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铬(Ⅵ)-二乙基二硫代甲酸钠共沉淀-原子吸收光谱法测定环境水样中铁、锰、锌、镉 被引量:3

AAS Determination of Iron,Manganese,Zinc,Cadmium in Environmental Water Samples After Enrichment by Coprecipitaion with Cr(Ⅵ)-DDTC
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摘要 提出了以二乙基二硫代甲酸钠螯合铬(Ⅵ)作为载体共沉淀富集水体中铁、锰、锌和镉的方法。沉淀经离心分离,甲基异丁酮溶解后,以微量进样300 μL火焰原子吸收光谱法测定铁、锰、锌,以石墨炉原子吸收光谱法测定镉。用水样10.0 mL,在pH 4.6的邻苯二甲酸氢钾缓冲介质中加入20 g·L-1重铬酸钾溶液150 μL,20 g·L-1 DDTC溶液1.0 mL可达到完全共沉淀分离,所得沉淀经离心分离后用甲基异丁酮2.0 mL溶解,并用于AAS分析。在优化的条件下,铁、锰、锌和镉的检出限(3σ)分别为9.0,6.8,1.8,0.03 μg·L-1,相对标准偏差(n=6)在1.8%-3.8%之间。方法用于实际水样的测定,用标准加入法测得回收率在93.7%-105.0%之间。 . Trace amounts of Fe ( Ⅲ ), Zn ( Ⅱ ), Mn ( Ⅱ ) and Cd ( Ⅱ ) in environmental water sample was enriched by coprecipitation by DDTC-Cr precipitate. The sample solution (10. 0 mL) was adjusted to pH 4.6 with phosphate buffer solution and 150μL of 20 g . L-1 K2Cr2O2 solution were added to form DDTC-Cr precipitate. One mL of 20 g . L-2 DDTC solution was necessary for complete to precipitation of the 4 elements. The precipitates were separated by centrifugation and dissolved in 2. 0 mL of MIBK, which was used for AAS determinatiorL The volume of the MIBK solution introduced for AAS analysis was 300 μL, and Fe( Ⅲ ), Zn( Ⅱ ), Mn(Ⅱ ) and CA( Ⅱ ) were determined by FAAS, while CA( Ⅱ ) was determined by GFFAAS. Under the optimum conditions, values of detection limit (3s/k) found were (μg . L-1) 9. 0 (for Fe), 6. 8 (for Mn), l. 8 (for Zn) and 0. 03 (for CA). Values of RSD's (n=6) found were in the range of 1.8% --3. 8% respectively. Recovery was tested on the base of samples of sea water and river water by standard addition method, giving results in the range of 93. 7%--105.0% .
作者 祝旭初
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2010年第1期84-86,共3页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
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