水体沉积物中汞形态分析方法进展

文中对近年来汞的形态分析的发展作了评述.主要涉及色谱法、原子吸收光谱法、原子荧光光谱法、电化学分析法、中子活化法及毛细管电泳法在汞形态分析中的应用(引述文献32篇).     

荧光光谱法测定工业废水中痕量汞的研究

利用汞（Ⅱ）在适量一乙醇和β－环糊精存在下对四（４－三甲铵苯基）卟啉（ＴＡＰＰ）的荧光熄灭作用,提出了测量汞的高灵敏荧光光度新方法,拟定条件下的荧光激发峰λｅｘ＝４１４ｎｍ,荧光发射峰λｅｍ＝６４６ｎｍ,荧光熄灭值△Ｆ与Ｈｇ（Ⅱ）的质量浓度在０～３μｇ／２５ｍＬ范围内呈线性关系。本法操作简便,不必加热,也无需催化剂,应用迅速且体系稳定。本法用于测定工业废水等样品中的痕量汞,与其它方法的结果吻合。     

沉积物样品中痕量元素汞的形态分析研究进展

归纳总结了沉积物中汞形态分析研究进展,内容包括沉积物汞的赋存形态,样品的预处理和不同形态汞的原子光谱法、色谱法、电感耦合等离子体质谱法及联用技术等分析方法,指出了存在的问题和未来的发展方向。     

环境样品中痕量锑的形态分析研究进展

环境样品中不同形态锑,其生物活性及其毒性不同,其形态分析具有重要意义。由于环境样品中锑的含量相对较低,不同形态锑的分析具有挑战性。归纳总结了环境样品中痕量超痕量锑的形态分析概况及近年来的发展趋势,内容主要包括样品的前处理和不同形态锑的分析方法,指出了未来的发展方向。     

燃煤烟气中汞的形态及其分析方法

从实验研究和模型分析两方面评述了目前研究燃煤烟气中汞的化学形态分布的各种分析方法 ,对各种方法的优缺点进行了比较 ,同时指出了将来的研究方向。实验研究中的汞形态测量方法可以归纳为取样分析法和在线分析法两大类 ,EPA法 2 9是使用最为广泛的一种方法 ,不同方法在总汞的测量方面有较好的一致性 ,而在测量氧化物形态时存在一定偏差。取样分析法中对取样介质的选择吸收性和收集效率不确定性、分析物的回收效率等的研究是热点问题 ,而在线分析法是目前正在发展的新兴方向。虽然在煤燃烧过程中使用化学热力平衡模型分析有一定的局限性 ,但在目前缺乏动力学参数的条件下 ,它仍是一个十分有效的手段 ,在化学热力学模型的基础之上发展化学动力学模型是模型分析方面一个主要的、新兴的研究方向。     

阻抑褪色光度法测定痕量汞

提出一种测定痕量汞的新的光度法。该法基于Ｈｇ（Ⅱ）对Ｈ２Ｏ２与离子缔合物ＡｇＣｌ·ＰＶＡ·Ａｇ~＋·Ｆｉｎ~－褪色反应的抑制效应,该离子缔合物对应于聚乙烯醇存在下Ｆａｊａｎｓ（法扬斯）法的终点,线性回归方程△Ａ＝０．０２＋ ４．０×１０~（－３）Ｃ_（Ｈｇ（Ⅲ））（μｇ／Ｌ）,相关系数ｒ＝０．９９９２,Ｈｇ（Ⅱ）浓度在４．０～２０．０μｇ／Ｌ范围内服从比耳定律,检出限０．０４μｇ／Ｌ。该法用于废水样中Ｈｇ（Ⅱ）的测定,结果与双硫腙法结果相符。     

粉煤灰中痕量汞的催化光度法测定

在 p H3.5乙酸 -乙酸钠缓冲溶液中痕量汞 ( )对 K4[Fe( CN) 6 ]与 4 ,7-二苯基 -1 ,1 0 -邻菲 口罗啉 ( BPT)显色反应有催化作用 ,加入硫脲能提高其灵敏度 ,显色程度与 Hg( )量在一定范围内呈线性相关。借此建立测定痕量 Hg( )的分光光度法。实验表明 ,有色溶液的最大吸收波长为 535nm,摩尔吸光系数为 4 .5× 1 0 6 L·mol- 1· cm- 1 ,催化程度与 Hg( )量在 0 .0～ 2 .0 μg/ 50 m L范围内符合比耳定律 ,选择性较好。结合萃取分离 ,本法可用于测定粉煤灰中的痕量汞。     

天然水中痕量无机汞和有机汞的氢化物原子荧光光谱法分析

建立了天然水中溶解的痕量无机汞和有机汞的氢化物原子荧光光谱法分析方法,该方法经标准物质(PACS-1)和加标回收实验研究表明重现性好、准确度高。在此基础上,应用该方法分析了该校人工湖水中的无机汞和有机汞,发现无机汞和有机汞的含量均低于0.1 礸/L。     

高效液相色谱及其联用技术在汞形态分析中的应用

本文对近二十年来高效液相色谱及其联用技术在汞的形态分析中的应用进行了综述，着重讨论了样品的前处理方法，高效液相色谱用于汞化合物的形态分离以及检测器的选择。     

Construction and Evaluation of a Gold Tubular Electrode for Flow Analysis: Application to Speciation of Antimony in Water Samples

A tubular gold electrode (TGE) is described for the first time by summarizing the important aspects of its construction and evaluation. Applicability of the TGE is evaluated in the speciation of Sb(III) and Sb(V) using anodic stripping voltammetry in a single flow manifold. Studies with surface active interferences and metallic cations were performed. The proposed conditions for antimony determination showed good tolerance towards cationic, anionic and nonionic surface active substances. A linear response for antimony was obtained for solutions containing significant amounts of several metallic cations. Linear calibration curves for Sb(III) were obtained in the range 1–10 ppb with a detection limit of 0.19 ppb (CV=2.91%, n=5, [Sb(III)]=5 ppb). For Sb(V), linear calibration curves were in the range 1–15 ppb with a detection limit of 0.32 ppb (CV=1.41%, n=5, [Sb(V)]=5 ppb). The figures of merit achieved sustain for the good applicability of the proposed method as it allows the determination of antimony at levels below maximum values permitted in consuming waters. Results of antimony concentration determined in water samples were validated against the ICP‐MS reference procedure or compared with reference water samples.     

河水中痕量铜的形态分析研究

采用离子交换树脂分离／分光光度法研究了铜的形态分离分析条件，提出了铜的形态分析方法。用此法测定了珠江水中痕量铜的总量、悬浮态、溶解态、阴离子态、阳离子态、非离子态及其形态分布，结果令人满意。     

A Tin(II) Chloride Based Reduction Method for Multiple-Metal Trace Analysis of Natural Waters

Based on tin(II) chloride reduction in basic medium, a method of general use is proposed for the estimation of the whole gamut of multiple trace metals in natural waters by the atomic absorption method. The quantitative aspects of the method related to variables such as pH of the medium, amount of reductant and operational conditions are studied as a function of absorption sensitivity. The proposed method utilizes only a 50.0 ml portion of the water sample and yields above 90 per cent recoveries for various metals from a single aliquot of the sample. The reported data pertain to the estimation of silver, chromium, copper, iron, lead, mercury, manganese, magnesium, nickel and strontium, reported as averaged over replicate measurements at +-2S confidence level. The precision in individual cases is found to be better than +1.8%.     

全蝎中4种微量元素的形态分析

对中药全蝎中铜、锌、铁和镁4种微量元素存在的形态及含量进行了研究。文中叙述了全蝎样品中元素的各种形态(可溶态、悬浮态、无机态、有机态)的提取方法和分离,采用火焰原子吸收光谱法测定了各试液中4种微量元素的含量。结果显示,全蝎中4种元素的总提取率在39.9%~63.2%之间,浸留比在73.6%~126.0%之间,悬浮态颗粒吸附率在10%左右,铜、锌、铁、镁的有机态与无机态的比例在250.0%~550.0%之间。     

Liquid Chromatography with Pulsed Amperometric Detection for Speciation of Mercury

Liquid chromatography with pulsed amperometric detection (PAD) at an Au electrode was successfully applied for speciation of mercury: inorganic mercury, methylmercury and ethylmercury. The optimized conditions for triple-step potential waveforms utilized in PAD were: E₁ 1800 mV, t₁ 50 ms; E₂ 300 mV, t₂ 3850 ms; E₃ 750 mV, t₃ 100 ms; mercury oxidation was monitored at E₃. With the eluent of HClO₄ (0.10 M) + KCl (1.0 mM) + CH₃CN (1.0%) at a flow rate 0.80 mL/min, three mercury species were fully separated in 6 min on a glass column (3 mm × 10 cm) packed with Chemcosorb C₁₈ (5 μm). However, the first peak (inorganic mercury) was commonly overlapped by the solvent front. The relative standard deviations (n = 6) for methylmercury (15 ppb) and ethylmercury (30 ppb) were 4.2% and 2.8%, respectively. The linear range tested was 2 – 500 ppb (r = 0.9998) for methylmercury, and was 4 – 1000 ppb (r = 1.000) for ethylmercury. The detection limits (S/N = 3) were 1.2 ppb and 1.8 ppb for methylmercury and ethylmercury, respectively. The results of determination of the mercury-containing species thimerosat in three commercial contact-lens solutions agreed satisfactorily with the expected values.     

Determination of Ethylenethiourea (ETU) at Trace Levels in Water Samples by Cathodic Stripping Voltammetry

A stripping voltammetric method for the determination of ethylenethiourea in water samples is described based on its adsorptive deposition at the hanging mercury drop electrode (HMDE). In a borate buffer (pH 9.0) as supporting electrolyte, ETU is deposited at +100 mV (vs. Ag/AgCl) and stripped during the cathodic scan. The linear range for the measurements was from 2.0 to 100 μg L^?1, with a detection limit calculated as 1.4 μg L^?1 after a deposition time of 300 s and a RSD of 1.9% (n=5) for 50 μg L^?1 of ETU measured. The interferences of some organic compounds and metallic ions were tested. Recoveries between 93 and 110% were obtained using the standard addition method for spiked samples of natural and drinking waters. The method is rapid and applicable in the monitoring of ETU residues in water samples.     

汞形态分析中的前处理技术

对近二十年来汞的分离富集技术进行了回顾，并对不同基体样品的分离富集方法进行了总结。     

积雪草中五种微量元素的形态分析

按照传统煎煮法对积雪草中铁、锰、锌、铜和锶5种元素进行提取,用微孔滤膜分离提取液中的可溶态与悬浮态,利用阳离子交换树脂柱、大孔吸附树脂柱和螯合树脂柱对可溶态中的游离态和非游离态、有机态和无机态、稳定态和不稳定态进行分离后,采用火焰原子吸收光谱法(FAAS)对各种形态中的上述5种元素进行测定。结果显示,积雪草中5种元素的提取率为11.88%～22.86%,浸留比为14.04%～31.44%。该法测定各元素的回收率为95.6%～104.3%,相对标准偏差在0.37%～1.14%之间,具有较好的精密度和准确度。