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1.
微波消解-氢化物发生原子荧光法测定植物中汞和砷   总被引:2,自引:0,他引:2       下载免费PDF全文
采用微波消解-氢化物发生原子荧光法测定植物中汞和砷,优化了试验条件。汞在0μg/L-1.00μg/L、砷在0μg/L~20.0μg/L范围内线性良好,方法检出限汞为0.005mg/kg(以取0.1g样品消解定容至10mL计),砷为0.010mg/kg(以取0.1g样品消解定容至25mL计),植物样品测定的RSD≤4.5%,加标回收率为90.0%~107%。  相似文献   

2.
微波消解-石墨炉原子吸收法测定土壤中钒   总被引:3,自引:0,他引:3       下载免费PDF全文
建立了微波消解-石墨炉原子吸收测定土壤中钒的方法,优化了微波消解程序。方法在0μg/L~100μg/L范围内线性良好,以称样0.5000g、定容体积50mL计,方法检出限为0.2μg/g,环境土壤标准样品测定的RSD为2.5%,加标回收率为92.0%-104%。  相似文献   

3.
以氯化钯为基体改进剂,采用微波消解石墨炉原子吸收法测定土壤和沉积物中的铍,优化了微波消解条件,考察了共存元素对测定的干扰。方法在0μg/L~4.00μg/L范围内线性良好,检出限为0.01μg/g(以取样质量0.2000g、定容体积50mL计),标准样品平行测定的RSD为3.5%~6.7%,实际样品的加标回收率为84.0%-113%。  相似文献   

4.
采用微波消解-原子荧光光谱法测定大气细颗粒物中的砷,确定了最佳样品处理方法与测定条件。方法在0μg/L~40.0μg/L范围内线性良好,标准曲线相关系数达0.999以上,检出限为0.01μg/L。土壤标准品的测定值在标准值范围内,大气PM2.5滤膜样品加标回收率为96.0%~102%,5次平行测定的RSD为1.5%~3.6%。  相似文献   

5.
建立了微波消解-火焰原子吸收光谱法测定土壤中锶的方法.用微波消解土壤、电热板加热赶酸的方法对土壤样品进行前处理,优化了微波消解条件.检出限为3.0 mg/kg,加标回收率为84.7% ~ 107%,相对标准偏差均小于5%.方法快速、简便、准确度高、线性范围宽.  相似文献   

6.
采用程序控温石墨全自动消解仪消解土壤样品,原子荧光光谱法测定总砷。通过试验确定原子荧光光度计的最佳工作条件,使得该方法在2.00μg/L ~20.0μg/L 范围内线性良好,检出限为0.025 mg/kg,加标回收率在96.0%~10^5%之间,RSD为1.9%~3.3%。用该方法与国标法同时测定土壤标准样品和实际样品,结果无显著差异。  相似文献   

7.
以微波消解的方法处理土壤样品,采用硝酸—盐酸作为消解体系,设定最佳的样品前处理条件,使用水浴温恒加速砷的还原速率,同时利用仪器自动配置标准曲线。同时设定仪器最优测定条件,再用双道原子荧光光谱法测定土壤样品中的砷。通过国家标准参考物质和加标回收试验,对方法进行验证。结果表明,采用该方法,砷的浓度范围在2.00~20.00μg/L时校正曲线呈线性,检出限为0.003mg/Kg,测定土壤标准物质,砷测定结果均在标准值允差范围内, RSD范围为1.31%,测定土壤中砷的回收率为106.6%。说明该方法稳定性好、精密度高、操作简便、成本低,适用于高效测定大量土壤样品中砷含量。  相似文献   

8.
采用微波消解一氢化物发生原子荧光光谱法同时测定芦苇中砷和镉,优化了试验条件。砷在0ug/L-80.0ug/L、镉在0ug/L~10.0ug/L范围内线性良好,检出限分别为0.010ug/L和0.012ug/L,样品测定的RSD为0.7%-2.0%,平均加标回收率为84.0%~107%。  相似文献   

9.
微波消解-分光光度法测定土壤中的全硼   总被引:1,自引:0,他引:1  
研究了分光光度法测定土壤中的全硼时样品的微波消解方法.建立了合理的分析步骤.进行了微波消解条件的选择及测定结果精密度、准确度实验.实验结果为:消解完全仅需25min,相对标准偏差7.6%,其方法的加标回收率为98.4%~112%.结果表明,微波消解-分光光度法测定土壤中的全硼是一种快速、准确且低环境污染的方法.  相似文献   

10.
采用微波消解电感耦合等离子体发射光谱法同时测定废气中的铅、镉、砷,在优化的试验条件下,方法在0 mg/L~5.00 mg/L范围内线性良好,铅、镉、砷的检出限分别为0.250 μg/m3、0.125 μg/m3、0.375 μg/m3(按采样体积400 L、定容体积50 mL计),空白滤筒平行测定6次的RSD为2.3%~10.5%,加标回收率为83% ~ 112%,与标准方法的测定结果无显著差异.  相似文献   

11.
微波消解ICP-MS法测定宣威和富源土壤中的微量元素   总被引:5,自引:2,他引:3  
建立了微波消解-ICP-MS法测定土壤中32种微量元素的方法。采用氢氟酸-硝酸-过氧化氢体系微波消解,稀释定容后用ICP-MS对溶液进行元素的测定,在优化仪器工作参数后,以双内标铑(Rh)和铼(Re)进行校正。元素检出限为0.01~0.45ng/ml,测定国家标准物质西藏土壤成分分析标准物质GBW 08302中的元素,测定值与标准值或参考值基本一致,用该法测定云南宣威和富源两地24份土壤样品结果表明,该方法快速、简便、准确,适于土壤中多种微量元素的测定。  相似文献   

12.
Suitable techniques have been developed for the extraction of arsenic species in a variety of biological and environmental samples from the Pak Pa-Nang Estuary and catchment, located in Southern Thailand, and for their determination using HPLC directly coupled with ICP-MS. The estuary catchment comprises a tin mining area and inhabitants of the region can suffer from various stages of arsenic poisoning. The important arsenic species, AsB, DMA, MMA, and inorganic arsenic (As III and V) have been determined in fish and crustacean samples to provide toxicological information on those fauna which contribute to the local diet. A Hamilton PRP-X100 anion-exchange HPLC system employing a step elution has been used successfully to achieve separation of the arsenic species. A nitric acid microwave digestion procedure, followed by carrier gas nitrogen addition- (N2)-ICP-MS analysis was used to measure total arsenic in sample digests and extracts. The arsenic speciation of the biological samples was preserved using a Trypsin enzymatic extraction procedure. Extraction efficiencies were high, with values of 82-102%(As) for fish and crustacean samples. Validation for these procedures was carried out using certified reference materials. Fish and crustacean samples from the Pak Pa-Nang Estuary showed a range for total arsenic concentration, up to 17 microg g(-1) dry mass. The major species of arsenic in all fauna samples taken was AsB, together with smaller quantities of DMA and, more importantly, inorganic As. For sediment samples, arsenic species were determined following phosphoric acid (1 M H3PO4) extraction in an open focused microwave system. A phosphate-based eluant, pH 6-7.5, with anion exchange HPLC coupled with ICP-MS was used for separation and detection of AsIII, AsV, MMA and DMA. The optimum conditions, identified using an estuarine sediment reference material (LGC), were achieved using 45 W power and a 20 minute heating period for extraction of 0.5 g sediment. The stability and recovery of arsenic species under the extraction conditions were also determined by a spiking procedure which included the estuarine sediment reference material. The results show good stability for all species after extraction with a variability of less than 10%. Total concentrations of arsenic in the sediments from the Pak Pa-Nang river catchment and the estuary covered the ranges 7-269 microg g(-1)and 4-20 [micro sign]g g(-1)(dry weight), respectively. AsV was the major species found in all the sediment samples with smaller quantities of AsIII. The presence of the more toxic inorganic forms of arsenic in both sediments and biota samples has implications for human health, particularly as they are readily 'available'.  相似文献   

13.
This paper describes the measurement of total antimony and antimony species in "real world" mine contaminated sediments using ICPMS and HPLC-ICPMS. Low and high temperature microwave extraction procedures (90 degrees C and 150 degrees C, respectively) using a range of nitric-hydrochloric acid combinations were examined as to their efficacy to extract antimony from six mine contaminated soils and a certified reference material. The use of the higher temperature with nitric-hydrochloric acid (1:2 (v/v)) was suitable to release antimony from sediments and the certified reference material, NIST 2710 Montana soil. Antimony concentrations obtained using this acid mixture were similar to those obtained using a more aggressive extraction with nitric, hydrochloric, perchloric and hydrofluoric acid mixture. A 25 mM citric acid solution at 90 degrees C for 15 min extracted 47-78% of antimony from soils. A Hamilton PRP X-100 anion exchange column with 20 mM EDTA mobile phase, pH 4.5, flow rate 1.5 mL min(-1) and column temperature of 50 degrees C was used to separate antimony species. Column recoveries ranged from 78-104%. The predominant form of antimony was Sb(5+). Little conversion of Sb(5+) occurred (<5%) during extraction, however, significant conversion of Sb(3+) occurred (approximately 36%). The extraction of antimony species with citric acid should be useful in the determination of inorganic antimony available to plants, as plants commonly excrete carboxylic acids, including citric acid, into their rhizospheres to mobilise trace elements for nutritional purposes.  相似文献   

14.
石墨炉原子吸收光谱法测定土壤中的微量砷   总被引:6,自引:0,他引:6  
土壤样品经HNO3-HCIO4消解处理后,采用Ni作为基体改进剂,偏振塞曼效应扣去背景,实现了砷的石墨炉原子吸收法的直接测定。该方法操作简单,干扰少,灵敏度高,砷的检测下限为0.7ng/ml,样品分析回收率94%-108%,相对标准偏差5.1%。  相似文献   

15.
建立了一种电感耦合等离子体质谱测定土壤中微量稀土金属的方法.分析了土壤标准样品中的微量稀土元素,结果与标准值一致.土壤实际样品分析也得到可靠结果.该方法样品采用微波溶样,灵敏度高,是一种比较可靠的微量稀土元素分析新方法.  相似文献   

16.
建立了王水水浴消解-原子荧光法测定土壤中砷汞的方法,确定还原剂为硼氢化钾,测砷和汞时硼氢化钾的最优质量分数分别为2%和0.05%,载流为5%盐酸。该法砷和汞分别在质量浓度0.0~40.0μg/L和0.00~4.00μg/L范围内线性良好,相关系数均0.999 5,砷和汞的检出限分别为0.009和0.001 mg/kg,相对标准偏差分别为3.90%和2.67%,加标回收率分别为94.1%~107.6%和92.0%~104.0%。采用本法对国家标准土壤样品和东海县部分农田土壤样品进行测定分析,结果良好,表明该法操作简单、灵敏度高、实用性好,适用于土壤中砷和汞的测定。  相似文献   

17.
高效液相色谱-原子荧光光谱联用分析土壤中形态砷   总被引:2,自引:0,他引:2  
采用高效液相色谱(HPLC)-原子荧光光谱(AFS)联用技术分析土壤中亚砷酸盐[As(Ⅲ)]、二甲基砷(DMA)、一甲基砷(MMA)和砷酸盐[As(Ⅴ)]等4种形态砷,以磷酸为提取剂、抗坏血酸为还原剂,优化了水浴提取条件。As(Ⅲ)、DMA、MMA和As(Ⅴ)在7 min之内实现了完全分离,在1.00μg/L~100μg/L范围内线性良好,实验室检出限分别为0.25μg/L、0.36μg/L、0.39μg/L和0.51μg/L,土壤标准样品平行测定的RSD≤7.4%,加标回收率为79.5%~95.0%,提取率为74.6%~90.4%。  相似文献   

18.
A recently developed method for the determination of arsenic species (arsenite, arsenate, monomethylarsonate, MMAA, and dimethylarsinate, DMAA) has been applied to the study of arsenic speciation in plants. This method uses ion-exchange liquid chromatography coupled on-line to atomic fluorescence spectrometry through continuous hydride generation. Various extraction procedures have been studied in detail using three plant certified reference materials. None of the procedures tested revealed fully satisfying results with all kinds of plant samples; microwave assisted extraction with 0.3 mol dm-3 orthophosphoric acid was found to be the most convenient for dealing with terrestrial plants. Species stability appears good. This method was applied to real world cultivated plant parts. Arsenate appears to predominate in soils, roots and leaves; unidentified species (probably arsenosugars) play an important role (60%) in rice fruits. Carrot was found to be the most contaminated edible plant part, containing 1 mg kg-1 essentially as arsenate species. MMAA was detected in all soils and some plant parts especially shallots at low levels, whereas DMAA was found only in one soil sample and in hot pepper leaves. Arsenite is a minor component of all soils; it is also present in some plant parts at low levels. However, no evident relationships were found between As speciation in the various plant parts and much more detailed studies will be necessary to elucidate As behaviour in plants.  相似文献   

19.
The use of pressure feedback microwave digestion technique has permitted rapid and efficient digestion of soil and sediment samples. The evaluation of different acid mixtures to digest soil samples were studied by mixed-level orthogonal array design. The selected acid mixture of HCl-HNO3-HF was employed in the survey of Pb, Zn, Cu, Cr and Mn in soil samples. Surface soil samples were collected from industrial, residential and nature reserve areas in Singapore. The five metal concentrations were determined by flame atomic absorption spectrometry and graphite furnace atomic absorption spectrometry. The lead and other metal contents in NBS SRM 1645, NIES CRM No. 2 and NRCC BCSS-1 sediment standard references were determined concurrently with the survey samples. Five measured metal loading on the surface soils was in the order: industrial area > residential area > nature reserve area. The trace metal concentrations in surface soil from areas of heavy traffic are higher than those from residential areas. The main sources of trace metal pollution are vehicular exhaust and industrial activities.  相似文献   

20.
土壤重金属含量测定不同消解方法比较研究   总被引:19,自引:1,他引:18  
消解是影响土壤重金属测定结果准确性的关键步骤.比较电热板消解、微波消解和全自动石墨消解3种消解方法的操作流程,同时对不同类型土壤样品中Cu、Zn、Pb、Cd、Cr、Ni 6种元素含量进行对比测定,结果表明,电热板消解设备简单,但步骤繁锁,操作不当易造成组分损失;微波消解速度快,测定结果精密性和准确性较好,但仍需人工赶酸程序且罐位少,不适合大批量样品分析;全自动石墨消解不仅测定结果精密性和准确性较好,而且自动化程度高,可实现无人值守,大大节省人力,尤其适合大批量样品的分析.  相似文献   

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