氢化物发生-原子荧光光谱法测定铅锭中砷锑铋

用硝酸溶样,盐酸定量沉淀铅,在不分离大量铅基体沉淀的情况下,加硫脲和抗坏血酸掩蔽干扰元素,采用氢化物发生－原子荧光光谱测定铅定中的砷、锑、铋。     

碱性体系在线氢化物发生—原子荧光光谱法测定痕量铋

提出了一种碱性体系在线氢化物发生－原子荧光光谱法测定痕量铋的分析方法。设计了在线氢化物发生系统流路及操作程序，研究了碱性体系氢化物发生的各项最佳条件。方法操作简便快速，能有效地消除过渡元素的严重化学干扰。应用于黄铜标样中痕量铋的直接测定，获得满意结果。     

氢化物发生-原子荧光光谱法测定高纯锌中痕量铋

在标准中加入锌基体,以硫脲-抗坏血酸-盐酸羟胺混合溶液为预还原剂,硼氢化钾-盐酸还原体系,采用氢化物发生-原子荧光光谱测定高纯锌中痕量铋.方法加标回收率为98.5%～105.0%,相对标准偏差为3.9%.方法适用于高纯锌中质量分数为2.0×10-5～1.0×10-2%铋的测定.     

氢化物发生-原子荧光光谱法测定钢铁中的痕量铋

采用氢化物发生-原子荧光光谱法测定钢铁中的痕量铋。考察了观察高度、负高压、灯电流、载气流速、屏蔽气流速、介质酸度、载流酸度和硼氢化钾浓度等因素对测定结果的的影响,并优化了测定条件,研究了钢铁材料中常见元素对铋测定的影响。结果表明,用硫脲和抗坏血酸作抑制剂可以消除大量元素的干扰。铋浓度在0～100ng/mL与荧光强度呈良好的线性关系,方法的检出限为0.187ng/g。对20ng/mL的铋标准溶液平行测定10次,相对标准偏差为2.5%。用该方法对国家标准钢样品进行了测定,测定结果与标准值相符合。     

原子荧光光谱法测定皮革中9种重金属元素的含量

皮革样品经硝酸-高氯酸（4+1）混合酸湿法消解后,用氢化物发生-原子荧光光谱法测定其中砷、锑、汞、铅和镉的含量;样品经干法灰化后,用火焰原子荧光光谱法测定其中铬、钴、铜和镍的含量。对各元素的稀释介质、还原剂和仪器工作条件作了详细的叙述。9种元素的质量浓度与吸光度分别在一定的范围内呈线性关系;砷、锑、铅、钴和镍的检出限（3S/N）为0.5 mg·kg^-1,汞、镉和铜的检出限（3S/N）为0.05 mg·kg^-1,铬的检出限（3S/N）为5.0 mg·kg^-1。应用此法分析了皮革样品,以标准加入法做回收试验,回收率在89.2%～106%之间。     

原子荧光光谱法测定煤中砷含量

主要研究了原子荧光光谱法测定煤中砷含量的方法,该法回收率为(95.75~98.34)%,RSD2.36%。通过与砷钼蓝分光光度法测定煤中砷含量比较,和对该法的精密度和准确度进行探讨,结果表明,该法操作简单,快速,灵敏度高,测定砷浓度范围大,适用于煤中砷含量测定。     

氢化物发生-原子荧光光谱法测定水系沉积物中铋和汞

水系沉积物试样用盐酸-硝酸-水(3+1+4)混合溶液溶解,氢化物发生-原子荧光光谱法测定铋和汞的含量。对介质酸度、硼氢化钾浓度、负高压和灯电流等影响铋和汞测定因素进行了试验并予以优化。铋和汞的检出限(3S/N)分别为0.02,0.01μg.L-1,相对标准偏差(n=11)均小于0.5%。应用此法分析了水系沉积物标准样品,测定值与推荐值相符。     

氢化物发生-原子荧光光谱法测定镍基高温合金中痕量铋

建立了氢化物发生-原子荧光光谱法测定镍基高温合金中痕量铋的方法,荧光强度与铋浓度在0~30.0μg.L-1范围内呈线性关系,相关系数为0.9991,检出限为0.29μg.L-1。方法应用于高温合金中痕量铋测定,精密度和准确度可满足实际测试工作的要求。     

原子荧光光谱法测定玩具材料中可迁移砷

玩具材料和玩具部件按《玩具安全》(GB6675—2014)规定的程序制样和用盐酸提取后,加入硫脲-抗坏血酸将提取溶液中砷预还原为适合氢化物发生的价态As(Ⅲ),再加入硼氢化钾使其还原成砷氢化物,建立了原子荧光光谱法测定玩具材料中可迁移砷含量的方法。方法的检出限为0.017mg/kg,多种代表性玩具材料的砷元素加标回收率在94.4%~104%。方法适用于各种玩具材料中可迁移砷的分析。     

样品基体化学改进剂-石墨炉原子吸收光谱法测定镍合金中痕量铋

镍基合金是航空工业的重要金属材料,合金中铋、铅、锡等易挥发元素的含量对合金材料性能影响很大[1,2].原子光谱法常被用于分析镍基合金中的痕量元素,如火焰原子吸收光谱法(FAAS)、氢化物发生-原子吸收(荧光)光谱法(HG-AAS/AFS) [3]、电感耦合等离子体-质谱法(ICP-MS).     

Binary modifiers for the determination of zinc in pure copper and nickel-based alloy by longitudinal Zeeman electrothermal atomic absorption spectrometry

The determination of zinc in pure copper and nickel-based alloy was successfully accomplished with a longitudinal Zeeman-effect correction and end-capped transversely heated graphite atomizer. Since aqua regia (an acid mixture of nitric acid and hydrochloric acid, 1:3, v/v) was used as the dissolving reagent, volatile ZnCl₂ was formed. Consequently, less Zn was found in the sample. EDTA could improve the atomic absorption profiles. Binary modifiers, EDTA + Pd(NO₃)₂ and EDTA + Mg(NO₃)₂, were effective for eliminating the chloride interference and the spectral interference from Cu I 213.853 nm. The experimental results obtained with and without the modifiers were compared. Increase of 200 °C in the pyrolysis temperature resulted from the addition of binary modifiers for both pure copper and nickel-based alloys. For pure copper, the atomization temperature increased from 1400 to 1600 °C whereas the atomization temperature increased from 1100 to 1600 °C for nickel-based alloys. The analytical performance of the proposed method was evaluated. Zinc contents in the pure copper and nickel-based alloy standards determined with both binary modifiers agreed closely with the certified values. The recovery ranged from 93 ± 2 to 104 ± 6% at 95% confidence level. The detection limits obtained by the binary modifiers of EDTA + Pd(NO₃)₂ and EDTA + Mg(NO₃)₂ were 0.77 and 0.31 pg, respectively.     

Determination of As,Sb and Bi in high-purity copper by electrothermal atomic absorption spectrometry

As, Sb and Bi were determined in copper electric cables by atomic absorption spectrometry with electrothermal atomization in a graphite furnace. The interferences in the determination of As, Sb and Bi caused by eleven cationic species and six types of acid were studied. The different volatilization of the copper matrix in comparison to the analyte was studied, as a means of increasing the analyte signal/non-specific absorption signal ratio.     

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.     

超声辅助溶剂萃取-原子荧光法用于土壤中汞的形态分析

建立了超声辅助溶剂萃取联用原子荧光法测定土壤样品中迁移毒性态汞中无机汞和有机汞的分析方法.实验优化了萃取溶剂种类,溶剂浓度,各种辅助措施和超声波振荡时间等各种萃取条件.方法的检出限为0.01 μg/L,相对标准偏差(n=11)为2.1%.方法已应用于珠江三角洲4个代表性菜园土壤样品汞形态分析.     

固相微萃取-原子荧光测定鱼样品中痕量甲基汞

研制了一种用HF处理石英纤维表面的萃取纤维和一次性微量注射器组成的固相微萃取装置,研究了用甲基聚硅氧烷作为萃取头涂层对氢化甲基汞的萃取,得到的最佳条件是：在室温条件下,缓冲液的pH值为5、萃取时间为lh、NaCl的用量为2g、洗脱时间为50min、KBH4质量浓度为60g／L。在上述优化条件下,甲基汞的萃取率可以达到70％,检出限为0.17ng。测定了鱼样品中甲基汞,所测鱼虾中甲基汞的质量分数为12．4～53．4ng／g,加标回收率为87．6％～112．8％。     

水产品中甲基汞测定的液相色谱-原子荧光光谱联用方法的改进

对本实验室前期建立的食品中甲基汞的液相色谱-原子荧光光谱联用测定方法进行了改进。采用无毒的半胱氨酸代替有毒试剂巯基乙醇作为流动相中的配位剂,流动相组成为5%(v/v)乙腈-1 g/L半胱氨酸-50 mmol/L乙酸铵水溶液,使汞化合物分离时间缩短至8 min。在优化条件下,甲基汞标准曲线的线性范围为1～50 μg/L,检出限(S/N=3)为0.3 μg/L。采用超声波辅助5 mol/L HCl提取样品中的甲基汞,提取液经C18固相萃取小柱净化后进样。鱼、虾、贝等不同种类水产动物样品以及水产类膳食样品的甲基汞加标回收率为89%～112%。对标准参考物质NIST1566b、BCR464和GBW10029以及英国食品分析水平评估计划(Food Analysis Performance Assessment Scheme, FAPAS)的罐装鱼肉样品(样品编号07115)的测定结果与参考物定值相符,验证了该方法的可靠性与准确性。本方法可满足食品中甲基汞检测的需要。     

电气材料铜及铜合金中痕量杂质砷元素的氢化物发生-原子荧光光谱法测定

本文建立了氢化物发生-原子荧光光谱法测定电气材料铜及铜合金中痕量杂质元素砷的方法。通过使用L-半胱氨酸与铜基体形成络合物,抗坏血酸充分预还原砷,消除了基体干扰,并实现了铜及铜合金中痕量杂质砷的准确测定。在经过优化的实验条件下,砷的检出限为0.12 ng·m L-1,线性相关系数优于0.999,相对标准偏差小于4%。用加标回收法测定实际样品,回收率在92%到103%之间。该法操作简便,灵敏度高,无需基体预分离。