薄膜梯度扩散-分光光度法富集测量水中痕量Mo (VI)

建立了薄膜梯度扩散(DGT)- 硫氰酸钾(PT)分光光度法(DGT-PT法)富集测量水中痕量Mo (VI) 的分析方法。本研究先以聚季铵盐(PQAS)溶液为结合相的DGT技术 (PQAS DGT) 原位分离富集水中Mo (VI),再以PT分光光度法测定DGT结合相中Mo (VI)的含量,最后依据DGT方程计算水中Mo (VI)的浓度。DGT-PT法测得配制水中Mo ( VI) 的回收率为96.3% ~ 101.3%,相对标准偏差(RSD)为1.3% ~4.0%;测得工业废水中Mo (VI) 的浓度为27.13 ~ 121.79mg/L,加标回收率为96.0% ~ 101.6%。当采样时间为48h,PQAS DGT对水中Mo (VI) 富集近18倍,可显著降低分析方法的检测限,实现水中痕量Mo (VI) 的定量检测。     

薄膜梯度扩散-分光光度法富集测量水中痕量Cr(VI)

建立了薄膜梯度扩散(DGT)-二苯碳酰二肼(DPC)分光光度法富集测量水中痕量Cr(VI)的分析方法。先以聚季铵盐(PQAS)溶液为结合相的DGT技术(PQAS DGT)原位分离富集水中Cr(VI),再以DPC分光光度法测定DGT结合相中Cr(VI)的含量,最后依据DGT方程计算水中Cr(VI)的浓度。DGT-DPC法测得配制水中Cr(VI)的回收率为95.1%~101.3%,相对标准偏差为1.60%~3.58%;测得工业废水中Cr(VI)的浓度为18.54~137.61μg/L,加标回收率为94.3%~101.8%。当采样时间为48h,PQAS DGT对水中Cr(VI)富集近10倍,可显著降低分析方法的检测限,实现水中痕量Cr(VI)的定量检测。     

薄膜梯度扩散-分光光度法富集测量水中痕量Cr(Ⅵ)

建立了薄膜梯度扩散(DGT)-二苯碳酰二肼(DPC)分光光度法富集测量水中痕量Cr(Ⅵ)的分析方法.先以聚季铵盐(PQAS)溶液为结合相的DGT技术(PQAS DGT)原位分离富集水中Cr(Ⅵ),再以DPC分光光度法测定DGT结合相中Cr(Ⅵ)的含量,最后依据DGT方程计算水中Cr(Ⅵ)的浓度.DGT-DPC法测得配制水中Cr(Ⅵ)的回收率为95.1％～101.3％,相对标准偏差为1.60％～3.58％;测得工业废水中Cr(Ⅵ)的浓度为18.54 ～ 137.61μg/L,加标回收率为94.3％～101.8％.当采样时间为48h,PQAS DGT对水中Cr(Ⅵ)富集近10倍,可显著降低分析方法的检测限,实现水中痕量Cr(Ⅵ)的定量检测.     

壳聚糖富集火焰原子吸收法测定天然水中痕量镉

提出了壳聚糖分离富集火焰原子吸收法检测水中痕量镉的新方法。研究了富集的最佳条件及洗脱方法。回收率达98％,灵敏度0.021μg·L~(-1)。方法灵敏度高,选择性好,用于天然水中痕量镉的测定,获得满意结果。     

泡沫塑料吸附-火焰原子吸收光谱法测定水中痕量镉

用原子吸收光谱法测定水中镉时,为提高测定灵敏度,多采用有机试剂萃取富集的方法[1]。但萃取所用的试剂挥发性强、毒性大,对环境污染较大,损害人体健康。试验中发现,在I-存在的条件下,泡沫塑料(以下简称泡塑)可定量富集磷酸介质中以[CdI4]2-形式存在的镉,并且富集后的镉可在硫脲溶液中得到完全解脱。本文对该体系进行了研究,建立了测定水中痕量镉的方法,该方法中镉的吸附率高,解脱方便,测定结果稳定可靠,用于水样中痕量镉的分析,结果满意。1试验部分1.1仪器与试剂GGX-9型原子吸收光谱仪。镉标准溶液:按常规方法配制成1 g·L-1,使用时逐级…     

原子捕集火焰原子吸收法测定水中镉

采用自制原子捕集装置，选择了镉在不锈钢管上捕集的合适条件，使测镉的灵敏度比常规火焰原子吸收法提高了116倍。应用于工业废水中痕量镉的测定，获得满意结果。     

阴离子交换树脂分离富集水中痕量镉

先用草酸处理水样中的镉离子,生成的[Cd(C2O4)2]2-络阴离子通过强碱性阴离子交换树脂分离富集,最后用火焰原子吸收分光光度法测定了水样中的痕量镉。该法简便,选择性好,富集倍数高,应用于实际水样的检测,回收率为98%~102%,结果令人满意。     

萃取色层富集原子吸收光谱法测定环境水中痕量铜

利用固定有双硫腙的活性硅胶萃取色层法富集环境水中痕量铜,0.1mol·L-1盐酸-50g·L-1硫脲作为洗脱剂,火焰原子吸收尤谱法测定。研究了富集剂的吸附容量,最佳吸附条件和洗脱条件。试验表明,该富集剂的使用寿命长远20次,富集倍数高达200倍;对于同浓度水样平行测定6次,其相对标准偏差为3.2％;应用于实际水样分析,加标回收率在95％～110％之间。     

共沉淀分离富集原子吸收光谱法测定氯化物中痕量镉

研究了吡咯烷二硫代氨基甲酸铵 (APDC)及其氧化产物 (DPTD)体系在 pH3.5条件下定量共沉淀氯化物中痕量镉 ,用FAAS测定 ,检出限可达 1.3× 10 - 3mg·L- 1。加标回收率在 97%～ 10 3%之间 ,克服了基体干扰 ,取得了较满意的结果。     

薄膜梯度扩散技术结合相研究进展

薄膜梯度扩散(DGT)技术是一种新型原位被动采样技术,已被广泛应用于水体、土壤、沉积物中目标物的采集与测量。结合相是DGT技术的重要组成部分,决定了与目标物的结合能力、结合速度、结合容量以及目标物的形态选择性等。DGT结合相分为固态结合相和液态结合相。本文重点综述了树脂、氧化物、无机盐、活性炭、改性硅胶、分子印迹、共聚物、复合、液态等结合相在DGT技术中的应用,展望了DGT结合相的发展前景。     

Determination of osmium in waste water by graphite furnance atomic absorption spectrometry

The determination of osmium in waste water by electrothermal atomic absorption spectrometry (AAS) with a graphite furnace atomiser has been investigated. The atomisation characteristics of osmium on the atomiser were found to result in optimal ashing and atomisation temperatures of 300–500 and 3180 °C, respectively.The characteristic mass (the mass of element giving 0.0044 abs.) of osmium after optimization was found to be 1.6ng, which is better than obtained with flame AAS and ultraviolet/visible (UV) absorption spectrophotometry. The detection limit (s/n = 3) was 3.6ng (or 0.36 (g ml^–1). The relative std. deviation obtained with graphite furnace AAS was 3.0%.The interference caused by large amounts of common cations and anions in waste water were evaluated and thiourea as matrix modifier was shown to be able to eliminate many interferences. The recovery of osmium spiked in waste water was considered almost satisfactory at the 1–50 g ml^–1 range and the results were shown to well agree with the analytical values obtained by UV absorption spectrophotometry.     

Determination of cadmium in tobacco smoke and zinc in tap water by solvent extraction flame atomic absorption spectrometry

Procedures are described for the determination of cadmium in tobacco smoke and zinc in tap water by flame atomic absorption spectrometry after chelation with benzyl 2-pyridyl ketone 2-pyridylhydrazone and extraction with isobutyl methyl ketone. Calibration graphs in the organic layer were linear up to 1.3 g/ml, with sensitivities of 80 ng/ml (Zn) and 71ng/ml (Cd), and limits of detection of 49 ng/ml for zinc and 38 ng/ml for cadmium. RSD values were 2.9% at 0.42 g/ml (Cd) and 4.7% at 0.17 g/ml (Zn).     

超级微波消解-石墨炉原子吸收光谱法测定虾蛄中镉含量

目的 比较超级微波和普通微波消解方法,建立超级微波-石墨炉原子吸收法测定虾蛄中镉的方法。方法 分别采用超级微波和普通微波消化大虾标准物质,对比消解效果,优选消解方法,采用石墨炉原子吸收法测定,优化基改改进剂、灰化温度等工作参数,确定最佳的分析方法,同时加标回收验证方法的准确性与可靠性。结果 两种消解方法下测得结果均在参考值范围内,在选定方法条件下,镉在质量浓度0.0～2.0 μg/L范围内线性关系良好,相关系数γ=0.999,检出限为0.04 μg/L,定量限为0.12 μg/L,加标回收的准确度为88.5%～105.2%,精密度为2.93%～4.92%。结论 超级微波消解法优于普通微波消解,其耗酸量低、高效便捷、测得数据准确稳定,便于在基层推广,适用于批量虾蛄样品的镉污染监测工作。     

Determination of nickel in water by electrothermal atomic absorption spectrometry with preconcentration on a tungsten foil

A preconcentration method for nickel in waters involving adsorption on tungsten foil, followed by electrothermal atomic absorption spectrometry (ETAAS) with a tungsten tube atomizer is described. The most suitable pH for nickel adsorption was 5 and the optimum immersion time was 2 min. Severe interferences from co-existing elements (Al, Ca, Cu, Fe, K, Mg, Na, Pb and Zn) on the Ni AA signal were observed. Under optimal conditions, the preconcentration of nickel on W foil could eliminate interferences from these elements. The detection limit of nickel by preconcentration-ETAAS was 0.1 ng/ml (3S/N). The method with preconcentration on tungsten foil was applied to the determination of nickel in river water. The recovery of spiked nickel was 93–102%. The tungsten foil preconcentration method is sensitive, simple, and convenient. This adsorption method can be utilized inin situ-sampling of ultra-trace nickel in environmental samples (water). Furthermore, after sampling it is easy to carry and store the W-foil without contamination for long time.     

流动注射在线离子交换预富集火焰原子吸收光谱法测定水样中微量锰

提出了以732强酸型阳离子树脂作填充材料,流动注射在线离子交换预富集火焰原子吸收光谱法测定水样中微量锰的分析方法。优化了各项化学条件和流路参数等,考察了共存离子的干扰。富集倍数可达24倍,分析速度为15～20样/h,检出限为2.0ng/mL,相对标准偏差为2.8%(n=15)。对雨水加标回收,回收率为97%～103%。     

超级微波消解-石墨炉原子吸收光谱法测定不同类型土壤中的镉

采用超级微波消解仪对样品进行前处理,对比不同消解体系的消解效果,选择合适的消解体系,采用石墨炉原子吸收光谱法测定镉浓度,同时优化基体改进剂、灰化温度等工作参数,确定最佳的分析条件。探讨并建立超级微波消解-石墨炉原子吸收光谱法测定不同类型土壤镉含量的方法。在最优条件下,标准曲线在0～1.0μg/L浓度范围内线性关系良好,相关系数r=0.999,检出限浓度为0.04μg/L,定量限浓度为0.12μg/L,方法准确度为94.5%～110%,相对标准偏差RSD为0.60%～5.4%,方法应用于不同类型土壤标准物质镉的测定,测得结果均在标准值范围内。方法简便快捷、准确高效、用酸量低、节约环保,便于在基层推广,适用于批量处理不同类型镉污染土壤样品。     

On-line simultaneous pre-concentration procedure for the determination of cadmium and lead in drinking water employing sequential multi-element flame atomic absorption spectrometry

An on-line pre-concentration system for the sequential determination of cadmium and lead in drinking water by using fast sequential flame atomic absorption spectrometry (FS-FAAS) is proposed in this paper. Two minicolums of polyurethane foam loaded with 2-(6-methyl-2-benzothiazolylazo)-orcinol (Me-BTAO) were used as sorptive pre-concentration media for cadmium and lead. The analytical procedure involves the quantitative uptake of both analyte species by on-column chelation with Me-BTAO during sample loading followed by sequential elution of the analytes with 1.0?mol?L^?1 hydrochloric acid and determination by FS-FAAS. The optimisation of the entire analytical procedure was performed using a Box–Behnken multivariate design utilising the sampling flow rate, sample pH and buffer concentration as experimental variables.

The proposed flow-based method featured detection limits (3σ) of 0.08 and 0.51?µg?L^?1 for cadmium and lead, respectively, precision expressed as relative standard deviation (RSD) of 1.63% and 3.87% (n?=?7) for cadmium at the 2.0?µg?L^?1 and 10.0?µg?L^?1 levels, respectively, and RSD of 6.34% and 3.26% (n?=?7) for lead at the 5.0?µg?L^?1 and 30.0?µg?L^?1 levels, respectively. The enrichment factors achieved were 38.6 and 30.0 for cadmium and lead, respectively, using a sample volume of 10.0?mL. The sampling frequency was 45 samples per hour. The accuracy was confirmed by analysis of a certified reference material, namely, SRM 1643d (Trace elements in natural water). The optimised method was applied to the determination of cadmium and lead in drinking water samples collected in Santo Amaro da Purificação City, Bahia, Brazil.