HPLC和HPLC-MS/MS测定地表水中酚类化合物

采用高效液相色谱法(HPLC)和高效液相色谱-三重四级杆质谱联用法(HPLC-MS/MS)测定地表水及饮用水中11种酚类化合物,通过优化测定条件,使HPLC法在0.020 mg/L~50.0 mg/L范围内,HPLC-MS/MS法在0.500μg/L~250μg/L范围内线性良好,方法检出限分别为0.005μg/L~0.031μg/L和0.005μg/L~1.56μg/L。未检出的实际样品加标回收率分别为57.2%~96.7%和81.3%~113%,RSD分别为1.5%~5.3%和3.9%~17.7%。     

黄河甘宁蒙段表层沉积物中总磷3种提取方法的比较

通过微波消解法、标准测试方法(SMT)和碱熔法分别测定了水系沉积物成分分析标准物质GBW07307a(GSD-7a)中的总磷(TP)含量,并分别采用3种方法对采集于黄河流域甘宁蒙段表层沉积物样品进行TP含量和样品加标回收率的测定。结果表明:测定标准物质的相对误差绝对值:微波消解法碱熔法SMT法;变异系数:微波消解法碱熔法SMT法。同时,微波消解法提取的表层沉积物TP含量的范围为634.3~909.2μg/g;SMT法TP含量的范围为627.1~889.5μg/g;碱熔法TP含量的范围为559.1~784.8μg/g。微波消解法的测定结果相对偏高,SMT法的测定结果相对偏低。样品加标回收率平均值:微波消解法SMT法碱熔法;变异系数:微波消解法碱熔法SMT法。综合测定标准物质中TP含量以及样品加标回收率实验结果的准确度和精密度,对于黄河甘宁蒙段表层沉积物,使用SMT法提取TP较优于微波消解法和碱熔法。     

固相萃取-GC/MS法测定地表水中3-甲基吲哚

采用微球硅胶键合C_(18)固相萃取柱萃取水样中的3-甲基吲哚,并用气质联用法测定,方法在0 mg/L~10.0 mg/L范围内线性良好,方法检出限为0.2μg/L。空白水样3个质量浓度水平的加标回收率为89%~94%,7次测定结果的RSD为2.3%~6.9%。用该方法测定7个实际地表水样品,其中4个地表水样品检出3-甲基吲哚,地表水样的加标回收率为81.5%~97.0%。     

紫外光度法测定地表水中石油类的油标选择

精选了一种新油标。采用这种油标,可使紫外分光光度法测地表水中石油类的令人满意,省工省时。     

南漪湖沉积物磷的赋存形态及对上覆水的影响

以宣城市南漪湖为例,采用改进的无机磷分级提取方法对全湖共39个点位沉积物中磷(P)赋存形态进行系统研究,并分析其与上覆水体、间隙水等相互关系.结果表明,南漪湖水体磷污染水平已经处于高位,沉积物间隙水磷与上覆水体磷空间分布特征具有密切关系.南漪湖沉积物中总磷(TP)含量变化范围为463.3～1016.6mg/kg,其中各形态磷空间分布具有明显的差异性,与外源磷输入等密切相关.赋存形态含量大小、相对比例顺序依次为:钙结合态磷(Ca-P)>铁结合态磷(Fe-P)>铝结合态磷(Al-P)>还原剂可溶性磷(RS-P)>残渣态磷(Res-P)>弱吸附态磷(L-P).沉积物中TP含量与Fe-P、RS-P、Res-P极显著正相关,与L-P含量显著正相关.外源磷输入和水产养殖对南漪湖沉积物内源磷中Fe-P和RS-P贡献可能较大.南漪湖沉积物内源磷对上覆水体的潜在风险较高,其中生物有效性较高的L-P、Al-P、Fe-P和Rs-P的总和相对比例可达60%左右.沉积物中磷形态与间隙水磷浓度关系较密切,其中Al-P、Ca-P对间隙水中磷迁移转化具有重要影响.南漪湖主要出入湖河口沉积...     

DISTRIBUTION AND GRAIN-SIZE PARTITIONING OF METALS IN BOVFOM SEDIMENTS OF AN EXPERIMENTALLY ACIDIFIED WISCONSIN LAKE1

ABSTRACT: A study of concentrations and distribution of major and trace elements in surficial bottom sediments of Little Rock Lake in northern Wisconsin included examination of spatial variation and grain-size effects. No significant differences with respect to metal distribution in sediments were observed between the two basins of the lake, despite the experimental acidification of one of the basins from pH 6.1 to 4.6. The concentrations of most elements in the lake sediments were generally similar to soil concentrations in the area and were well below sediment quality criteria. Two exceptions were lead and zinc, whose concentrations in July 1990 exceeded the criteria of 50 μg/g and 100 μg/g, respectively, in both littoral and pelagic sediments. Concentrations of some elements, particularly Cu, Pb, and Zn, increased along transects from nearshore to midlake, following a similar gradient of sedimentary organic carbon. In contrast, Mn, Fe, and alkali/alkaline-earth elements were at maximum concentrations in nearshore sediments. These elements are less likely to partition to organic particles, and their distribution is more dependent on mineralogical composition, grain size, and other factors. Element concentrations varied among different sediment grain-size fractions, although a simple inverse relation to grain size was not observed. Fe, Mn, Pb, and Zn were more concentrated in a grain-size range 20–60 tm than in either the very fine or the coarse fractions, possibly because of the aggregation of smaller particles cemented together by organic and Fe/Mn hydrous-oxide coatings.     

LONG-TERM PATTERNS OF WATER QUALITY IN A MANAGED WATERSHED IN OREGON: 1. SUSPENDED SEDIMENT1

The cumulative effects of forest management activities on water quality at a downstream point were monitored from 1972-1980 during development of a watershed for timber resources. Suspended sediment concentration and turbidity were measured at two hydrologic stations which bracketed a 10-km reach of the Middle Santiam River in the Western Cascades of Oregon as it flowed through an 8000-ha block of intensively managed forest land. Slope failures often accompany road building and harvesting in steep forested watersheds and pose the most serious threat to water quality. Although 180 km of road were constructed and 3400 ha of old-growth forests were harvested from slopes averaging over 60 percent, long-term changes in sediment yields remained undetectable during the period of measurement. The geologic characteristics of the basin and the road construction and maintenance techniques as prescribed by Oregon's forest practice regulations helped to minimize the occurrence of slope failures so that long-term changes in suspended sediment export rates did not occur. Throughout the nine-year measurement period, seven slope failures which added sediment directly to streams produced measurable short-term responses at the downstream sampling location, but these erosion events were too small and too infrequent to produce long-term changes in sediment yield from the watershed.     

地面水中叶枯灵的高效液相色谱测定

本文采用反相高效液相色谱法，在质控条件下，对河水，塘水两种地面水中叶枯灵的检验方法进行了测试，用Shimapck ODS柱为分析柱，以甲醇：水＝50：50为流动相，并用冰醋酸调PH至4－5，紫外检测波长281nm，两种水样的平均回收率分别为91．7－96．3％，90－95．8％，相对标准偏差为4．3％，最低检出限为0．0261mg/l，为地面水中叶枯灵卫生标准的实施提供了简便，灵敏，正确的配套测试手段。     

Industrial Tailings in Traunsee (Austria) Revisited: The Status of 1999

Alkaline tailings from a salt work and a soda plant have been pumped into the southernmost part of Traunsee at Ebensee for many decades. A survey in 1981 showed an accumulation of more than 3 × 10⁶ m³ alkaline mud in the Bay of Ebensee and the existence of slumping structures and turbidites in the profundal zone of the lake. A new survey of the industrial tailings has been performed in 1999. Compared to the earlier survey, the accumulation in the Bay of Ebensee has grown to >4 × 10⁶ m³, which suggests an average yearly input of 90 000 m³. Slumping structures and turbidites document the unstable situation of the tailings near the waste inlet. The lake area occasionally affected by the turbidity currents in the profundal zone has increased to 19%. Within the central profundal area these tailings reach <1 m in thickness.