化学蒸气发生-四通道原子荧光光谱法同时测定高纯金中的痕量As,Sb,Bi,Te

采用化学蒸气发生-四通道原子荧光光谱法测定了高纯金中的痕量砷、锑、铋和碲。用乙酸乙脂萃取分离金,水相还原后采用化学蒸气发生-四通道原子荧光光谱法测定高纯金中的痕量砷、锑、铋和碲。在最佳条件下,方法对As,Sb,Bi,Te的检出限分别为0.04,0.05,0.04,0.03 ng/mL(3σ);测定精密度分别为0.98,0.89,0.94,0.99%(对10 ng/mL As,Sb,Bi和Te混合标准,n=7)。方法对实际样品中的As,Sb,Bi,Te进行了同时测定,测定结果与标准方法无明显差异,各元素的加标回收率为95%～105%。     

氢化物发生-原子荧光光谱法同时测定高纯铟中As、Sb

研究了氢化物发生-原子荧光光谱法测定高纯铟中微量As、Sb元素的条件,选择了适宜的反应条件以及仪器的最佳工作条件,考察了铟基体对被测元素的干扰,采用基体匹配的方法消除干扰,建立了氢化物发生-原子荧光光谱法测定高纯铟中微量的As、Sb的分析方法。As、Sb的检出限分别为0.18和0.28 ng/mL,测定下限为1.2×10-5和1.9×10-5,相对标准偏差分别为1.9%和1.7%,回收率为97.4%和103%,适用于5～6 N高纯铟中微量As、Sb的测定。     

微波等离子体原子发射光谱新技术同时测定环境水样中多种元素

环境水样经不同酸消解后,利用微波等离子体原子发射光谱法(MP-AES)和多模式样品导入系统(MSIS)对环境水样中可蒸气发生元素(As,Hg,Sb和Se)及重金属元素(Cd,Cu,Cr,Ni,Pb,Ti,V和Zn)同时分析,分别根据溶液中元素信号强度变化和测定值与加标值差异,优化氢化物发生条件和考察测定的基体及谱线干扰影响.结果表明,在还原剂溶液(1.0％ NaBH4,m/V)和载流HCl(5％,V/V)的最佳实验浓度下,相比HC1消解,水样经HNO3消解可获得满意分析结果;环境标准样品中元素测定值与标准值一致,样品分析相对标准偏差在0.34％ ～ 3.2％范围内.高浓度的K,Ca,Na和Mg等元素对测定无明显影响,稀土元素和稀有元素对重金属光谱干扰严重,需选择合适谱线分析.本方法除对Hg和Se的检出限稍高外(6.5和37.1μg/L),其它目标元素检出限为1.6～9.8μg/L,能够满足地表水环境质量标准和生活饮用水卫生标准的质量控制要求.     

电感耦合等离子体质谱法测定多西他赛注射液中17种元素

建立电感耦合等离子体质谱（ICP-MS）法测定多西他赛注射液中17种元素（Al、As、Ba、Cd、Co、Cr、Cu、Fe、Hg、Li、Mn、Ni、Pb、Sb、Tl、V、Zn）。采用浓硝酸与过氧化氢作为消解液，经微波消解处理样品后，用ICP-MS法进行测定。Hg质量浓度在0.05～4 ng/mL范围内、其余16种元素质量浓度在0.5～40 ng/mL范围内线性关系良好，相关系数均大于0.999，各元素的检出限为0.000 5～0.6 mg/kg，样品加标回收率为92.2%～108.8%，测定结果的相对标准偏差为1.1%～2.8%。该方法操作简便，线性范围宽，分析速度快，灵敏度高，可同时测定多种元素，适用于多西他赛注射液中多种元素的测定。     

ICP-MS法测定亚热带水果中的重金属含量

用电感耦合等离子体质谱(ICP–MS)法测定亚热带水果中Pb,Cd,As,Hg元素的含量,对实验条件进行优化,样品用微波消解法进行预处理,用Bi,In,Ge作内标校正基体干扰和漂移。Pb,Cd,As的线性范围为0.0～20.0ng/mL,Hg的线性范围为0.0～2.0 ng/mL,线性相关系数均为0.999 9。Pb,Cd,As,Hg元素的检出限分别为0.027,0.008,0.011,0.051 ng/mL,测定结果的相对标准偏差(n=6)在3.63%～5.72﹪之间,加标回收率为90.2%～102.0%。用该法测定茶叶、大米和小麦3种国家标准物质,测定结果均在标称值范围内。     

氢化物发生-原子荧光光谱法测定1：5万区域地质调查样品中的As、Sb、Bi、Hg等4种元素

建立了氢化物发生-原子荧光光谱法测定1∶5万区域地质调查样品中的As、Sb、Bi、Hg等4种元素的分析方法,通过采用王水(1+1)分解样品,在盐酸(5%)介质中用硼氢化钾作为还原剂对As、Sb、Bi、Hg等4种元素进行氢化物发生-原子荧光光谱法测定。方法检出限为0.008 9(As)、0.008 1(Sb)、0.008 1(Bi)、0.001 7(Hg)μg/g,测定结果的相对标准偏差(RSD,n=12)为0.82%～7.6%,准确度△lgC=-0.01～0.02。方法简便、成本低,检测结果准确,检出限、准确度及精密度均能达到行业规范要求,适用于1∶5万区域地质调查样品水系沉积物、土壤中As、Sb、Bi、Hg等4种元素的测定。     

垃圾渗滤液中 As和 Hg的流动注射蒸气发生非色散原子荧光光谱法测定

建立了垃圾渗滤液中As和Hg的流动注射蒸气发生－非色散原子荧光光谱的测定方法。在低温下采用硝酸－过氧化氢体系消化处理样品;硫脲－抗坏血酸将As(V）还原后测定样品中的总As;Hg的测定用Hg蒸气发生原子荧光光谱法。对测量条件进行了优化,在优化实验条件下测得As和Hg的检出限分别为0．08和0．007μg/L,10次测定的相对标准偏差分别为0．48％和0．85％（对8．0μg/L As和1．0μg/L Hg标准溶液）。共存的NaCI、MgCI2、CaCI2、Na2SO4、NaF以及微量共存金属离子（Cd、Se、Zn、Pb、Cu、Fe、Mn、AI）对As和Hg的测定没有干扰。用标准校正曲线和标准加入法对样品测定结果进行了比较,实验结果表明二者吻合较好。     

电感耦合等离子质谱法测定化妆品中的有害元素

用电感耦合等离子质谱法测定了抽检化妆品中有害元素Pb、As、Hg.采用内标元素Sc校正As,内标元素Eu校正Pb和Hg,获得满意的测定结果.方法检出限为0.03～0.05 ng/mL,变异系数（CV%）为0.3%～5.0%,加标回收回收率为95%～105%.     

预还原氢化物发生-原子荧光光谱法快速测定化探样品中的As、Sb、Bi、Hg

通过对化探样品进行王水密闭溶解,饱和的硫脲-抗坏血酸预还原,运用氢化物发生-原子荧光光谱法实现了地质样品中As、Sb、Bi、Hg元素的任意配对以及连续快速测定。实验确定了原子化器高度为14mm,最佳溶样时间为1h。在优化条件下,结果显示还原剂(硫脲-抗坏血酸)对Hg、Bi测定结果无影响,且Hg、Bi测定结果在预还原20min至48h内都很稳定,测定结果良好,Cu、Co、Ni、Au、Ag、Cd、As、Sb、Bi、Se、Ge等金属离子对预还原测定汞均无干扰,对比实验表明还原剂体系下汞荧光强度值基本不变。方法的检出限低、精密度好、准确度高、操作简便,有效避免了元素污染问题,可满足大批量地质样品分析测定的需要。     

乙醇基体改进ICP-MS法直接测定植物中的痕量As、Se、Sb和Te

建立了HNO3-H2O2高压密闭消解、2%乙醇基体改进电感耦合等离子体质谱法(ICP-MS)测定植物中As、Se、Sb和Te的新方法。探讨了乙醇基体对As、Se、Sb和Te信号的增敏效应,以2%乙醇作基体改进剂,各元素信号增敏因子在2~6之间。方法的检出限(3σ)分别为0.0450、2.49、0.0892、0.0202μg/L,相对标准偏差均小于3.6%。     

Simultaneous determination of arsenic,mercury, antimony and selenium in biological materials with prior collection of gaseous products followed by neutron activation analysis

A method combining prior collection of gaseous products with subsequent neutron activation analysis has been developed for simultaneous determination of traces of arsenic, mercury, antimony and selenium in biological materials. The generation of hydrides of arsenic, antimony and selenium and cold vapor of mercury in the vapor generaion and collection system was investigated by the use of radiotracers of the respective elements. The result indicates that selenium and mercury can be completely evaporated from the digested sample solution in 5M HCl with the addition of 5% sodium tetrahydroborate solution, while additional reduction proces by potassium iodide and ascorbic acid is needed for complete evaporation of arsenic and antimony. The gaseous products were collected in a quartz tube for neutron irradiation. The detection limits of these elements were fount to be in the range of 10^–7 to 10^–8 g under the present experimental conditions. The reliability was checked with NBS standard reference materials.     

Separations involving sulphides : Separation of thorium or titanium from some elements that form thiosalts

Sodium sulphide can be used to separate arsenic, antimony, tellurium, selenium, molybdenum, mercury, gold, platinum or rhenium from thorium and antimony, tellurium, selenium or mercury from titanium     

电感耦合等离子体发射光谱法测定粗二氧化碲中 铜、铅、锑、铋、砷和硒

粗二氧化碲作为碲精炼或碲化工产品生产的重要原料,其中共存元素铜、铅、砷、锑、铋、硒含量的准确测定对于生产过程质量控制和贸易结算具有重要意义,但目前没有粗二氧化碲中铜、铅、砷、锑、铋、硒含量检测的标准分析方法。采用王水和饱和氟化氢铵分解试样,在王水和酒石酸介质中,选用Cu 327.393 nm、Pb 220.353 nm、Sb 217.582 nm、Bi 223.061 nm、As 193.696 nm、Se 196.026 nm为分析谱线,采用电感耦合等离子体发射光谱(ICP-AES)法测定粗二氧化碲中铜、铅、锑、铋、砷和硒含量。各元素校准曲线的相关系数均大于0.999;铜、铅、锑、铋、砷和硒的检出限分别为0.0004%、0.0005%、0.0006%、0.0007%、0.0004%和0.0007%,定量检出限分别为0.0012%、0.0016%、0.0020%、0.0025%、0.0013%和0.0025%。按照实验方法测定5个粗二氧化碲样品中铜、铅、锑、铋、砷和硒,测定结果的相对标准偏差(RSD,n=7)为0.79%~4.8%,加标回收率为96.0%~103%。方法简单,精密度和准确度较高,可用于测定粗二氧化碲中铜、铅、砷、锑、铋、硒含量。     

Stability studies of arsenic, selenium, antimony and tellurium species in water, urine, fish and soil extracts using HPLC/ICP-MS

The stability of arsenic, selenium, antimony and tellurium species in water and urine (NIST SRM 2670n) as well as in extracts of fish and soil certified reference materials (DORM-2 and NIST SRM 2710) has been investigated. Stability studies were carried out with As(III), As(V), arsenobetaine, monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), phenylarsonic acid (PAA), Se(IV), Se(VI), selenomethionine, Sb(III), Sb(V) and Te(VI). Speciation analysis was performed by on-line coupling of anion exchange high-performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP-MS). Best storage of aqueous mixtures of the examined species was achieved at 3 degrees C whereas at -20 degrees C species transformation especially of selenomethionine and Sb(V) took place and a new selenium species appeared within a period of 30 days. Losses and species transformations during extraction processes were investigated. Extraction of the spiked fish material with methanol/water led to partial conversion of Sb(III), Sb(V) and selenomethionine to two new antimony and one new selenium species. The other arsenic, selenium and tellurium species were almost quantitatively extracted. For soil spiked with MMA, PAA, Se(IV) and Sb(III), recoveries after extraction with water and sulfuric acid (0.01 mol/L) were below 20%.     

Simultaneous determination of arsenic, antimony, selenium and tin by gas phase molecular absorption spectrometry after two step hydride generation and preconcentration in a cold trap system

A cold trap system for the simultaneous determination of arsenic, antimony, selenium and tin by continuous hydride generation and gas phase molecular absorption spectrometry is described. The hydride generation is carried out in two steps; first, tin hydride is generated at low acidity and second, arsenic, antimony and selenium hydrides are formed at higher acidity. All the hydrides are collected in a liquid nitrogen cryogenic trap and transported to the flow cell of a diode array spectrophotometer, where molecular absorption spectra are obtained in the 190-250 nm range. Five calibration solutions containing arsenic, antimony, selenium and tin are solved using multiple linear regression analysis. Tests are performed in order to extend the same manifold to other hydrides but no signals are obtained for bismuth, cadmium, lead, tellurium and germanium. Under the optimum conditions found and using the wavelengths of maximum sensitivity (190, 198, 220 and 194 nm), the analytical characteristics of each element are calculated. The detection limits are 0.050, 0.020, 0.12 and 1.1 mug ml(-1) and the RSD values are 3.7, 3.1, 3.5 and 3.0% for As, Sb, Se and Sn, respectively. The method is applied to As, Sb, Se and Sn determination in natural spiked water samples.     

Determination of trace arsenic, antimony, selenium and tellurium in various oxidation states in water by hydride generation and atomic-absorption spectrophotometry after enrichment and separation with thiol cotton

A novel procedure for determination of trace As(III) and As(V), Sb(III) and Sb(V), Se(IV) and Se(VI), Te(IV) and Te(VI) in water by atomic-absorption spectrophotometry after separation and enrichment with "thiol cotton" and hydride generation has been established. The sorption behaviour of various oxidation states of arsenic, antimony, selenium and tellurium, and the conditions of quantitative sorption and desorption of these species were studied. The procedures for reducing species from higher oxidation states were optimized. Interferences from other species and their elimination were investigated. The selectivity of the procedure for the determination of species in higher and lower oxidation states was examined. The procedure has been successfully used to determine arsenic, antimony, selenium and tellurium in water, in the range from pg ml to ng ml . The recoveries for added spikes were in the range 90-110%, with coefficients of variation in the range 3-8%     

Simultaneous determination of trace arsenic, antimony, bismuth and selenium in biological samples by hydride generation-four-channel atomic fluorescence spectrometry

A new and sample technique for the simultaneous determination of trace arsenic, antimony, bismuth and selenium in biologic samples by hydride generation-four-channel nondispersive atomic fluorescence spectrometry was development. The conditions of instrumentation and hydride generation of arsenic, antimony, bismuth and selenium were optimized. For reducing hexavalent Se to the tetravalent state was to heat the sample with 6 mol l⁻¹ HCl, and then pre-reducing pentavalent As and Sb to the trivalent state was achieved by the addition of 0.05 mol l⁻¹ thiourea. The interferences of coexisting ions were evaluated. Under optimal conditions, the detection limits for As, Sb, Bi and Se were determined to be 0.03, 0.04, 0.04 and 0.03 ng ml⁻¹, respectively. The precision for seven replicate determinations at the 5 ng ml⁻¹ of As, Sb, Bi and Se were 0.9, 1.2, 1.3 and 1.5% (R.S.D.), respectively. The proposed method was successfully applied to the simultaneous determination of As, Sb, Bi and Se in a series of Chinese certified biological reference materials using simple aqueous standard calibration technique, the results obtained are in good agreement with the certified values.     

HG/LT-GC/ICP-MS coupling for identification of metal(loid) species in human urine after fish consumption

Human urine samples after fish consumption have been investigated by low-temperature gas chromatography with inductively coupled plasma mass spectrometric detection after sample derivatization by hydride generation (HG/LT-GC/ICP-MS). This analytical technique enabled the identification of organometal(loid) compounds in human urine; species of the six elements germanium, arsenic, selenium, tin, antimony, and mercury were determined. Three different organic selenium species, two germanium species, seven arsenic species, four tin species, five antimony species, and one species of mercury were found; 18 of the 22 species detected could be identified. The relative detection limits ranged between 2 and 12 pg x L(-1) (x=element). These organometal(loid) compounds probably build up in the human body under the influence of micro-organisms, in the presence of hydrogen sulfide and methane, in the human intestine.     

Radiochemical activation analysis of arsenic,selenium and antimony in biological samples

A method for the neutron activation analysis of arsenic, selenium and antimony has been developed. A radiochemical separation is performed by distillation followed by precipitation of the individual elements. Selenium and arsenic are precipitated by reduction to the elemental form while antimony is precipitated as sulfide. The chemical yields and detection limits using 0.5 g samples are the following: As 90–100%, 0.4 ppb, Se 80–100%, 8 ppb and Sb 50–70%, 0.2 ppb. Results from the analysis of nine international biological standard samples are given.     

Tracer study of a chemical separation procedure for the determination of impurities in selenium by means of thermal neutron activation analysis

A chemical separation procedure has been developed for the determination of about 50 trace elements in high-purity selenium. The method consists of two distillation steps, followed by a precipitation step. In the first distillation step the halogens, osmium, and part of the ruthenium are volatilised in the second the selenium is distilled together with antimony, tin, arsenic, mercury and germanium. Selenium is precipitated from the second distillate by reduction to the element. The whole procedure has been tested by means of radioactive tracers. Interferences from the selenium matrix with respect to the arsenic and bromine determinations are discussed.