高效液相色谱-电感耦合等离子体质谱检测海藻中的砷

以阴、阳离子交换色谱与电感耦合等离子体质谱联用检测砷的形态,测定了我国不同海域海藻(海带、紫菜)10种样品中的砷.样品总砷的浓度为1.7~38.7mg/kg As(干重).所有样品萃取物中,砷糖为砷的主要形态,在大多数紫菜样品中砷糖PO4为主要化合物0.4~12.7 mg/kg As(干重),其次为砷糖OH 1.0~7.8 mg/kg As(干重).海带样品除含有以上两种砷糖外,还含有砷糖SO3(8.9~17.6 mg/kg As干重),及DMA(1.7~3.2 mg/Kg As干重),无机砷在所有样品萃取物中未检出.     

微波消解-电感耦合等离子体质谱法测定土壤中的锂和铍

构建微波消解法-电感耦合等离子体质谱法体系测定土壤中的锂和铍的含量。样品加入硝酸、氢氟酸、盐酸,在微波消解仪中进行程序升温消解,用~6Li元素作为内标元素,用ICP-MS测定锂元素和铍在土壤样品中含量。结果表明,测定方法线性相关系数都在0.999以上,锂的方法检出限为0.11 mg/kg;铍的方法检出限为0.03 mg/kg,采用国家土壤标准样品做准确度验证,结果准确度高,精密度好,能满足测试要求,表明建立的方法能够满足土壤中锂和铍的检测。     

ICP-AES法测定铁精矿中硅、磷、砷含量

本文试验研究了电感耦合等离子体发射光谱分析方法测定铁精矿中的硅、磷、砷含量的仪器工作条件及分析谱线,考查了酸碱加入量及基体对测定结果准确度的影响,加标回收率分别为硅99.1%、磷102%、砷101.5%,RSD值均小于5%。分析方法应用于生产,收到了提高检测数据准确度和指导生产实效性的好效果。     

氢化物发生——电感耦合等离子体原子发射测定砷分族元素的氢化物发生

氢化物发生－－电感耦合等离子体原子发射光谱法是现代分析技术的一种重要手段,本文中就该方法测定砷分族元素的氢化物发生原理,影响因素以及氢化物装置进行了阐述。     

微波消解氢化物发生-ICP-AES测定巴豆中砷锑铋

建立了微波消解-氢化物发生-电感耦合等离子体发射光谱联用技术测定中药巴豆中砷、锑、铋的方法,并对微波消解、氢化物发生条件、电感耦合等离子体原子发射光谱工作条件等进行了优化选择,砷、锑、铋的检出限分别为1.5,1.9,1.2μg·L-1,相对标准偏差分别为4.1%,3.8%,4.2%,结果满意.     

江苏绿茶中稀土元素的组成特征及分布模式

通过测定绿茶中稀土元素(REE)含量,研究江苏绿茶的REE组成特征及分布模式。采用微波消解及电感耦合等离子体质谱法(ICP-MS)测定9个品种的江苏绿茶中15种稀土元素含量,采用SPSS统计软件进行数据分析。结果表明:江苏绿茶的REE、轻稀土和重稀土含量分别为0.917、0.720和0.197μg/g;绿茶明显富集轻稀土,而轻、重稀土间则存在较大的分馏作用;江苏绿茶中的稀土分布模式与江苏镇江土壤和中国大陆土壤(平均值)中的稀土分布模式较接近;江苏绿茶中的REE总量普遍低于2.0 mg/kg,食用安全风险相对较小;轻稀土的生物学效应比重稀土更为显著;稀土元素沿绿茶的迁移传递中没有表现出明显的生物放大作用。     

微波消解-同位素稀释质谱法测量鱼中汞含量

建立了微波消解-同位素稀释电感耦合等离子体质谱法(ID-ICP-MS),用于测定国际物质量咨询委员会(CCQM)K43.1比对样品剑鱼中汞含量。对质谱测量汞的条件进行了优化,同时为了消除汞的记忆效应,比较了5%(体积分数)HNO₃、1‰(体积分数)2-巯基乙醇以及交替使用5μg/gAu和10μg/g EDTA3种方法对仪器的清洗效果。实验结果表明：射频功率1500～1600W,载气流速1.18L/min,取样深度7.5～6.9mm,积分时间0.4s条件下,能够获得准确的同位素比值;5μg/g Au和10μg/g EDTA溶液交替清洗在同样的洗涤时间内可使仪器本底最低。本文方法测定鱼中汞含量的平均值为(5.26±0.15)mg/kg, 在标准值(5.30±0.24)mg/kg的不确定度范围内。     

微波消解-ICP-OES法测定小叶榕药材中微量元素

【目的】建立一种小叶榕（Ficus microcarpa）药材中微量元素的测定方法。【方法】采用微波消解样品,电感耦合等离子体质谱法（ICP-OES）测定小叶榕药材中12种微量元素的含量。【结果】电感耦合等离子体质谱法测定药材中微量元素的含量线性好、操作简便、快速准确、灵敏度高。小叶榕药材中含量丰富的微量元素,从高到低依次为Mg、Fe、A1、Mn、Zn等。【结论】建立了微波消解-ICP-OES测定小叶榕药材中多种微量元素的分析方法。     

微波消解-HG-ICP-AES法测定郁金中砷硒

建立了微波消解-氢化物发生-电感耦合等离子体原子发射光谱联用技术测定郁金中微量元素砷、硒的方法,对微波消解、氢化物发生、电感耦合等离子体原子发射光谱工作条件进行了优化选择,并对增敏剂进行了选择.在最佳实验条件下,A s和Se的检出限分别为0.13μg.L-1和0.34μg.L-1,相对标准偏差分别为0.83%和1.8%,回收率分别为98%和95%.实验操作简便,结果满意.     

四川道地药材:“川麦冬”中铅、砷、汞的含量测定及安全性评价

用电感耦合等离子体质谱法测定四川三台县所产川麦冬药材中铅、砷、汞的含量并进行分析,结果表明:9批川麦冬中铅、砷、汞的含量范围分别为0.011～0.030、0.077～0.48和0.004 32～0.016 90 mg/kg,均低于《药用植物及制剂外经贸绿色行业标准》和《中国药典》(2010版)中限量标准,但川麦冬作为保健食品,砷含量有超标现象,有必要对川麦冬的生产按中药材生产质量管理规范(GAP)的要求进行规划和管理,以期为川麦冬的用药质量及评估提供参考.     

长城窝堡井田煤中砷赋存状态的初步研究

对长城窝堡井田煤中砷的含量和赋存状态的研究得出:研究区煤中砷含量较高,算术平均含量高达95.5 mg/kg,远高于中国煤中砷的含量;砷与灰分之间关系不明显,砷主要赋存在以黄铁矿为主的硫化物中,有机硫是导致煤中有机结合态砷存在的一个因素.     

Arsenic hyperaccumulator Pteris Vittata L. and its arsenic accumulation

An arsenic hyperaccumulator Pteris vittata L. (Chinese brake) was first discovered in China by means of field survey and greenhouse cultivation. Field survey showed that Chinese brake had large accumulating capacity to arsenic; the orders of arsenic content in different parts of the fern were as follows: leaves>leafstalks>roots, which is totally different from that of ordinary plants; bioaccumulation coefficients of the above ground parts of the fern decreased as a power function of soil arsenic contents. In the control of pot trials with normal unpolluted soil containing 9 mg/kg of arsenic, the bioaccumulation coefficients of the above ground parts and rhizoids of Chinese brake were as high as 71 and 80 respectively. Greenhouse cultivation in the contaminated soil from mining areas has shown that more than 1 times greater arsenic can be accumulated in the leaves of the fern than that of field samples with the largest content of 5070 mg/kg As on a dry matter basis. During greenhouse cultivation, arsenic content in the leaves of the fern increased linearly with time prolonging. Not only has Chinese brake extraordinary tolerance and accumulation to arsenic, but it grew rapidly with great biomass, wide distribution and easy adaptation to different environmental conditions as well. Therefore, it has great potential in future remediation of arsenic contamination. It also demonstrates important value for studies of arsenic physiology and biochemistry such as arsenic absorption, translocation and detoxification mechanisms in plants.     

Arsenic hyperaccumulator Pteris Vittata L. and its arsenic accumulation

An arsenic hyperaccumulator Pteris vittata L. (Chinese brake) was first discovered in China by means of field survey and greenhouse cultivation. Field survey showed that Chinese brake had large accumulating capacity to arsenic; the orders of arsenic content in different parts of the fern were as follows: leaves>leafstalks>roots, which is totally different from that of ordinary plants; bioaccumulation coefficients of the above ground parts of the fern decreased as a power function of soil arsenic contents. In the control of pot trials with normal unpolluted soil containing 9 mg/kg of arsenic, the bioaccumulation coefficients of the above ground parts and rhizoids of Chinese brake were as high as 71 and 80 respectively. Greenhouse cultivation in the contaminated soil from mining areas has shown that more than 1 times greater arsenic can be accumulated in the leaves of the fern than that of field samples with the largest content of 5070 mg/kg As on a dry matter basis. During greenhouse cultivation, arsenic content in the leaves of the fern increased linearly with time prolonging. Not only has Chinese brake extraordinary tolerance and accumulation to arsenic, but it grew rapidly with great biomass, wide distribution and easy adaptation to different environmental conditions as well. Therefore, it has great potential in future remediation of arsenic contamination. It also demonstrates important value for studies of arsenic physiology and biochemistry such as arsenic absorption, translocation and detoxification mechanisms in plants.     

珠江三角洲典型区水土中砷的分布

 为了解研究区水土中砷的来源及分布,采集地表水样5组、土壤样32组、地下水样14组进行分析。结果表明研究区地表水已受到砷污染。表层土壤(0~10 cm)中砷全量为198~274 mg/kg,平均全量为237 mg/kg,土壤中砷的形态分布以极难迁移的残渣态为主,各形态平均含量的顺序依次为残渣态＞弱有机结合态＞氧化物结合态＞碳酸盐态＞强有机结合态＞水溶态＞离子交换态。底层土壤(30~40 cm)中砷全量为115~281 mg/kg,平均全量为212mg/kg,土壤中砷的形态也以残渣态为主,土壤中砷的各种形态的平均含量顺序依次为残渣态＞弱有机结合态＞氧化物结合态＞碳酸盐态＞强有机结合态＞离子交换态＞水溶态,底层土壤中砷的各种形态的均量均低于表层土壤。包气带砷全量随深度增加先降低后升高,水溶态、离子交换态以及碳酸盐态的含量均随深度的增加而逐渐降低;而弱有机结合态、氧化物结合态、强有机结合态以及残渣态的含量随深度增加均呈无规律变化。地下水砷含量在00028~0021mg/L之间,均值为00114 mg/L,超标率达429％。地表污水灌溉下渗以及含水介质中原生砷的释放是研究区地下水砷的主要来源。     

氢化物发生—原子荧光光谱法测定水样中的砷和汞

建立了氢化物发生-原子荧光光谱法测定汞和砷含量的分析方法,并用于水样中汞和砷含量的测定.其中汞和砷具有良好的线性关系,相关系数均大于0.99.实验还表明两元素的检出限低,精密度好.通过加标回收实验考察了方法的准确性,结果表明:加标回收率为93.6%-107%,符合回收率规定要求,应用此法分析的水样中Hg和As的含量符合国家饮用水标准.     

大学生常用化妆品中砷含量的检测分析

目的:对高校学生常用各类型化妆品中砷含量进行调查分析。方法:新银盐法测定4种不同种类化妆品样品中砷含量,结果依据2007年版《化妆品卫生规范》(砷含量不得超过10 mg/kg)进行卫生学评价。结果:所检测的4类化妆品(防晒霜、润肤霜、粉底、面霜)中,砷含量在0.186 1~4.045 3 mg/kg之间,浓度依次为润肤霜>防晒霜>粉底>面霜。结论:本次实验所测定的化妆品样品中砷含量未超过国家标准。     

207Pb/206Pb determination of zircons by laser probe-inductively coupled plasma mass spectrometry

Laser probe_inductively coupled plasma mass spectrometry (LP_ICP_MS) was used to determine 207 Pb/ 206 Pb ratios in single zircon grains. A Nd∶YAG laser operating at 1 064 nm and a Fisons_VG PQII Turbo ICP_MS were employed. For the known zircons, the 207 Pb/ 206 Pb results of LP_ICP_MS are close to the thermal ionization mass spectrometry (TIMS) results. The spatial resolution of this method is 40-50 μm and the sensitivities for lead isotopes are about 300-400 cps/ppm. The precision of 207 Pb/ 206 Pb ratio is 0.3%-4% and depends on the lead concentration of the sampling pits. LP_ICP_MS provides a simple, rapid and economic method for zircon 207 Pb/ 206 Pb determination.     

微波压力消解-原子荧光法测定土壤及其小麦中有害元素砷的研究

为测定小麦中的微量砷,并研究其自然迁移规律和生物吸收比的特性,以河南省安阳县白壁镇郭盆村的土壤和小麦为样品,用微波炉密闭消解体系进行消解,用氢化物-原子荧光法进行测定,在优化的测定条件下,砷标准曲线的工作范围为0～80μg/L,相关系数r>0.999,检出限为0.073 1μg/L,仪器测定标准溶液的RSD为1.4%(n=11),加标回收率为91.57%～107.1%.研究结果表明小麦中砷的生物吸收比随土壤中总砷含量的增加而增加,但小于1%.