利用top-down技术评定ICP-MS法测定水中镉的测量不确定度

根据不同分析人员在连续30周内水质中镉实验室质控样品的分析数据,采用top-down技术中的控制图法评定电感耦合等离子体质谱(ICP-MS)法测定水中镉的不确定度。方法依据《生活饮用水标准检验方法金属指标》(GB/T5750.6—2006 1.5)测定镉质量浓度为2.00μg/L的质控样品,测定均值为2.010μg/L,通过评定,不确定度为0.100μg/L。     

ICP-MS法测定水稻田表层土壤中重金属元素Zn、Cd、Pb、Cu、Cr、Mn的研究

报道了用ICP-MS法直接测定水稻田表层土壤中的重金属元素Zn、Cd、Pb、Cu、Cr、Mn含量的方法.土壤样品经HNO3-HF-HClO4彻底消化后,加入内标元素45Sc、115In、204Tl,采用内标法进行测定,有效地克服了基体效应、接口效应及仪器波动所产生的影响;通过优化仪器的工作参数,选择待测元素适当地测定同位素,有效克服了因质谱干扰所带来的影响.对污染土壤标准物质(编号GBW08305)进行测定,测定结果与标准值相吻合.该方法的加标回收率是98.0%～102.0%,相对标准偏差是2.2%～3.5%,具有线性范围宽、简单、快速、准确等特点.     

好氧反硝化脱氮气态中间产物的研究分析

对好氧反硝化处理硝氮废水产生的中间气态产物进行了研究。结果发现系统的好氧反硝化会产生一定量的中间气态产物NO、N2O,但逸出量相对较少,在进水COD/N=10时,NO逸出0.43mg,占总脱氮量的0.17%,N2O逸出9.17mg,占总脱氮量的3.55%;进水COD/N=20时,NO逸出0.23mg,占总脱氮量的0.05%,N2O为0.78mg,占总脱氮量的0.17%。同时发现碳源是影响好氧反硝化进程的主要因素。     

Calibration for the determination of 19 trace elements in serum and urine

A fast, high-throughput and accurate method was developed for determination of Al, As, Ba, Cd, Co, Cr, Cs, Cu, Fe, Mn, Ni, Pb, Se, U, Zn, Sb, Sn, I and Hg in urine and serum by inductively coupled plasma mass spectrometry. The samples were directly analyzed after 1/20 (v/v) dilution in 0.4% (v/v) HNO₃ and 0.005% Triton X-100. Three calibration modes were tested: aqueous and matrix matching with urine and serum. The accuracy was tested using reference materials of serum, urine and spiking. Results showed that the use of matrix matching calibration reduced the interferences and improved the recoveries for Al, Co, Pb and I in urine. The matrix matching did not affect the results considerably for serum. When serum was spiked with As, Co, Cs, Pb, U, Hg, I, Ba, Al, Cr and Ni, only matrix matching presented good recoveries. Helium was used as a collision cell gas reducing effectively polyatomic interferences for Al, Mn, Cu, Ni, Cr, Zn, As and Fe. Selection of the best internal standard was carried out for each element. The use of diluted HNO₃ improved the limit of detection. Finally, the method was applied successfully in samples of urine from workers occupationally exposed.     

我国东北地区土壤铀同位素水平、分布和来源

系统采集了我国东北地区132个表层土壤样品,采用混合酸全溶分解样品,使用UTEVA萃取色谱分离样品溶液中的铀,应用串联四极杆电感耦合等离子体质谱（ICP-MS/MS）测量样品溶液中²³⁸U、²³⁵U、²³⁴U,获得了研究区域表层土壤中3种铀同位素浓度水平和分布.首次大范围报道该地区表土中²³⁴U水平,发现在部分土壤中²³⁴U发生明显的同位素分馏.²³⁵U/²³⁸U原子比值分布显示区域大气核武器试验的放射性颗粒物在山脉迎风坡有明显沉积,导致大兴安岭等山脉的西侧²³⁵U/²³⁸U原子比值较高.但该区域铀同位素整体上处于环境本底水平,受人类核活动影响较小.来源分析表明研究区域表土中铀主要来源于成土母岩的岩石风化以及人类的工业和农业活动.     

水中硼测定方法比对研究

对姜黄素分光光度法、甲亚胺-H分光光度法和电感耦合等离子体-质谱法测定硼的方法性能进行了比对研究,为硼的测定方法的选择提供了良好的科学依据。     

ICP—MS法测定饮用水中的铅

采用ICP—MS法对饮用水中的铅进行了分析测定。并进行了载气流量的选择、定量离子质荷比的选择和内标的选择等实验．本实验铅的质荷比选用206,207和208三个加在一起计算。方法的检测限为0．5×10-3mg／L,精密度实验的变异系数为3．25％～7．63％。     

ICP-MS半定量分析及其应用

ICP-MS具有等离子发射光谱检测能力高、测量速度快、测量元素多等特点,能对样品中存在元素进行定性及半定量分析,半定量分析准确度为±30%.同时还能快速确定样品中存在的元素及浓度范围.     

用同位素方法评估天津市汽油无铅化进程

用同位素技术研究和评估天津市汽油无铅化进程.采用稀酸浸出法处理天津市1994～2001年冬春季节123个玻璃纤维滤膜大气颗粒物样品,测量了大气铅浓度和同位素丰度比(²⁰⁶Pb/²⁰⁷Pb).结果表明,1994～2001年是我国汽油无铅化的重要时段,这期间大气颗粒物样品铅浓度有所下降,铅的同位素丰度比逐渐增加,表征了汽油无铅化进程中汽车尾气的贡献率减少,其他来源的贡献率上升.在汽油无铅化后,我国还应加强对铅污染的综合治理.     

A pilot study on iodine in soils of Greater Kabul and Nangarhar provinces of Afghanistan

A robust and rapid methodology for the determination of iodine by inductively coupled plasma mass spectrometry in environmental samples is presented. Data were initially obtained for the validation of the analytical measurements, using 17 commercially available soil reference materials. The methodology was then tested on soil and water samples collected in Afghanistan where iodine deficiency and its effects are reportedly prevalent. Sample collections were conducted in Greater Kabul; the iodine in agricultural soils was determined to be in the range of 1.6–4.2 mg/kg and that in water drawn for drinking and irrigation was found to range from 9.9 to 22.7 μg/L. Samples were also collected in a second region, Nangarhar province, which is located to the east of Kabul, where goitres in the local population had been reported. The iodine content in soils and water at this location was 0.5–1.9 mg/kg and 5.4–9.4 μg/L, respectively. The organic content of soils in Kabul was found to be in the range of 1.9–4.2%; in Nangarhar, organic content ranged from 1.7 to 4.5%. All of the Afghan soils were slightly alkaline at pH 7.6–8.2.