碱性微波提取-ICP/MS法测定土壤中六价铬

采用碱性微波提取法处理土壤样品,用电感耦合等离子体质谱（ICP/MS）法测定试样中的六价铬,以标准物质测定相对误差的绝对值作为试验指标建立正交模型,确定碱性微波消解的提取温度95 ℃、提取时间30 min、氯化镁用量005 g、提取液体积6 mL为最佳试验条件,采用He碰撞池技术和在线内标分别消除基体带来的质谱和非质谱干扰。条件优化后,方法检出限为0.10 mg/kg,实际样品6次测定结果的RSD分别为13.0%和5.7%,加标回收率为120%和106%。将该方法用于有证标准土壤样品的测定,测定结果均在标准值范围内。     

电感耦合等离子法测定环境积尘中铅的研究

用细毛刷清扫收集普通居民房顶积尘,参照土壤样品预处理方法-普通酸分解法处理样品,以国标样品、不确定度实验、加标回收实验为质控手段,探索采用电感耦合等离子法测定环境积尘中铅的含量。实验结果表明,该法能将积尘样品完全消解,且电感耦合等离子法测试方法性能稳定、快速、准确,优于其他方法。     

Speciation of mercury in South African coals

Total mercury (Hg_TOT) concentrations were determined by inductively coupled plasma mass spectrometry (ICP MS) for South African Highveld coals. The distribution of Hg in coals was investigated using a four-stage sequential leaching protocol and isotope dilution/gas chromatography coupled to ICP MS (ID-GC-ICP MS). The results show that Hg_TOT ranged from 144 to 303?µg?kg^?1 with a mean of 199?±?26?µg?kg^?1, while Hg_TOT leached from coals using different solvents ranged between 103 and 310?µg?kg^?1 (mean: 218?±?60?µg?kg^?1). Hg leaching rates of 53–78% were achieved in crushed coals. Hg⁰, Hg²⁺, and CH₃Hg⁺ were identified in all coals. CH₃Hg⁺ in studied coals ranged between 0.1 and 0.4 (mean: 0.2) µg?kg^?1. GC ICP MS chromatograms also showed unknown Hg peaks which were identified as other organomercury species such as ethylmercury. Modes of occurrence of Hg in coals were variable with the organic-bound (37–40%) and the sulfide-bound (37–39%) being the dominant mercury forms. Increasing the HCl concentration in the used protocol increased the amount of Hg leached (16%) during this step.     

Monitoring of heavy metals and butyltin compounds in coastal waters of Ligurian Sea: Results of a mussel watch project

From December 1994 up to October 1995 a “Mussel Watch Project”; was carried out to assess the quality of water of the Ligurian Sea and to identify the possible sources of heavy metal pollution. Several metals and organotin compounds were measured in mussels (Mytilus galloprovincialis, Lam) transplanted in different months from a marine farm to eight sites of the Ligurian coast.

Spatial differences and temporal trends in tissue concentrations of Zn, Cu, Ni, Cr, Fe, Al, V, Cd and Mn were evaluated. Concentrations resulted in the same range as those obtained in a previous Mussel Watch Project carried out in the same area. In general, areas of known pollution display high concentrations of these metals, but also some areas not greatly influenced by human activities showed high concentrations of some metals.

Data from this study show little evidence of any overall seasonal pattern except for Cu, Zn and V, concentrations of which were a function not only of sampling site, but also of reproductive cycle.

Organotin compounds show differences in terms of both concentration and speciation between the investigated sites.     

母乳与牛乳中微量元素的比较

用ＩＣＰ－ＡＥＳ法对母乳和牛乳中Ｋ、Ｎａ、Ｃａ、Ｍｇ、Ｐ、Ｆｅ、Ａｌ、Ｚｎ、Ｓｒ、、Ｐｂ、Ｍｎ、Ｂａ和Ｃｕ等１３种元素含量进行了测定。结果发现母乳与牛乳的营养成分差异较大。研究了深入探讨微量元素在人体内重要的生理功能提供了有用的参考数据。     

沉淀分离富集-电感耦合等离子原子发射光谱测定土壤中可溶态稀土元素

研究电感耦合等离子体原子发射光谱测定土壤中微量可溶态稀土元素的方法。在适宜的ｐＨ＝１０－１１条件下,以ＭｇＣｌ２为载体沉淀分离除去浸提液中的大部分基体杂质如Ｎａ＾＋,Ａｃ＾－,Ｃａ＾２＋,Ｍｇ＾２＋等,有效地消除了这些杂质的干扰,提高了测定方法的准确度;同时,待测可溶态稀土元素被沉淀集,样品中总稀土及单一稀土加标回收率为８８％－１１０％,样品测定结果满意,方法简便快速。     

高分辨电感耦合等离子体质谱法测定地下水中稀土元素

采用高分辨电感耦合等离子体质谱法测定地下水中14种稀土元素,并选择Rh作内标,可消除测定中的质谱干扰和非质谱干扰,使方法在0μg/L~100μg/L范围内线性良好。方法检出限为0.002μg/L~0.005μg/L,实际水样的加标回收率为80.0%~117%,RSD为2.1%~3.8%。     

超声提取-电感耦合等离子体质谱法分析土壤中重金属化学形态

采用超声提取处理土壤样品,用ICP-MS分析样品中Cu、Zn、Pb、Cd、Ni、Cr等6种重金属元素形态,通过试验分析超声提取时土壤样品粒径、超声提取时间对提取效率的影响。方法在0.500μg/L~100μg/L之间线性良好,检出限为0.007μg/L~0.8μg/L,实际样品测定结果的RSD为4.7%~22.7%。土壤中重金属4种形态之和的总量与全量的相对偏差为11.0%~36.4%。将该方法与连续振荡法的试验结果比对,表明两方法对土壤样品的提取效率无显著性差异。     

微波消解-ICP/MS法测定水系沉积物中多种元素

采用微波消解-电感耦合等离子体质谱法测定水系沉积物中12种元素,通过优化试验相关条件消除质谱干扰和非质谱干扰对测定的影响,使方法在0μg/L~200μg/L范围内线性良好,当取样质量为0.25 g,定容体积为50 m L时,各元素的方法检出限为0.002 mg/kg~0.05 mg/kg。用该方法测定沉积物标准物质,6次测定结果均在标准值范围内,RSD为1.3%~6.1%,实际样品的加标回收率为83.0%~97.0%。     

不同溶样方法测定石灰石多组分含量的研究

采用铂金坩蜗熔融、银坩埚熔融和盐酸直接溶解方法测定了石灰石中多组分的含量。并同时使用ICP测定石灰石中SiO2、Al2O3、Fe2O3的成分。研究结果表明：在测定石灰石中CaO、MgO和Fe2O3含量时,采用盐酸直接溶解方法,具有方法简单、分析快速的优点,且准确度能达到要求;在测定石灰石中CaO、MgO、SiO2、Al2O3,和Fe2O3含量时,采用银坩埚代替铂金坩埚熔样,具有成本低的优点,且准确度亦能达到要求;采用ICP测定标准石灰石样的SiO2、Al2O3和Fe2O3组分具有快速、简单和准确度高的特点。