β修正吸光光度法测定食品中微量铅

用 β修正二硫腙光度法对铅进行测定。结果表明此法能准确消除显色液中剩余二硫腙吸收影响 ,使测定误差减小 ,其灵敏度比经典的单波长二硫腙法提高 1.3倍 ,相对标准偏差为0 82 %～ 3.95 % ,加标回收率为 95 %～ 10 1%。方法应用于食品中铅的测定 ,结果满意。     

Sonoelectrochemistry in Acoustically Emulsified Media: The Detection of Lead

The double extraction of target lead ions which are then voltammetrically quantified via acoustically assisted anodic stripping voltammetry is demonstrated. The technique involves first the extraction of lead from the aqueous volume into an organic phase containing the ligand dithizone (diphenylthiocarbazone). Second, the chelated lead is then stripped into a clean electrochemically clean aqueous solution where the lead from the original solution can be quantified. This method is shown to be applicable in electrochemically fouling media, providing a high sensitivity with a limit of detection for lead in the order of 10^?7 mol dm^?3. A theoretical extraction model is presented for the optimal conditions of extraction. The technique is applied to the analysis of lead in wine samples offering quantitative data, which is in good agreement with those obtained from an independent technique (AAS).     

横向光热偏转技术检测双硫腙（H2Dz）固体试样光谱特性

用横向光热偏转技术测量双硫腙固体试样的光谱特性及Ｈ２Ｄｚ的浓度与横向光热偏转辐度之间的关系，检测限可达ｎｇ量级，为固体不透明材料的微量特性分析提供了一个简便的方法。     

Sensitized extraction spectrophotometric determination of Hg(II) with dithizone after its flotation as ion-associate using iodide and ferroin

This paper describes a simple and highly selective method for the separation, preconcentration and spectrophotometric determination of extremely low concentration of mercury. The method is based on the flotation of an ion-associate of HgI₄²⁻ and ferroin between aqueous and n-heptane interface at pH 5. The ion-associate was then separated and treated with ammonia and dithizone solutions to extract only the mercury chelate with CH₂Cl₂. The measurement is feasible when the volume of the water sample containing Hg(II) was varied over 50-800 ml. Beer's law was obeyed over the concentration range of 8 × 10⁻⁹ to 1.6 × 10⁻⁷ mol l⁻¹ with an apparent molar absorptivity of 6.53 × 10⁶ l mol⁻¹ cm⁻¹ for a 500 ml aliquot of the water sample. The detection limit (n = 7) was 5.0 × 10⁻¹⁰ mol l⁻¹ and the R.S.D. (n = 5) for 8.0 × 10⁻⁷ mol l⁻¹ of Hg(II) was 3.7%. A notable advantage of the method is that the determination of Hg(II) is free from the interference of almost all cations and anions found in the environmental and waste water samples. The determination of Hg(II) in tap, synthetic sea water and human hair samples was carried out by the present method and cold vapor atomic absorption spectrometry (CV-AAS). The results were satisfactorily comparable so that the applicability of the proposed method was confirmed to the real samples.     

双硫腙修饰固体银汞合金电极吸附伏安法测定痕量铅

制作了银汞合金电极,在其表面用双硫腙进行修饰,溶液中铅离子与电极表面的双硫腙发生螯合作用被富集。当电极电位在-0.20~-0.70V间进行阴极化扫描时,配合物中铅离子在电极表面被还原,于-0.40V左右形成灵敏的还原峰。选择了反应介质并优化了pH值、双硫腙用量、富集时间等实验参数。利用该修饰电极测定铅的线性范围为0.02~1.2mg/L,检出限为10μg/L。对0.6mg/L Pb2 溶液进行11次平行测定,相对标准偏差为4.1%。该法用于实际水样铅的测定,回收率为94.8%。     

双硫腙包覆钛酸锶钡粉体对水中镉的吸附性能

用草酸盐化学共沉淀法合成钛酸锶钡粉体,用双硫腙对该粉体表面进行包覆修饰,制成新型有机包覆吸附剂。用傅里叶变换红外光谱对包覆粉体进行了表征;以火焰原子吸收为检测手段,研究了该吸附剂对水中Cd2+ 的吸附性能,考察了洗脱条件;通过红外光谱,初步探讨了包覆和吸附作用机理。结果表明,双硫腙以氢键作用牢固地包覆于钛酸锶钡粉体上;该包覆粉体对水中的Cd2+具有较高的选择性吸附能力,其吸附量受介质的pH值影响,当pH值小于3时,该吸附剂对水中的Cd2+几乎不吸附,当pH值大于6时,吸附量达到最大;常温下,20 min内吸附达到平衡;吸附在双硫腙包覆钛酸锶钡粉体上的Cd2+,可用5% EDTA溶液完全洗脱。建立了吸附富集,火焰原子吸收法测定水中Cd2+的新方法,方法检出限为0.2 μg·L-1,相对标准偏差为2.9%。应用于自来水和地表水中Cd2+的测定,结果满意。     

表面活性剂-膜富集-紫外可见漫反射光谱法测定水中的痕量铅

提出了结合表面活性剂、膜富集和紫外可见漫反射光谱测定水中痕量铅的方法。在pH 8.5的氨水氯化铵缓冲溶液中,剧烈搅拌下,铅与双硫腙形成疏水性的红色络合物,该络合物能够被混合纤维素酯膜富集,并且在非离子表面活性剂聚氧乙烯月桂醚(Brij-30)的存在下,该络合物被混合纤维素酯膜富集的效率得到了很大提高,然后待膜自然干燥后直接测得膜表面的漫反射光谱。本文对表面活性剂类型、表面活性剂浓度、反应酸度、双硫腙浓度和反应时间等条件进行了优化。研究结果表明,在最佳实验条件下,最大吸收波长为485 nm,在5～100 μg·L-1范围内铅离子的浓度与其络合物的吸光度呈良好的线性关系,相关系数的平方R2为0.990 6,检出限为2.88 μg·L-1。研究发现下列共存离子不干扰铅离子的测定：500倍的K+,Na+,Ca2+,Mg2+,NH4+,NO-₃,Cl-,CH₃COO-,SO2-₄;10倍的Al3+(10%的NaF进行掩蔽),Fe3+(10%的NaF和酒石酸钾钠进行掩蔽),Hg2+和Zn2+(10%的NaSCN和酒石酸钾钠进行掩蔽);同等浓度的Cd2+,Cu2+。采用本方法测定瓶装水中的痕量铅,结果与石墨炉原子吸收光谱法(GFAAS)测定的结果基本一致,加标回收率在95.4%～104.5%之间,标准偏差(SD)在0.5～1.5 μg·L-1之间,说明本方法具有较好的准确性。本方法操作简单、灵敏度高,适用于瓶装水中痕量铅的测定。     

Determination of platinum and palladium in environmental samples by graphite furnace atomic absorption spectrometry after separation on dithizone sorbent

A graphite furnace atomic absorption method of platinum and palladium determination after their separation from environmental samples has been presented. The samples were digested by aqua regia and the analyte elements were separated on the dithizone sorbent. The procedure of sorbent preparation was described and their properties were established. Two various procedures of elution by thiourea and concentrated nitric acid were described and discussed. The low limit of detection was established as 1 ng g⁻¹ for platinum and 0.2 ng g⁻¹ for palladium.There was also investigated the behaviour of platinum and palladium introduced into the soil in various chemical forms.     

The Application of Nafion Metal Catalyst Free Carbon Nanotube Modified Gold Electrode: Voltammetric Zinc Detection in Serum

Metal catalyst free carbon nanotube (MCFCNT) whiskers were first used as an electrode modification material on a gold electrode surface for zinc voltammetric measurements. A composite film of Nafion and MCFCNT whiskers was applied to a gold electrode surface to form a mechanically stable sensor. The sensor was then used for zinc detection in both acetate buffer solution and extracted bovine serum solution. A limit of detection of 53 nM was achieved for a 120 s deposition time. The zinc in bovine serum was extracted via a double extraction procedure using dithizone in chloroform as a zinc chelating ligand. The modified electrode was found to be both reliable and sensitive for zinc measurements in both matrices.