便携式分光光度计测定水中总磷

采用螺旋口瓶盖密封消解 -便携式分光光度计建立了环境水样中总磷的分析方法。该法与 GB1 1 893 89(过硫酸钾 -钼蓝法 )方法有良好的可比性。分析结果具有良好的准确性与重现性 ,方法对标准样品的准确度在 98%以上 ,检出限为 0 0 2 2 mg L,变异系数在 0 6 %～ 2 4 %之间 ;实际水样的测试结果与 GB1 1 893-89法的偏差为 2 %～ 4 % ;工业废水的加标回收率为 1 0 2 %～ 1 0 5 %。该方法可应用于污染源的抽查和突发性水环境污染事故的现场监测。     

毛细管柱气相色谱法测定水中痕量拟除虫菊酯杀虫剂

采用石油醚萃取水样 ,萃取液经氮气吹扫浓缩后 ,用气相色谱仪对水样中拟除虫菊酯杀虫剂——甲氰菊酯、三氟氯氰菊酯 (功夫 )、高效氯氰菊酯、氰戊菊酯、溴氰菊酯进行了定量测定。由于毛细管柱的高柱效和微池 ECD的高灵敏度 ,使得上述目标组分与水样中的其它杂质能达到较好的分离 ,即使含量极低也能被检出。本方法省去了样品萃取液的净化处理这一步骤 ,可较快地测定拟除虫菊酯杀虫剂 ,在污染事故应急监测方面具有实用性。     

A simple ligandless microextraction method based on ionic liquid for the determination of trace cadmium in water and biological samples

A simple and efficient ionic liquid-based ligandless microextraction method has been developed for preconcentration of cadmium ions (Cd²⁺) as a step prior to its determination by flame atomic absorption spectrometry (FAAS) with a micro-sample introduction system. In this approach, the ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C₄mim][PF₆] and ethanol were used as extractant and dispersive solvents to preconcentrate the Cd²⁺ in different waters, acid digested scalp hair, and nail samples. Some analytical parameters influencing the extraction efficiency of Cd²⁺ and its subsequent determination, including pH, IL volume, dispersant solvent volume, sample volume, temperature, incubation time, and matrix effect, were optimized. Under optimal conditions, the limit of detection (LOD), limit of quantification (LOQ), and enhancement factor (EF) were 0.4 μg L^?1, 1.3 μg L^?1, and 50, respectively. The relative standard deviation (RSD) of 100 μgL^?1 Cd²⁺ was 4.3% (n = 6). The validity of the proposed method was checked by determining Cd²⁺ in certified reference material (TM-25.3 fortified water) and standard addition; the results showed sufficient recovery (>98%) of Cd²⁺ within the certified value. The method was applied for preconcentration and determination of cadmium in waters and biological samples.     

Synthesis of 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 resin: Applications for the separation and preconcentration of trace metal ions prior to their determination by inductively coupled plasma atomic emission spectrometry

A simple, sensitive column solid-phase extraction procedure for separation and preconcentration of Cu(II), Ni(II), Co(II), and Cd(II) in spiked and natural water samples using 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 (XAD-4-DHN) chelating resin prior to their determination by inductively coupled plasma atomic emission spectrometry was discussed. The optimum experimental parameters such as pH, volume of sample and eluent, flow-rates of uptake and stripping, and sorption capacity of the chelating resin, were evaluated. The effect of the electrolytes and the cations on the preconcentration of metal ions was also investigated. The chelating resin could be reused for more than 20 cycles of sorption–desorption without any significant change (<1.0%). Recoveries obtained from this method range from 96 to 102% with R.S.D of 2.50 (n = 4). The detection limits for Cu(II), Ni(II), Co(II), and Cd(II) were found to be 1.9, 0.9, 1.2 µg, and 1.4 µg L^?1, respectively. The proposed method was applied for the determination of Cu(II), Ni(II), Co(II), and Cd(II) in spiked, tap water, and river water samples.