异丙醇增感电感耦合等离子体质谱法直接测定土壤和沉积物中硒

提出了沸水浴混合酸法消解,以异丙醇为增感剂,电感耦合等离子体质谱直接测定土壤和沉积物中硒的方法。实验表明2mol/L硝酸-4mol/L盐酸混酸能有效溶出土壤和沉积物中各种形态的硒。相对于1%硝酸基体,4%(V/V)异丙醇基体中硒的ICP-MS响应值提高了12.1倍;而且4%(V/V)异丙醇基体可有效抑制硒的质谱干扰。ICP发射功率和雾化气流速是影响异丙醇在ICP-MS测定过程增敏效应的主要因素。以78硒为测定同位素,方法检出限为0.005mg/kg,实际样品测定精密度均小于5%。用于测定土壤和沉积物国家标准样品并对其消解液进行加标回收实验,结果令人满意。     

王水消解—原子荧光法测定土壤中的硒

样品经(1+1)王水于沸水浴中加热消解,用氢化物发生-原子荧光法测定土壤中硒的含量。对测定的影响因素:HCl浓度、KBH4浓度及共存离子的干扰等试验条件做了研究并予以优化。荧光强度与硒的质量浓度在30μg.L-1以内呈线性关系,方法的检出限(3s/b)为0.1μg·L-1,方法的相对标准偏差(n=6)小于5%,应用此法对标准物质ESS-3和土壤样品进行分析,测得硒的回收率在90%～110%之间。     

微波消解-原子荧光法测定土壤中汞、砷、硒

建立了微波消解-原子荧光法测定土壤中汞、砷、硒的方法.汞在0.00 μg/L～1.00 μg/L、砷在0.00 μg/L～10.0 μg/L、硒在0.00 μg/L～2.00 μg/L之间线性关系良好,以称样0.200 0 g计,检出限汞为0.005 mg/kg,砷为0.009 mg/kg,硒为0.025 mg/kg.经国家有证标准物质验证,方法精密度与准确度均能满足土壤环境样品的测试要求.     

弗罗里硅土净化和凝胶色谱净化在土壤苯并(a)芘测定中的应用

采用ASE萃取-弗罗里硅土净化-HPLC法和ASE萃取-GPC净化-HPLC法测定土壤中苯并(a)芘,并将2种方法的测定结果作比对。试验表明,方法在0.02 mg/L~0.500 mg/L之间线性良好,当取样量为10 g时,弗罗里硅土净化土壤样品方法检出限为8.93×10~(-5)mg/kg,平均加标回收率为72.7%~73.8%,3次测定结果的RSD为4.0%~4.5%;凝胶色谱净化土壤样品方法检出限为1.98×10~(-5)mg/kg,平均加标回收率为88.8%~90.2%,3次测定结果的RSD为2.1%~2.8%。     

抑制型电导-离子色谱法测定水中无机阴离子

采用抑制型电导-离子色谱法测定生活饮用水、污水和地表水中F-、Cl-、NO2-、Br-、NO3-、PO43-、SO42-等7种无机阴离子,对清洁水样过滤后直接测定,浑浊样品离心后取上清液过滤测定。F-在0.100 mg/L~1.20 mg/L范围内、其余6种阴离子在1.00 mg/L~12.0 mg/L范围内线性良好,方法检出限为0.031 mg/L~0.47 mg/L,水样平行测定的RSD为0.9%~1.8%,加标回收率为82.6%~110%。     

APDC-MIBK萃取火焰原子吸收分光光度法测定生活垃圾堆肥产品中铅、镉的研究

通过试验研究,建立了硝酸-氢氟酸-高氯酸消解、APDC-MIBK萃取火焰原子吸收分光光度法测定生活垃圾堆肥产品中的铅、镉.该方法铅的检出限为2mg/kg,镉的检出限为0.2mg/kg(按称取0.5g试样消解定容至50ml计算),用于不同地域堆肥样品测定,铅、镉的相对标准偏差(RsD)分别为2.29%～8.16%和5.17%～11.7%,加标回收率介于86.8%～107.2%和88.0%～108.0%之间.     

5-氯-2-(吡啶偶氮)-1,3-二氨基苯分光光度法测定水质钴

采用5-氯-2-(吡啶偶氮)-1,3-二氨基苯分光光度法测定水质钴。对分析方法的样品前处理、样品保存、样品分析条件、干扰消除、检出限及测定范围、实际样品测定进行了深入研究和技术改进。水样经消解后测定的方法检出限为0.009 mg/L,经富集后测定的方法检出限为4×10-4mg/L,干扰消除实验的回收率为96%~101%,地表水、地下水、生活污水及工业废水等4种类型水样的加标回收率为92%~103%。     

原子荧光法同时测定食品中的硒和汞

采用硝酸和双氧水微波消解-原子荧光法同时测定食品中硒和汞元素的含量,用5%的盐酸作为载流,10 g·L~(-1)的硼氢化钾作还原剂进行测定。结果表明,硒和汞元素校正曲线相关系数分别为0.9999和0.9998。方法检出限硒0.001 mg·kg~(-1),汞0.0001 mg·kg~(-1)。相对标准偏差硒为3.9%～9.7%,汞为3.9%～9.5%。表明该方法具有较好的准确性和稳定性。同时通过加标实验,硒和汞的加标回收率分别为96.0%～106.0%和96.0%～104.0%,进一步确认了该方法准确可靠。     

氢化物发生—原子荧光法测定河水中硒(Ⅳ)硒(Ⅵ)

在河水样品４ｍｏｌ／ＬＨＣｌ介质中硒生成氢化物，用氢化物发生法测定硒（Ⅳ）含量。将样品的４ｍｏｌ／ＬＨＣｌ溶液在沸水中加热还原硒（Ⅵ）至硒（Ⅳ）测定总量。总硒量减去硒（Ⅳ）量，分别求得硒（Ⅳ）和硒（Ⅵ）含量     

ASE-气相色谱法测定油田区土壤中多种石油烃

采用气相色谱法测定油田区土壤中C_(10)～C_(40)的石油烃,通过优化加速溶剂萃取的条件,使方法在62 mg/L～3 100 mg/L范围内线性良好,方法检出限为4.8 mg/kg。用该方法测定石油区短期、中期、长期油井污染土壤样品,5次测定结果的RSD为1.3%～5.2%,加标回收率为84.8%～98.5%,有证标准样品测定结果在可信区间内。     

环境中微量硒形态检测方法

对硒进入生物体的途径和形态进行了讨论，并着重介绍了现已报道使用的硒的形态检测方法。     

环境介质中硒的检测方法研究进展

结合国内外的研究进展,综述了环境介质中硒的各种检测方法。其中重点介绍了比较常用的测定方法,如原子吸收光谱法(AAS)、原子荧光光谱法(AFS)和电感耦合等离子体原子发射光谱法(ICP-AES)等,并展望了硒在检测方法上的发展趋势。     

酸性土壤有效态硒浸提方法的研究

本文提出了酸性土壤有效硒的0.1MKH_2PO_4浸提法.土壤和植物的分析结果表明:0.1MKH_2PO_4浸提有效态硒能反映土壤对植物的供硒状况.黑麦幼苗试验进一步证明KH_2PO_4浸提有效态硒可以作为酸性土壤有效硒的指标.     

Mercury, Methylmercury, and Selenium Concentrations in Eggs of Common Loons (Gavia immer) from Canada

Concentrations of Hg and Se were determined for a total of 125Common Loon (Gavia immer) eggs collected from lakes in Alberta, Saskatchewan, Ontario, Quebec, New Brunswick and NovaScotia, Canada between 1972 and 1997. Resulting data were compared to Hg and/or Se concentrations known or suspected tocause reproductive impairment in birds. Organic (methyl) Hg analyses were also performed on a subset of 24 loon eggs. Thirty-nine of 125 eggs had total Hg levels exceeding those (0.6 g g^-1 ww, or 2.5 g g^-1 dw)previously reported to be associated with reproductive impairment in common loons (Barr, 1986), and 9 of 125 eggshad Hg concentrations higher than the level associated withreproductive impairment in birds generally 1 g g^-1 ww; (Thompson, 1996). Selenium concentrations in loon egg samples were less than levels known to cause reproductiveimpairment in birds. A weak but significant positive correlation was observed between egg-Hg and -Se concentrations(r = 0.511, p < 0.05). On average, methylmercury accounted for about 87% of total Hg in 24 eggs analysed for both total and organic Hg. In this subset of eggs, the relationship between organic (methyl) Hg and Se was significant (r = 0.538, p = 0.007) while that found between inorganic Hg and Se in the same eggs was not significant (r = 0.353, p = 0.091). This relationship was unexpected and was contrary to relationships established for organic and inorganic Hg vs. Se in adult loon liver and kidney tissue (Scheuhammer et al., 1998b).     

Selenium in the Blackfoot, Salt, and Bear River Watersheds

Nine stream sites in the Blackfoot River, Salt River, and Bear River watersheds in southeast Idaho, USA were sampled in May 2001 for water, surficial sediment, aquatic plants, aquatic invertebrates, and fish. Selenium was measured in these aquatic ecosystem components, and a hazard assessment was performed on the data. Water quality characteristics such as pH, hardness, and specific conductance were relatively uniform among the nine sites. Of the aquatic components assessed, water was the least contaminated with selenium because measured concentrations were below the national water quality criterion of 5 g/L at eight of the nine sites. In contrast, selenium was elevated in sediment, aquatic plants, aquatic invertebrates, and fish from several sites, suggesting deposition in sediments and food web cycling through plants and invertebrates. Selenium was elevated to concentrations of concern in fish at eight sites (> 4 g/g in whole body). A hazard assessment of selenium in the aquatic environment suggested a moderate hazard at upper Angus Creek (UAC) and Smoky Creek (SC), and high hazard at Little Blackfoot River (LiB), Blackfoot River gaging station (BGS), State Land Creek (SLC), upper (UGC) and lower Georgetown Creek (LGC), Deer Creek (DC), and Crow Creek (CC). The results of this study indicate that selenium concentrations from the phosphate mining area of southeast Idaho were sufficiently elevated in several ecosystem components to cause adverse effects to aquatic resources in southeastern Idaho.     

氢化物发生原子荧光法测定饮用水中的微量硒

氢化物发生原子荧光法测定饮用水中的微量硒时。仪器条件和试剂的浓度选择很重要。本文对条件的最佳化进行了实验。并对方法的精密度、准确度和检出限进行了讨论。     

The American Dipper as a Bioindicator of Selenium Contamination in a Coal Mine-Affected Stream in West-Central Alberta, Canada

Elevated levels of selenium have been found in water and aquatic biota downstream from two open-pit coal mines in the Rocky Mountain foothills of Alberta. Birds are particularly sensitive to excessive dietary selenium. However, there is relatively little information on selenium accumulation in birds' eggs on fast-flowing mountain streams. We determined levels of selenium in water samples, caddisfly larvae and eggs of American dippers (Cinclus mexicanus) nesting on the Gregg River, downstream from the mines, and on reference streams in the same general vicinity. Selenium levels (mean, 95% confidence limits) in water samples and caddisflies collected from sites near dipper nests on the Gregg River (water: 4.26, 1.90–9.56 μg L⁻¹; caddisflies: 8.43, 7.51–9.46 μg g dry wt⁻¹) were greater than those collected from sites near nests on reference rivers (water: 0.38, 0.21–0.71 μg L⁻¹; caddisflies: 4.65, 4.35–4.97 μg g dry wt⁻¹). The mean (± 1SE) selenium level in dipper eggs from the Gregg River (6.3 ± 0.2 μg g⁻¹ dry wt) was significantly higher than it was in eggs from reference streams (4.9 ± 0.2 μg g⁻¹ dry wt). Concentrations of selenium in eggs were significantly correlated with those in water samples (r = 0.45). The maximum selenium level in eggs from the Gregg River (9.0 μg g⁻¹) may have been high enough to warrant concern from an ecotoxicological perspective. The American dipper can serve as a useful bioindicator of selenium contamination in mountainous, lotic ecosystems.     

二氨基联苯胺分光光度法测定水质中硒的方法改进

采用3.3＇-二氨基联苯胺分光光度法对测定水质中硒的方法进行改进，主要研究了样品中硒的测定条件，通过对不同显色波长、酸碱度显色条件、显色剂用量、酸碱度比色条件的研究，得出比较理想的定量分析条件。采用该方法测定硒，显色稳定，准确度、精密度均能达到要求。     

石墨炉原子吸收分光光度法测定地表水中硒的研究

研究了石墨炉原子吸收分光光度法测定地表水中硒过程中灰化电流的选择和加入基体改进剂减少干扰并提高灵敏度的方法。     

Microtrace Metalloids Speciation in Lakes Water Samples (Poland)

This paper presents the results of the determination of arsenic, antimony and selenium concentrations of inorganic speciation in surface water samples from Gniezno city (western Poland) and its neighborhood. The concentration of elements were up to 1.85 ng/ml for arsenic, 1.61 ng/ml for antimony and 0.45 ng/ml for selenium (detection limits: 0.04 ng/ml for As and Sb and 0.03 ng/ml for Se). A variety of concentrations for the determined elements has been obtained in waters from Gniezno city’s neighborhood and in water from down-town reservoirs which are under strong anthropogenic pressure.