Highly precise and reliable determination of heavy metals in soil micro-arthropod tissues remains a challenge because of the small size of the animals and their typical low abundance in metal-contaminated agricultural...Highly precise and reliable determination of heavy metals in soil micro-arthropod tissues remains a challenge because of the small size of the animals and their typical low abundance in metal-contaminated agricultural soils. The present study sought to develop a method for cadmium (Cd) determination in soil micro-arthropods by optimizing the sample digestion procedure, reducing sample weight, modifying sample pre-treatment and validating the methodology with field samples. The optimized digestion conditions comprised a sample mass of 50-150 μg, digestion reagent of nitric acid:hydrogen peroxide (3:1), digestion temperature of 105 ℃, digestion period of 3 h and digestion volume of 30 μL. Defecation of the standard Collembola Folsomia candida (92 h) and the indigenous Collembola Onychiurus yodai (42 h) and ultrasonic cleaning of F. candida increased the accuracy of Cd determination. The recovery of Cd using the refined procedure was 98.9% and the limits of detection and quantification were 0.002 and 0.008 μg L-1, respectively. The within-batch precision values were 〈 3%. The Cd concentrations in the tissues of the Collembola Isotorna sp. collected from a range of metal-contaminated fields determined by the improved method were consistent with the Cd concentrations in the field soils. The results indicate that the optimized method can be used for more accurate or reliable determination of Cd concentrations in soil micro-arthropod tissues.展开更多
Isotope plays an important role in both tracing and dating in earth science, especially 87Rb-86 Sr system. With the development of earth science, whole-rock analysis can't sufficiently meet the requirements for scien...Isotope plays an important role in both tracing and dating in earth science, especially 87Rb-86 Sr system. With the development of earth science, whole-rock analysis can't sufficiently meet the requirements for scientific research and the micro-analysis becomes more and more significant. Laser ablation multi-collector inductively-coupled plasma mass-spectrometry(LA-MC-ICP-MS) has been extensively applied in micro-zone analysis due to its low sample-consumption, high accuracy, in situ and low requirements on matrix, but it is still difficult to accurately measure Sr isotope compositions especially for the samples with high Rb/Sr ratios and low Sr contents as it is restricted by severe quality discrimination and various types of mass spectrum interferences. Consequently, thermal ionization mass-spectrometry(TIMS), as the most accurate and precise method to analyze isotopic ratios, is still the most popular method of analyzing Sr ratios, especially for the samples with low Sr contents. This paper makes a systematic review on the high-precision Sr isotope analyses of low-Sr geological samples, including the micro-sampling technique, ultra-low procedural blank chemical method and TIMS measurement technique. The combination of ultra-low procedural blank and TIMS can be used to perform high-precision micro-analysis of the samples with ng magnitude, which will be undoubtedly an important direction for Rb-Sr geochronology, geochemistry and environmental studies.展开更多
基金supported by the National High Technology Research and Development Program of China (No. 2012AA101402-2)the National Natural Science Foundation of China (Nos. 41271264, 41325003)
文摘Highly precise and reliable determination of heavy metals in soil micro-arthropod tissues remains a challenge because of the small size of the animals and their typical low abundance in metal-contaminated agricultural soils. The present study sought to develop a method for cadmium (Cd) determination in soil micro-arthropods by optimizing the sample digestion procedure, reducing sample weight, modifying sample pre-treatment and validating the methodology with field samples. The optimized digestion conditions comprised a sample mass of 50-150 μg, digestion reagent of nitric acid:hydrogen peroxide (3:1), digestion temperature of 105 ℃, digestion period of 3 h and digestion volume of 30 μL. Defecation of the standard Collembola Folsomia candida (92 h) and the indigenous Collembola Onychiurus yodai (42 h) and ultrasonic cleaning of F. candida increased the accuracy of Cd determination. The recovery of Cd using the refined procedure was 98.9% and the limits of detection and quantification were 0.002 and 0.008 μg L-1, respectively. The within-batch precision values were 〈 3%. The Cd concentrations in the tissues of the Collembola Isotorna sp. collected from a range of metal-contaminated fields determined by the improved method were consistent with the Cd concentrations in the field soils. The results indicate that the optimized method can be used for more accurate or reliable determination of Cd concentrations in soil micro-arthropod tissues.
基金supported by National Natural Science Foundation of China (Nos. 90914007, 41125013)111 Plan (B07039)+1 种基金special fund of Ministry of Science and Technology,State Key Laboratory of Geological Processes and Mineral Resources (No. MSFGPMR201404)fund of Central University Fundamental Research (No. CUG090105)
文摘Isotope plays an important role in both tracing and dating in earth science, especially 87Rb-86 Sr system. With the development of earth science, whole-rock analysis can't sufficiently meet the requirements for scientific research and the micro-analysis becomes more and more significant. Laser ablation multi-collector inductively-coupled plasma mass-spectrometry(LA-MC-ICP-MS) has been extensively applied in micro-zone analysis due to its low sample-consumption, high accuracy, in situ and low requirements on matrix, but it is still difficult to accurately measure Sr isotope compositions especially for the samples with high Rb/Sr ratios and low Sr contents as it is restricted by severe quality discrimination and various types of mass spectrum interferences. Consequently, thermal ionization mass-spectrometry(TIMS), as the most accurate and precise method to analyze isotopic ratios, is still the most popular method of analyzing Sr ratios, especially for the samples with low Sr contents. This paper makes a systematic review on the high-precision Sr isotope analyses of low-Sr geological samples, including the micro-sampling technique, ultra-low procedural blank chemical method and TIMS measurement technique. The combination of ultra-low procedural blank and TIMS can be used to perform high-precision micro-analysis of the samples with ng magnitude, which will be undoubtedly an important direction for Rb-Sr geochronology, geochemistry and environmental studies.