单柱离子色谱法测定痕量草酸根离子

本文采用单柱离子色谱系统测定了Ｃ２Ｏ＾２－４，以１．３ｍｍｏｌ／Ｌ葡萄糖酸钠／１．３ｍｍｏｌ／Ｌ硼砂为淋洗液测定Ｃ２Ｏ＾２－４，８常见阴离子Ｃｌ＾－，ＮＯ＾－３，ＨＰＯ＾２－４，ＳＯ＾２－４不干扰测定，Ｃ２Ｏ＾２－４的检出限为０．５７ｍｇ／Ｌ，相对标准偏差为１．０７％，工作曲线的线性范围为０．５７－５００ｍｇ／Ｌ，应用本方法测定了加Ｃ２Ｏ＾２－４的自来水样，Ｃ２Ｏ＾２－４的回收率为９９．５２％。     

原子荧光光谱法测定食品中的镉

研究了在水溶液中，Ｃｄ与ＫＢＨ４反应生成挥发性物种，以原子荧光光谱法测定食品中的痕量Ｃｄ的分析方法，方法的检出限为０．１２μｇ／Ｌ，线性范围０～５０μｇ／Ｌ，回收率为８６％～１１２％。     

安替比林基重氮氨基—2,4—二硝基苯间接分光光度法测定痕量氰化物

１引言氰化物是环境监测和食品检验中必测的剧毒物之一。研究表明，在ｐＨ＝１０．５～１２．８的条件下，氰离子使银与安替比林基重氮氨基－２，４－二硝基苯（ＡＰＤＮＢＴ）络合物褪色，其褪色程度与氰离子的浓度呈良好的线性关系，从而建立了新的间接测定氰离子的分光光度方法。对于浓度低于０．０５ｍｇ／Ｌ时氰离子的测定，提出了标准加入分光光度法，提高了低含量氰离子测定的准确度和可靠性。２实验部分２．１仪器和试剂７２２型光栅分光光度计，ｐＨｓ－２型酸度计；银标准溶液为１５．０ｍｇ／Ｌ，氰离子标准溶液为５．０ｍｇ／Ｌ…     

锌柱还原分光光度法测定微量砷

对锌柱还原砷及其测定进行了研究，胂化氢以Ａｇ＾＋－ＰＶＡ－ＥｔＯＨ－Ｈ２Ｏ为吸收液，在λｍａｘ４００ｎｍ处进行吸光度测定，砷在０－１．８ｍｇ／Ｌ范围内与吸光度呈良好线性关系，其ε＝８．７×１０＾４Ｌ．ｍｏｌ＾－１．ｃｍ＾－１。检出限为２４μｇ／Ｌ。     

氧氟沙星—镁络合吸附波的研究

本文用多种电化学方法研究了氧氟沙星与镁离子的相互作用及其极谱伏安行为，在０．０１ｍｏ１／Ｌ的ＮＨ３－ＮＨ４Ｃ１缓冲溶液中（ｐＨ＝９．２），氧氟沙星与镁离子络合，产生一灵敏的还原峰，峰电位ＥＰ＝－１．７０Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ）．该峰为不可逆的络合吸附峰，还原峰电流与镁离子浓度在４×１０－６～２×１０－５ｍｏｌ／Ｌ范围内呈良好的线性关系，可望用于镁离子的分析测定．本文还测定了该络合物的络合比，探讨了电极反应机理与络合物结构．     

水杨醛—5—溴—水杨酰腙与锌的高灵敏度荧光反应及其应用

合成了新荧光试剂水杨醛－５－溴－水杨酰腙（ＳＡＢＳＨ），详细研究了试剂与锌的荧光反应新体系的最适宜条件．在ｐＨ７．９的异丙醇／水（体积比１∶１）溶液中，该试剂与Ｚｎ２＋形成配合物，组成比为１∶２（金属∶试剂），λｅｘ／λｅｍ＝３９３ｎｍ／４６５ｎｍ．所建立锌的荧光分析方法的线性范围为０～４００μｇ／Ｌ，相对标准偏差为１．２％，检出限为１．３μｇ／Ｌ．考察了３６种离子的干扰情况．方法成功地用于面粉、大米、人尿和矿泉水中痕量锌的测定．     

氧化藏红T褪色催化荧光法测定痕量钒

研究了在酸性介质中柠檬酸存在下，痕量钒（Ｖ）催化溴酸钾氧化藏红Ｔ的褪色反应及其动力学条件，建立了催化荧光测定痕量钒的新方法。催化反应在沸水浴中进行８ｍｉｎ，为假零级反应，反应的表观活化能力为９９．２１ｋＪ／ｍｏｌ，反应速度常数为０．１２／ｓ；该方法的检出限为２．２×１０＾－８ｇ／Ｌ；线性范围为０．２￣２．４μｇ／Ｌ研究了共存离子的影响，用于人发和煤灰中痕量钒的测定，结果令人满意。     

离子色谱法测定糙米中微量总溴的研究

本文研究了在有乙醇存在的碱性介质中，含溴熏蒸剂中的溴被转化为无机溴，随后用带电导检测器的离子色谱进行分离测定的方法。在Ｄｉｏｎｅｘ ＡＳ４Ａ分离柱上，用１．０ｍｍｏｌ／Ｌ ＮａＨＣＯ３／２．０ｍｍｏｌ／Ｌ Ｎａ２ＣＯ３作为流动相进行洗脱，被测组份得到了满意的仞了。方法简便、快速。对样品中溴离子的检测限为１．２５ｍｇ／ｋｇ，相对标准偏差与回收率分别为５．７３％和９４．９％。首次用于实际糙米样品中微量     

催化光度法测定痕量锌

ｌ引言光度法测定微量锌已多有报道。常用的有双硫腙法、锌试剂法等。这些方法对超痕量锌的测定普遍存在灵敏度较低问题。本文研究了在Ｈ２ＳＯ４介质中，Ｚｎ２＋催化Ｈ２Ｏ２氧化酸性铬蓝Ｋ褪色反应及动力学条件，据此建立了分光光度法测定痕量锌的新方法。实验表明，采用固定时间法，在本方法实验条件下，反应速度ｌｏｇ与Ｚｎ２＋含量在０～０．０８ｍｇ／Ｌ范围呈线性关系，方法检出限为１．５６×１０－１０ｇ／ｍＬ。方法灵敏度高，重现性好，用于测定人发中痕量锌时，结果满意。２实验部分２．１仪器和试剂７２１型分光光度计（上海…     

大量锆存在下铪镧钼杂多酸—耐尔蓝体系测定给

本文研究了耐尔蓝（ＮＢ）－给镧钼杂多酸（ＨｆＬａＭｏ－聚乙烯醇（ＰＶＡ）体系测定铪的超高灵敏光度法。在ＰＶＡ存在下，铪，镧和钼酸铵形成杂多酸，继而与耐尔蓝形成离子缔合物。其适宜条件为〔ＨＣｌｏ４〕＝１．２ｍｏｌ／Ｌ，〔Ｌａ×３＋〕＝２．９×１０＾－７ｍｏｌ／Ｌ，〔ＭｏＯ４×２－〕＝１．１×１０＾－３ｍｏｌ／Ｌ，〔ＮＢ〕＝２．７×１０＾－６ｍｏｌ／Ｌ，ＰＶＡ０．０８％。离子缔合物的最大吸收波长在５９     

光诱导蒸气发生-高效液相色谱-电感耦合等离子体质谱联用测定汞形态

以紫外光诱导化学蒸气(UV-CVG)发生为接口,建立了高效液相色谱与电感耦合等离子体质谱联用测定无机汞、甲基汞的分析方法.对色谱条件、紫外光化学反应还原剂甲酸浓度、紫外光化学反应管长度等系统操作条件进行了优化.在优化的系统条件下,4 μg/L无机汞和甲基汞的色谱峰高的相对标准偏差(RSD,n=11)分别为0.72％和0.66％;无机汞和甲基汞的线性范围为0.1～10μg/L,100 μL进样检出限分别为0.011和0.0093 μg/L.用DORM-2角鲨鱼肉参考物质验证了方法的准确性,测试结果与推荐值吻合;对沼泽湿地水样中无机汞和甲基汞的加标回收率分别在99％～106％和94％～110％范围内.     

对氯苯基荧光酮与锌显色反应的研究及应用

在阳离子表面活性剂溴化十六烷基三甲胺（CTMAB）存在下,研究了对氯苯基荧光酮（P—CPF）与锌的显色反应条件和光度性质。在pH=8．4的Na2HPO4-KH2PO4缓冲溶液中,锌与P—CPF形成1：1的红色络合物,所形成的络合物的最大吸收波长位于568nm处,表观摩尔吸光系数为7．20×10^4L·mol^-1·cm^-1;红色络合物至少稳定10h以上,锌含量在0～2．40μg／5mL范围内符合比耳定律。拟定方法用于药物中微量锌的测定,结果满意。     

电解冷蒸气发生原子荧光法测定痕量汞

以电解冷蒸气发生技术结合原子荧光光谱仪,采用自行设计的圆盘电解池,进行汞的电解还原冷蒸气发生情况的研究.实验表明,铂作为阴极时,Hg的电化学发生响应信号与化学还原法获得的信号强度相当;同时发现,载气引入位置是影响Hg响应信号强度的重要因素.在1.0 mol/L H2SO4作为阴极液及0.8 A的电解电流条件下,Hg的检出限为1.2 ng/L(3σ); 相对标准偏差为1.7%(n=11).利用此体系分析了标准物质及生物样品中的痕量汞,结果满意.     

Enhancement reagents for simultaneous vapor generation of zinc and cadmium with intermittent flow system coupled to atomic fluorescence spectrometry

Simultaneous vapor generation of zinc (Zn) and cadmium (Cd) was evaluated by atomic fluorescence spectrometry coupled with an intermittent flow vapor generation system. Some complexing reagents, surfactant and transition metal ions were respectively tested as enhancement reagents. Experiments showed that an appropriate amount of 8-hydroxyquinoline or phenanthroline and nickel ion simultaneously, effectively improved the vapor generation efficiency of Zn and Cd. The volatile species generation was presumed to be a hydrogenation process interpreting how the enhancement reagents played an important role in vapor generation. Additionally, due to the instability of volatile species, reaction temperature, rapid and sufficient mixing of reagents and rapid separation of the volatile species from liquid phase were also crucial. The method of simultaneous determination of Zn and Cd by intermittent flow vapor generation led to the development of atomic fluorescence spectrometry. The detection limits (3σ_b) were 1.6 μg l⁻¹ for Zn and 0.01 μg l⁻¹ for Cd and the relative standard deviations were 3.6% for Zn (50 μg l⁻¹, n=11) and 1.7% for Cd (2 μg l⁻¹, n=11) respectively. Results for the determination of Zn and Cd have been confirmed by the analysis of CRMs with good agreement between the certified and found values.     

Solution cathode glow discharge induced vapor generation of mercury and its application to mercury speciation by high performance liquid chromatography-atomic fluorescence spectrometry

A novel solution cathode glow discharge (SCGD) induced vapor generation was developed as interface to on-line couple high-performance liquid chromatography (HPLC) with atomic fluorescence spectrometry (AFS) for the speciation of inorganic mercury (Hg(2+)), methyl-mercury (MeHg) and ethyl-mercury (EtHg). The decomposition of organic mercury species and the reduction of Hg(2+) could be completed in one step with this proposed SCGD induced vapor generation system. The vapor generation is extremely rapid and therefore is easy to couple with flow injection (FI) and HPLC. Compared with the conventional HPLC-CV-AFS hyphenated systems, the proposed HPLC-SCGD-AFS system is very simple in operation and eliminates auxiliary redox reagents. Parameters influencing mercury determination were optimized, such as concentration of formic acid, discharge current and argon flow rate. The method detection limits for HPLC-SCGD-AFS system were 0.67 μg L(-1) for Hg(2+), 0.55 μg L(-1) for MeHg and 1.19 μg L(-1) for EtHg, respectively. The developed method was validated by determination of certified reference material (GBW 10029, tuna fish) and was further applied for the determination of mercury in biological samples.     

在线化学蒸气发生-电感耦合等离子体原子发射光谱法测定废催化剂中的微量铑

使用电感耦合等离子原子发射光谱(ICP-AES)研究了贵金属铑和NaBH4在酸性水溶液中的化学蒸气发生反应的条件,并测定了有机合成催化剂中的铑。研究结果表明:在NaBH4和样品溶液流速为2mL/min、废液排放流速为6mL/min的条件下的最佳蒸气发生条件为:载气流速0.4L/min、HNO3浓度为1.0mol/L、NaBH4浓度为1.2%(m/V)。研究中获得的铑化学蒸气进样效率是常规的气动雾化进样效率的2.7倍;检出限是6.9μg/L,略优于气动雾化法;线性范围20～1500μg/L;线性相关系数是0.9986;RSD是1.6%。样品分析加标回收率分别是94%和97%。用本法测得的样品值与原子吸收法的测得值吻合很好。     

A new vapor generation system for mercury species based on the UV irradiation of mercaptoethanol used in the determination of total and methyl mercury in environmental and biological samples by atomic fluorescence spectrometry

A new vapor generation system for mercury (Hg) species based on the irradiation of mercaptoethanol (ME) with UV was developed to provide an effective sample introduction unit for atomic fluorescence spectrometry (AFS). Preliminary investigations of the mechanism of this novel vapor generation system were based on GC–MS and FT–IR studies. Under optimum conditions, the limits of determination for inorganic divalence mercury and methyl mercury were 60 and 50 pg mL⁻¹, respectively. Certified reference materials (BCR 463 tuna fish and BCR 580 estuarine sediment) were used to validate this new method, and the results agreed well with certified values. This new system provides an attractive alternative method of chemical vapor generation (CVG) of mercury species compared to other developed CVG systems (for example, the traditional KBH₄/NaOH–acid system). To our knowledge, this is the first systematic report on UV/ME-based Hg species vapor generation and the determination of total and methyl Hg in environmental and biological samples using UV/ME–AFS. Figure A new vapor generation system for mercury species using mercaptoethanol under UV irradiation was developed as an effective sample introduction unit for atomic fluorescence spectrometry     

Sorption–Spectrophotometric and Test Determination of Zinc(II) as the Mixed-Ligand Complex of 1,10-Phenanthroline and Bromophenol Blue

The interaction of Zn(II), Cd(II), and Pb(II) with 1,10-phenanthroline noncovalently immobilized on silica in the presence of Bromophenol Blue was studied. The optimum conditions of the reaction and the composition of mixed-ligand complexes that are formed at the surface were found, and a scheme was proposed for the interaction at the interface. A sorption–spectrophotometric procedure and a test scale were developed for the determination of zinc with detection limits of 0.011 and 0.018 mg/L, respectively. The procedure was used for the determination of labile zinc species in soil.     

火焰原子吸收光谱法测定红土镍矿中铜、锌、铬含量

红土镍矿样品用盐酸、硝酸分解,残渣用焦硫酸钾熔融,在稀盐酸介质中,采用氘灯扣除背景,分别用原子吸收光谱仪于波长324.8,213.9,357.9 nm处,使用空气–乙炔火焰,测量铜、锌、铬的含量。在最佳实验条件下,铜、锌、铬的质量浓度分别在0.50～2.50,0.30～1.50,0.50～4.50 mg/L范围内与吸光度线性关系良好,相关系数r分别为0.9986,0.9943,0.9942。方法检出限铜为0.0067 mg/L,锌为0.0010 mg/L,铬为0.0014 mg/L,加标回收率为95.0%～105.7%。精密度试验验证铜、锌、铬的含量分别在0.01%～0.50%,0.01%～1.00%,0.01%～4.00%范围内重复性和再现性较好。此方法适合于红土镍矿中铜、锌、铬含量的测定。     

高灵敏度分光光度法测定茶叶中锌的含量

研究了在聚乙烯醇(PVA)存在下,Zn2+ - SCN—- RhB高灵敏度显色反应体系,采用分光光度法测定茶叶中微量锌的新方法.结果表明,络合物的最大吸收峰在605 nm处,摩尔吸光系数为1.59×106 L·mol—1·cm—1,Zn2+的质量浓度在0.0~0.04 μg/mL范围内服从比尔定律.该法用于测定茶叶中锌...