hydrogen bonds (e.g., NH3), both the phosphorus(III), P(ONO) ( 1 a ), and arsenic(III), As(ONO) ( 1 b ), compounds exhibit similar reactivity towards charged nucleophiles and electrophiles. Reactions of 1 a and 1 b with KOtBu or KNPh2 afford anionic complexes in which the nucleophilic anion associates with the pnictogen centre ([(tBuO)Pn(ONO)]? (Pn=P ( 2 a ), As ( 2 b )) and [(Ph2N)Pn(ONO)]? (Pn=P ( 3 a ), As ( 3 b )). Compound 2 a can subsequently be reacted with a proton source or benzylbromide to afford the phosphorus(V) compounds (tBuO)HP(ONO) ( 4 a ) and (tBuO)BzP(ONO) ( 5 a ), respectively, whereas analogous arsenic(V) compounds are inaccessible. Electrophilic substrates, such as HOTf and MeOTf, preferentially associate with the nitrogen atom of the ligand backbone of both 1 a and 1 b , giving rise to cationic species that can be rationalised as either ammonium salts or as amine‐stabilised phosphenium or arsenium complexes ([Pn{ON(H)O}]+ (Pn=P ( 6 a ), As ( 6 b )) and [Pn{ON(Me)O}]+ (Pn=P ( 7 a ), As ( 7 b )). Reaction of 1 a with an acid bearing a nucleophilic counteranion (such as HCl) gives rise to a phosphorus(V) compound HPCl(ONO) ( 8 a ), whereas the analogous reaction with 1 b results in the addition of HCl across one of the As?O bonds to afford ClAs{(H)ONO} ( 8 b ). Functionalisation at both the pnictogen centre and the ligand backbone is also possible by reaction of 7 a / 7 b with KOtBu, which affords the neutral species (tBuO)Pn{ON(Me)O} (Pn=P ( 9 a ), As ( 9 b )). The ambiphilic reactivity of these geometrically constrained complexes allows some insight into the mechanism of reactivity of 1 a towards small molecules, such as ammonia and water. 相似文献
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