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1.
用流动注射-氢化物发生-非色散原子荧光光谱法对海水中As(Ⅲ)和As(Ⅴ)的直接测定进行了研究,氢化物发生的最佳条件为:KHB4溶液浓度为5g.L^-1(含KOH5g.L^-1),流速10.0mL.min^-1;样品酸度为1.3mol.L^-1HCl,流速4.2mL.min^-1。对基体NaCl,MgCl2,CaCl2,Na2SO4以及微量共存金属离子(Cd,Zn,Pd,Cu)的干扰实验结果表明,基体和微量共存金属离子对As(Ⅲ)的测定没有干扰。样品中As(Ⅴ)的测定用硫脲进行预还原,通过总量和As(Ⅲ)的含量的差减得到As(Ⅴ)含量,在优化实验条件下下测量方法的检出限(3σ)为0.08ng.mL^-1;7次测定的相对标准偏差为0.48%-1.30%(8.0ng.mL^-1标准溶液)。标准曲线和标准加入法对海水  相似文献   

2.
本文采用GF-AAS加平台技术,基体改进剂,测定了中药片仔癀,六味地黄丸中铬、铅和镉的含量,铬、铅和镉的线性范围分别为0-0.8ng/mL,0-50ng/mL,0-5ng/mL,回收率分别为102-103%,99-101%,97.5-98%,本方法简便快速、准确。  相似文献   

3.
野外快速测定化探样品中的微量砷   总被引:3,自引:0,他引:3  
薛光 《分析试验室》1994,13(6):26-27
提出了一个野外快速测定化探样品中微量砷的新方法。该法采用砷化氢富集,以硫酸银泡塑班点法进行测定方法的检出限为0.5×10^-6g,测定范围为0 ̄10μg/10mL As。  相似文献   

4.
FETV-ICP-AES 直接测定中药漏芦中微量稀土元素的研究   总被引:2,自引:0,他引:2  
提出了以聚四氟然悬浮为氟化剂,氟化电热蒸发(FETV)等离子体发射光谱法(ICP-AES)直接测定中药漏芦中微量稀土元素La、Eu、Yb和Y的方法,改进了ETV与ICP之间的气路接口,研究了影响待测元素信号强度的有关因素,在优化实验条件下,方法的检出限为1.0-3.8ng/mL,相对标准偏差为2.7%-4.4%。此法已应用于中药漏芦中微量稀土元素的测定。  相似文献   

5.
新试剂5-氟偶氮胂Ⅰ荧光法测定铝的研究   总被引:2,自引:0,他引:2  
本文报道了新试剂5-氟偶氮胂Ⅰ(5-FAsA-Ⅰ)的合成方法,研究了荧光光度法测定铝的反应条件。Al(Ⅲ)与试剂在pH5.60HAc-NaAc缓冲介质中形成1+1红色配合物并呈现荧光,λex/λem=348.6/391.4nm,线性范围为0~0.2μg/mL,检测限为3.0ng/mL。用于分析茶叶样品中的铝,结果满意。  相似文献   

6.
 报道了采用乙酸乙酯萃取纯化样品,经重氮甲烷酯化、BSTFA硅烷化后,用气相色谱-质谱法的选择离子检测(SIM)定量模型,对pravastatin的血药浓度进行测定的方法。方法的最低检出限为0.015ng,在1.0~60ng/mL的浓度范围内,标准曲线呈良好的线性关系,r>0.99,CV<7.7%。  相似文献   

7.
氯酸钾-二甲基黄-钒(Ⅴ)体系催化光度法测定痕量钒   总被引:1,自引:0,他引:1  
本文研究了氯酸钾-二甲基黄-钒(Ⅴ)体系催化光度法测定痕量钒的条件及应用。钒含量在0~60ng/10mL范围内与lg(A_0/A)有良好的线性关系,检出限1.0×10 ̄(-11)g/mL。方法简便快速,应用于水及食品中痕量钒测定,结果满意。  相似文献   

8.
本文提出一种测定痕量钼的微分吸附计时电位法,利用悬汞电极作为工作电极,在0.12mol/LHAc-0.01mol/L,NaAc-3.2×10^-6mol/L茜素红的最佳底液中,测定钼的线性范围为0.4ng/mL~70ng/mL,吸附富集3min检测下限可达0.1ng/mL。探讨了影响方法灵敏度的主要因素,初步研究了电极过程,利用该方法直接测定了粮食样品中钼的含量。  相似文献   

9.
在pH3.8的H2SO4-NH4Ac介质中,Co(Ⅱ)-β-巯基丙酸(MPA)-NaNO2体系产生-灵敏的极谱催化波,峰电位在-0.84V(vs.SCE),钴浓度在0.02~100ng/mL范围内与峰电流呈线性关系。检出限为0.01ng/mL。本文对极谱波的性质和机理进行了初步探讨。本法用于土壤中总钴和有效钴的测定,结果满意。  相似文献   

10.
钴(Ⅱ)—β—巯基丙酸—NaNO2体系的极谱化波研究   总被引:1,自引:0,他引:1  
在pH3.8的H2SO4-NH4Ac介质中,Co(Ⅱ)-β-巯基丙酸(MPA)-NaNO2体系产生-灵敏的极谱催化波,峰电位在-0.84V(vs.SCE)钴浓度在0.02~100ng/mL范围内与峰电流呈线性关系,检出限为0.01ng/mL。本文对极谱波的性质和机理进行了初步探讨,本法用于土壤中总钴和有效钴的测定,结果满意。  相似文献   

11.
Ion exchange (IE)-vapor generation (VG)-inductively coupled plasma (ICP)-mass spectrometry (MS) method has been employed to simultaneously determine trace amounts of As, Se, and Hg in acidic conditions. Before hydride generation, anion-exchange column was used to separate the analytes from the matrix. Effects of sample solution acidity, eluant conditions and concentrating time were investigated and optimized. The method sensitivity was improved, as well as the ability to refrain interference caused by chloride, mental ions and other hydride-forming elements compared with (CF)VG-ICP-MS method. Limits of detection (3σ, n = 10) for As, Se, and Hg were As, 0.0021 ng/ml; Se, 0.0022 ng/ml; Hg, 0.0007 ng/ml, respectively; and recovery values for interference experiments were between 95.6 and 100.3%. The developed method was applied to four standard biological and geological materials, and the determined results of As, Se, and Hg were consistent with the certified values.  相似文献   

12.
采用硝酸-高氯酸湿式消解法消解样品,利用AFS-230E原子荧光光度计测定了赣州市赣江交汇处鱼体内砷和汞的含量,选择了最佳实验条件.结果表明,所得砷和汞的检出限分别为0.020、0.008 μg/L,测定砷、汞标准溶液各6次,所得砷、汞标准溶液的平均值分别为0.099、0.103 μg/mL,相对标准偏差RSD分别为2...  相似文献   

13.
通过王水系统对畜禽粪便中砷、汞元素进行了提取,利用原子荧光光谱仪同时测定了畜禽粪便中的砷、汞,并对灯电流、负高压、载气流量等检测条件进行了优化。结果表明,用王水对畜禽粪便中的砷、汞前处理,可同时测定样品中的砷、汞。砷、汞检出限分别为0.051 5、0.009 6μg·L1。该法快速简便,回收率好,砷的回收率为91.9%~103.0%,汞的回收率为93.9%~101.5%。该法精密度高、结果准确,砷、汞的最大标准偏差分别为4.03%、4.47%,完全适用于畜禽粪便中砷、汞的检测。  相似文献   

14.
为弥补标准检测方法的不足,建立了石墨消解-ICP-MS法同时检测铜精矿中Pb、Cd、As 和Hg等4种有害元素。确定了样品前处理和仪器分析条件。用铜精矿标准样品和参考样品分别进行7次重复实验,Pb、Cd和As的检测结果均在标准值范围内,Hg的检测结果与参考值基本一致。7次重复检测结果的变异系数符合GB/T 27417-2017《合格评定 化学分析方法确认和验证指南》要求。选择5种不同物相铜精矿作为待测样品,通过与标准方法比对,两种方法检测结果的绝对差符合标准方法的再现性要求,说明本方法适用于不同种类的铜精矿。本方法操作简单,可同时测定多种有害元素,实用性强。  相似文献   

15.
建立了一种顺序注射氢化物发生-原子荧光光谱法测定中草药中的Bi和Hg的方法,讨论了共存离子的干扰情况。在最佳实验条件下,Bi和Hg的检出限分别为0.0057μg/L和0.0197μg/L,加标回收率为93.4%~104.7%,相对标准偏差小于4.3%,被测中草药试样中共存的离子对Bi和Hg的测定没有干扰。方法可用于中草药试样中Bi和Hg的同时测定。  相似文献   

16.
Li Z  Yang X  Guo Y  Li H  Feng Y 《Talanta》2008,74(4):915-921
Chemical vapor generation (CVG) coupled with non-dispersive atomic fluorescence spectrometry (NDAFS) has been widely used for determination of vapor-forming elements, but most of such works have been focused on single element analysis, and reports dealing with more than three elements simultaneous determination by CVG-NDAFS are rare. In this work, a sensitive and robust analytical procedure for the simultaneous determination of arsenic, antimony, bismuth and mercury in geological materials using vapor generation-four-channel non-dispersive atomic fluorescence spectrometry has been developed. The conditions of instrumentation and vapor generation of arsenic, antimony, bismuth and mercury were optimized. The optimized concentrations of KBH(4) and HCl required for analytes generation were 1.3% (m/v) and 20% (v/v), respectively. The interferences of coexisting ions and mutual hydride interferences were investigated carefully. One thousand milligrams per litre of Fe(3+); 500mgl(-1) of Pb(2+), Zn(2+), Mn(2+); 50mgl(-1) Cu(2+), Ni(2+), Cr(6+), Co(2+); 10mgl(-1) Ag(+) and 5mgl(-1) Au(3+) does not interfere with the determination of As, Sb, Bi and Hg. Associating a dilution of 1:250 (m/v) in the procedure of sample pretreatment, the tolerant concentrations of As, Sb, Bi and Hg in real geological materials are 2500, 1000, 250 and 5000ppm, respectively. Under optimal conditions, the detection limits for As, Sb, Bi and Hg were determined to be 0.068, 0.047, 0.037 and 0.008ngml(-1), respectively. The precisions for seven replicate determinations at the 5ngml(-1) of As, Sb, Bi and 1ngml(-1) of Hg were 0.47, 0.60, 0.97 and 0.93% (R.S.D.), respectively. Sample digestion was carried out on 500mg sample with 3ml HNO(3) and 10ml HCl, followed by addition of thiourea solution for the quantitative reduction of As(V), Sb(V) to As(III), Sb(III). The proposed method was successfully applied to the simultaneous determination of As, Sb, Bi and Hg in a series of certified geological reference materials using simple aqueous standard calibration technique. The results obtained are in good agreement with the certified values.  相似文献   

17.
A simple and very inexpensive in-situ nebulizer/hydride generator was used with inductively coupled plasma mass spectrometry (ICP-MS) for the determination of As, Sb, Bi and Hg in water samples. The application of hydride generation ICP-MS alleviated the sensitivity problem of As, Sb, Bi and Hg determinations encountered when the conventional pneumatic nebulizer was used for sample introduction. The sample was introduced by flow injection to minimize the deposition of solids on the sampling orifice. The elements in the sample were reduced to the lower oxidation states with L-cysteine before being injected into the hydride generation system. This method has a detection limit of 0.003, 0.003, 0.017 and 0.17 ng ml−1 for As, Bi, Sb and Hg, respectively. This method was applied to determine As, Sb, Bi and Hg in a CASS-3 nearshore seawater reference sample, a SLRS-2 riverine water reference sample and a tap water collected from National Sun Yat-Sen University. The concentrations of the elements were determined by standard addition method. The precision was better than 20% for most of the determinations.  相似文献   

18.
化妆品中Hg、As和Pb的微波消解-   总被引:5,自引:0,他引:5  
采用微波消解 -氢化物发生ICP-AES法测定化妆品中的Hg、As和Pb ,加入L_半胱氨酸消除了过渡金属离子的干扰 ,考察了微波消解、氢化物发生的最佳条件。建立的方法简便快速 ,测定Hg、As和Pb的RSD分别为0.59%、1.2%、2.4 % (n=10) ,样品加标回收率分别为98.5%、99.3 %和100.1 %。该法已应用于化妆品的常规测定 ,得到满意的结果。  相似文献   

19.
《Analytical letters》2012,45(15):2257-2268
An analytical procedure was developed for determination of Hg, As, Pb, and Cd in soil samples using sequential injection vapor generation atomic fluorescence spectrometry (SI-VG-AFS) with sample preparation by microwave digestion system. The effects of analytical conditions on the fluorescence intensity were investigated and optimized. Under the optimized condition, the detection limits of the method were 5, 68, 40, and 3 ng L?1 for Hg, As, Pb, and Cd, respectively. The accuracy of method was verified by the determination of the certified reference soil, and the recoveries for Hg, As, Pb, and Cd were in the range of 98.7–106.1%. The proposed method has been successfully applied to determine the heavy metals in navel orange orchard soils in Ganzhou, and the environmental quality of the orchard soils was assessed based on the content of the heavy metals. According to the second criterion of environmental quality standard for soils, Pb content in all soil samples collected from the orchards of 18 districts were within safe limits, but a few orchards were slightly contaminated with Hg, As, and Cd. Comparison of heavy metal mean concentrations with the safe limits of environmental quality standard for soils, the quality of Ganzhou navel orange orchard soils were in line with the request of the green food production base.  相似文献   

20.
介绍了一种用于测定中成药中微量砷(As)和汞(Ag)元素的方法-微波消解-氢化物发生-原子荧光光谱法。讨论了仪器的工作参数、实验条件、共存元素对分析结果的干扰;同时,通过加标回收试验,对该法进行了验证。实验结果表明,该法具有快速、简便、准确等特点,适用于实验室常规分析。  相似文献   

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