一次消解测定蔬菜中多种重金属的简捷方法

针对一般实验室检测人员少,检测任务重的问题,研究了蔬菜通过一次湿化消解后,消解液可以测定多种重金属元素的方法,大大提高了效率,减轻了工作量.     

氢化物原子荧光法(HG-AFS)测定鸡蛋中的硒

本文建立了一种HG－AFS法测定食疗蛋中硒的方法，该方法简单，快速，同时也提高了分析的灵敏度。方法的检出限为0.3μg/L，食疗蛋中硒的样品测定的相对标准偏差＜10％，回收率在90％以上。     

氢化物原子荧光法测定中草药中痕量铅

提出了以重铬酸钾为氧化剂、碱性铁氰化钾为络合剂 ,在柠檬酸介质中进行铅的氢化物发生反应。采用断续流动氢化物发生器 ,对原子荧光法测定痕量铅的条件进行了系统研究 ,并考察了共存元素的干扰情况。在最佳测试条件下 ,测得铅的检出限 (3σ)为 0 .19μg·L- 1,相对标准偏差为 0 .92 %。应用于中草药中痕量铅的测定 ,回收率为 95 .1%～ 10 9.5 % ,结果满意     

Electrochemical vapor generation of selenium species after online photolysis and reduction by UV-irradiation under nano TiO<Subscript>2</Subscript> photocatalysis and its application to selenium speciation by HPLC coupled with atomic fluorescence spectrometry

An online UV photolysis and UV/TiO₂ photocatalysis reduction device (UV–UV/TiO₂ PCRD) and an electrochemical vapor generation (ECVG) cell have been used for the first time as an interface between high-performance liquid chromatography (HPLC) and atomic fluorescence spectrometry (AFS) for selenium speciation. The newly designed ECVG cell of approximately 115 L dead volume consists of a carbon fiber cathode and a platinum loop anode; the atomic hydrogen generated on the cathode was used to reduce selenium to vapor species for AFS determination. The noise was greatly reduced compared with that obtained by use of the UV–UV/TiO₂ PCRD–KBH₄–acid interface. The detection limits obtained for seleno-DL-cystine (SeCys), selenite (Se^IV), seleno-DL-methionine (SeMet), and selenate (Se^VI) were 2.1, 2.9, 4.3, and 3.5 ng mL^–1, respectively. The proposed method was successfully applied to the speciation of selenium in water-soluble extracts of garlic shoots cultured with different selenium species. The results obtained suggested that UV–UV/TiO₂ PCRD–ECVG should be an effective interface between HPLC and AFS for the speciation of elements amenable to vapor generation, and is superior to methods involving KBH₄.     

Comparative study of the instrumental couplings of high performance liquid chromatography with microwave-assisted digestion hydride generation atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry for chiral speciation of selenomethionine in breast and formula milk

A comparison of chiral separation and analysis of selenomethionine in breast and formula milk, using high performance liquid chromatography (HPLC) on a glycopeptide teicoplanin-based chiral stationary phase (Chirobiotic T), coupled to atomic fluorescence spectrometry (AFS) and inductively coupled plasma (ICP) MS detectors has been performed. The coupling HPLC-microwave-assisted digestion hydride generation requires on-line post-column analytes treatment, and a severe sample clean-up for fat and proteins elimination using centrifugation and ultrafiltration. Underivatized -selenomethionine enantiomers were completely resolved in 10 min using unbuffered water mobile phase at 1 ml min⁻¹ flow. Good selectivity and sensitivities (detection limits 3.1 and 3.5 ng ml⁻¹ as Se for - and -selenomethionine, respectively) were obtained, and method robustness and simplicity, together to the low cost of AFS detector, makes it suitable for infant milk routine analysis. HPLC–ICP-MS coupling exhibits very low detection limits (0.9 ng ml⁻¹, as Se) for each -selenomethionine enantiomers, but the method suffers from matrix influence, that produces a poor S/N ratio and low reliability.

The methods were applied to breast and formula milk samples with recoveries of 80% of the total selenium presence, which is attributable to the existence of other unknown species. -Selenomethionine was the only isomer present in breast milk, but a 30% of -selenomethionine was also detected in formula milk.     

High Stability of a Phosphenium Ion Allows Umpolung of P--H Bonds

The high intrinsic stability of 1,3,2-diazaphospholenium cations enhances ionic polarization of covalent P--X bonds in P -halogeno- and P -hydrido-diazaphospholenes. The physical properties of the latter suggest a hydridic nature of the P--H bond, and their reactivities display an "Umpolung" as compared to known reaction patterns of phosphines.     

碱性模式氢化物发生原子荧光光谱法测定铁矿石中砷

建立了碱性模式氢化物发生原子荧光光谱法测定铁矿石中砷的最佳仪器和实验条件。采用微波消解分解样品,在硫脲和L-半胱氨酸存在下将As（Ⅴ）还原为As（Ⅲ）,以1mol／L KOH作为介质,以0．75mol／L H3PO4作为载流,原子荧光光谱法测定样品中的砷。方法检出限为0．35μg／L,RSD在2．0％。9．4％之间,加标回收率95％～103％。对标准样品进行分析验证,结果与标准值相符。应用于铁矿样品的测定,结果满意。     

三种消解方法在测定近海沉积物中Pb、 Cu、 Cd、 Hg及As的应用

常压湿式消解、高压微波消解、常压微波消解3种方法被应用于近海沉积物中Pb、 Cu、 Cd、 Hg、 As 5种重金属元素的分析. 以近海海洋沉积物标准物质为样品经3种方法消解后, 通过石墨炉原子吸收法测定Pb、 Cu、 Cd和氢化物发生原子荧光法同时测定Hg、 As. 结果表明, 样品经常压湿式消解, 其Pb、 Cu、 Cd回收率在80%～123%内而Hg、 As回收率低;经高压微波消解, 标样中Pb、 Cu、 Cd、 As回收率在84%～117%内, 对Hg测定回收率偏低;常压微波消解更适合于Cu、 Cd、 Hg、 As的消解, 其回收率在95%～121%之间而Pb回收率低于42.4%. 常压湿式消解与常压微波消解被用于大亚湾人工渔礁区沉积物样品的处理, 有较好的测定结果.     

新乐工业新区土壤中多种元素的测定

采用湿法消解对不同厂区的土壤进行前处理,应用电感耦合等离子体原子发射光谱法(ICP-OES)测定土壤中的金属元素含量,使用原子荧光光谱法AFS测定砷的含量,测定的相对标准偏差为0.8%～3.0%,回收率为89.0%～105.5%。实验表明,方法简单快速、准确,较高的灵敏度和较低的检出限,均能满足土壤中多元素分析的要求。