流动注射-氢化物发生-原子吸收光谱法测定中草药中砷

中草药样品经硝酸-高氯酸-硫酸消化处理后,在酸性条件下用硫脲和抗坏血酸将砷(Ⅴ)还原为砷(Ⅲ),然后再以硼氢化钾为还原剂,稀盐酸为载液,用流动注射氢化物发生原子吸收光谱法测定砷含量.砷的质量浓度在1.6～32.0 μg·L-1范围内与其吸光度呈线性关系,检出限(3s/k)为0.32 μg·L-1.用此方法分析了3种草药样品,砷的测定值的相对标准偏差(n=6)在5.1%～8.1%之间,加标回收率在91.4%～106.1%之间.     

氢化物发生-原子吸收法测定饮用水中的砷、硒

建立了测定饮用水中砷、硒的氢化物发生－原子吸收法，探讨了盐酸、硼氢化钠溶液的浓度以及样品还原处理对测定结果的影响，测定结果的相对标准偏差（n=7)小于3％，回收率为89．1％－110．7％，测定砷的线性范围为0－40ug/L(r=0.9990)，测定硒的线性范围为0－50ug/L(r=0.9990)，砷、硒的检出限分别为1．06，0．78ug/L。     

流动注射氢化物发生-原子吸收光谱法测定中药中的微量砷

探讨了流动注射氧化物发生-原子吸收光谱法测定微量砷的最佳条件,建立了中药中微量砷的流动注射氧化物发生-原子吸收光谱分析方法。砷的检出限为0.59μg/L,线性范围为0～30μg/L,线性回归方程为A=0.02228c 6.282×10~(-3),相关系数r=0.9992,相对标准偏差为2.6％～4.4％,回收率为91％～103％。方法操作简便、快速,灵敏度及自动化程度高。     

氧弹燃烧-氢化物发生-原子吸收法测定硫磺中砷

研究了氧弹燃烧、NaOH溶液吸收预处理硫磺样品的方法,优化了HG-AAS法测定砷的最佳条件。     

流动注射氢化物发生-原子吸收光谱法测定食品中的无机砷

探讨并建立了流动注射氢化物发生-原子吸收光谱(FI-HAAS)法测定食品中无机砷的样品前处理方法.该法简便快捷,用6种国家标准参考样品进行考察,分析结果可靠.     

流动注射氢化物发生原子吸收光谱法测定酱油中砷

采用紫外消化技术处理样品 ,流动注射氢化物发生原子吸收光谱法测定酱油中砷。方法的检出限为 0 .14ng·ml- 1,线性范围为 0 .80～ 2 4 .0ng·ml- 1,相对标准偏差为 3.5 %～ 8.4 % ,样品加标回收率为 96 .9%～ 10 6 .5 %。方法的灵敏度高 ,选择性好 ,试剂及样品用量少 ,操作方便 ,分析快速 ,每小时可分析 6 0个样品 ,适于推广应用     

氢化物发生原子吸收法测定卡托普利

根据卡托普利与醋酸铅反应定量生成沉淀的特点 ,通过用氢化物发生原子吸收法测定沉淀中的铅 ,可间接测定卡托普利的含量。平均回收率 99.8% ,RSD值为 1 .6%     

氢化物发生－缝管原子捕集－原子吸收法测定钢铁和地质试样中的砷

介绍简易的氢化物发生原子吸收测砷的方法。喷雾器负压将ＫＢＨ_４吸入反应器，并将生成的ＡｓＨ_３吸入乙炔－空气焰原子化。石英缝管使灵敏度提高３．５倍。方法的检测限（３σ）为１．８ｎｇ／ｍＬ（５ｍＬ试样）。２０ｎｇ／ｍＬＡｓ（Ⅲ）标准液１０次测定的ＲＳＤ为３．８％。本法成功地应用于钢铁和地质标样中微量砷的测定。     

氢化物发生—缝管原子捕集—原子吸收法测定钢铁和地质试样中的砷

介绍简易的氢化物发生原子吸收测砷的方法，喷雾器负压将ＫＢＨ５吸入反应器，并将生成的ＡｓＨ３吸入乙炔－空气焰原子化。石英缝管使灵敏度提高３．５倍，方法的检测限为１．８ｎｇ／ｍＬ（５ｍＬ试样）。２０ｎｇ／ｍＬ Ａｓ（Ⅲ）标准液１０次测定的ＲＳＤ为３．８％。本法成功地应用于钢铁和地质标样中微量砷的测定。     

氢化物发生-原子吸收光谱法测定萤石粉中砷

提出了以氢化物发生-原子吸收光谱法测定萤石粉中砷的方法,研究了酸介质、还原剂、载气流量等因素对测定的影响,并选择出最佳工作条件.砷的检出限为0.052μg·g-1,线性范围为0.10～6.00 μg·L-1,回收率在90.0%～102.0%之间,相对标准偏差为9.8%.     

Determination of Inorganic and Total Arsenic in Wines by Hydride Generation Atomic Absorption Spectrometry

A method is described for the determination of inorganic arsenic species and total arsenic in wines by means of hydride generation atomic absorption spectrometry (HGAAS). Simple ethanol evaporation is the only pretreatment procedure proposed for wine samples prior to direct measurement of inorganic arsenic (AsIII) and As(V) species by HGAAS. The total arsenic content is determined after microwave digestion of the wine samples. The optimal parameters for the microwave digestion procedure and the next HGAAS measurement of arsenic are established. The detection limits achieved are 0.1µgL^–1 for inorganic and total arsenic determination. The relative standard deviation for both procedures and for ten independent determinations varied between 8 and 15% for arsenic species in the range of 1–30µgL^–1. The accuracy of the procedure for total arsenic determination was proved by comparative analysis using electrothermal atomic absorption spectrometry.     

流动注射氢化物发生-原子吸收光谱法 测定镍基合金中的硒和锡

建立了流动注射氢化物发生-原子吸收光谱法测定高温镍基合金中痕量硒和锡的方法。样品用HNO3和HF经微波消解后,制成以EDTA作掩蔽剂的碱性溶液(pH12～13),用标准加入法测定。方法测定硒和锡的检出限分别为1.0μg     

Determination of Inorganic Arsenic Species by Electrochemical Hydride Generation Atomic Absorption Spectrometry with Selective Electrochemical Reduction

A new direct procedure for the determination of inorganic arsenic species was developed by electrochemical hydride generation atomic absorption spectrometry （EcHG-AAS） with selective electrochemical reduction. The determination of inorganic arsenic species is based on the fact that As（Ⅲ） shows significantly higher absorbance at low electrolytic currents than As（Ⅴ） in 0.3 mol·L^-1 H2SO4. The electrolytic current used for the determination of As（Ⅲ） without considerable interferences of As（Ⅴ） was 0.4 A, whereas the current for the determination of As（Ⅲ） and As（Ⅴ） was 1.2 A. For equal concentrations of As（Ⅲ） and As（Ⅴ） in a sample, the interferences of As（Ⅴ） during the As（Ⅲ） determination were smaller than 5%. The absorbance for As（Ⅴ） could be calculated by subtracting that for As（Ⅲ） measured at 0.4 A from the total absorbance for As（Ⅲ） and As（Ⅴ） measured at 1.2 A, and then the concentration of As（Ⅴ） can be obtained by its calibration curve at 1.2 A. The methodology developed provided the detection limits of 0.3 and 0.6 ng·mL^-1 for As（Ⅲ） and As（Ⅴ）, respectively. The relative standard deviations were of 3.5% for 20 ng·mL^-1 As（Ⅲ） and 3.2% for 20 ng·mL^-1 As（Ⅴ）. The method was successfully applied to determination of soluble inorganic arsenic species in Chinese medicine.     

碱性氢化物发生—火焰原子吸收光谱法测定锡

对Ｓｎ－ＮａＯＨ－ＫＢＨ４体系进行了系统研究，采用三乙醇胺－ＥＤＴＡ联合干扰抑制剂，可消除一定量铁及合金元素的干扰，对于锡含量小于０．０１％的试样，用苯萃取锡后所有元素不干扰测定。测定液中锡量为０－４μｇ／１０ｍｌ，呈线性关系，灵敏度为０．００４ｍｇ／Ｌ／１％，检出限为０．００８ｍｇ／Ｌ，测定钢中大于０．００１％锡，结果满意。     

Determination of Bismuth in Geological Materials by Flow Injection Hydride Generation Atomic Absorption Spectrometry

Abstract

Flow injection analysis (FIA) has been applied to sample introduction in conjunction with automated hydride generation and AAS techniques for the determination of Bi in rock samples. The powdered rock sample is digested with a mixture of hydrofluoric, perchloric, and nitric acids. The evolved hydride is carried through to a heated quartz tube by a stream of argon, and the atomic absorption of Bi is measured at 223.2 nm.

Thiosemicarbazide and 1,10 - phenanthroline are used as masking agents to control interferences from Cu and Ni. The method permits the accurate determination of Bi in geological materials at levels as low as 10 ppb with an analysis rate of more than 50 digested samples per hour. Bi values on 13 international geological reference samples are reported.     

氢化物发生原子荧光法测定聚氯化铝中的砷含量

建立了氢化物发生原子荧光法测定聚氯化铝中砷含量的检测方法。将聚氯化铝样品用硫酸溶解,蒸至近干,用氢化物发生原子荧光法测定其中的砷含量。在最佳测定条件下,砷的质量浓度在0~10.0μg/L范围内与荧光强度呈良好的线性关系,相关系数r=0.999 3,砷的检出限为0.03μg/g,样品加标回收率为82.5%~90.0%,测定结果的相对标准偏差为1.5%~1.9%。该法具有快速、准确、灵敏度高等优点。     

双阳极电化学氢化物发生原子荧光光谱法测定砷

用双阳极电化学氢化物发生原子荧光光谱法测定砷,减少了化学试剂使用给环境带来的污染。在相同条件下,双阳极电化学氢化物发生效率为化学法的99.0%~101.6%。对各种实验参数和干扰情况进行了详细研究。在选定的实验条件下,100μL进样量的As(Ⅲ)线性范围为0~120μg/L;检出限为0.64μg/L(信噪比S/N=3);60μg/L的As(Ⅲ)标准溶液平行进样13次,荧光信号面积的相对标准偏差(RSD)为2.02%。用本法测得GBW07406号标准土壤样品中As含量为(205.2±1.4)μg/g与标准值(220±21)μg/g一致,仔猪饲料样品的加标回收率为97.0%~103.0%。本法灵敏度高、重现性好、结果准确。     

氢化物发生原子荧光法测定人发、玉米及辣椒中的砷

采用硝酸、高氯酸和硫酸湿法分解人发、玉米及辣椒,在盐酸介质中用硫脲-抗坏血酸将As(Ⅴ)还原为As(Ⅲ),氢化物发生原子荧光法测定,此法简便快速,相对标准偏差为2.4%。     

Arsenic Determination in Plant Samples by Hydride Generation and Axial View Inductively Coupled Plasma Atomic Emission Spectrometry

The present work describes a study on the determination of arsenic in plant samples with hydride generation coupled with an axial view inductively coupled plasma atomic emission spectrometer. The accuracy of the measurements was not affected by elements present in high concentrations in the plant matrix (K, Ca, Mg, and P). Interference from transition metals was not observed either. When using real samples (maize and oak leaves) with standard additions, a decrease in the recoveries was sometimes observed when using KI to reduce As(V) to As(III), which reached 13.5% in the most unfavourable case. The use of a mixture containing KI and ascorbic acid is recommended. The accuracy of the method was verified using three certified reference materials. No statistically significant differences were observed between the measured concentrations and the certified values. The optimized method was found to be sensitive (detection limit: 0.1 μg L⁻¹) and reliable. The results obtained under routine conditions over a period of several months also demonstrated its reproducibility.