浮选富集—原子吸收光谱法同时测定水中铜铅镉银

研究了浮选技术在富集水中铜铅镉银的应用,将这一技术与火焰原子吸收光谱法相结合,提高了灵敏度,操作简便.方法检出浓度铜为lμg·L~(-1),铅为10μg·L~(-1),镉为0.5μg·L~(-1),银为0.5μg·L~(-1),相对标准偏差和回收率均很满意.     

痕量Au Bi和Cd的萃取浮选及原子吸收光谱法测定

浮选法分离痕量金属离子,由于灵敏度高、选择性强已得到广泛应用。本文利用浮选法使Au~(3 )、Bi~(3 )和Cd~(2 )同KBr反应生成的络合阴离子与碱性染料罗丹明B(RB)生成既疏水又疏有机溶剂的三元离子缔合物,后者经甲苯浮选分出,用二甲基甲酰胺(DMF)溶解后,可用原子吸收法测定Au、Bi和Cd的含量。本方法用于海水,锌片和矿样中上述三种元素的微量测定,可提高检测灵敏度,而且K、Na、Ca、Mg等共存离子不生干扰。具体实验方法如下:     

火焰原子吸收光谱法测定高铋铅中的铜

建立了火焰原子吸收光谱法测定高铋铅中铜含量的方法。研究了多种溶样方法,最终采用硝酸-酒石酸溶解试样,在硝酸(10%)介质中以火焰原子吸收光谱法测定溶液中的铜量,加标回收率在99.4%~105%,相对标准偏差(RSD,n=7)小于3.5%。方法操作过程简单,精密度高,回收率良好,能够较好地满足分析检测的要求。     

火焰原子吸收光谱法直接测定食用菌中的铅和镉

采用火焰原子吸收法直接测定了食用菌中铅和镉的含量。方法灵敏、准确，测定时无须富集、萃取，操作简便，快速，铅和镉的相对标准偏差分别在3．3％～7．3％和3．1％～7．5％之间。回收率在94％～106％和95％～105％之间；检出限为0．016mg/L和0．008mg/L。     

浮选富集—原子吸收光谱法测定水中铅

近十多年来浮选富集技术得到很大发展,已应用于分析化学中.浮选富集是利用金属离子与KI、亚甲基蓝生成结合物M-I-MB体系,该络合物浮选于水相和有机相之上.分离后,所得浮选物已将溶液中金属富集.由于萃取浮选和溶剂萃取不同,与水相和有机相体积关系不大,故可取样量大,富集倍数高,使灵敏度得以提高.该技术广泛用于吸光光度法富集金属元素,但吸光光度法选择性差,需进一步分离,使操作复杂.现我们将此技术与原子吸收光谱法结合起来,不需进一步分离,可直接测定.选择性好,操作简便,结果满意.     

浊点萃取-火焰原子吸收光谱法测定痕量铜

2-磺酸基-4-甲氧基苯基重氮氨基偶氮苯(MOSDAA)和Cu(II)反应生成疏水性络合物后,被萃取到Triton X-114非离子表面活性剂胶束相中,火焰原子吸收光谱法测定其中的铜,建立了浊点萃取预富集-火焰原子吸收光谱法测定铜的方法。反应体系的pH、MOSDAA和Triton X-114的浓度、平衡温度及时间等实验条件被优化。在选择的实验条件下,方法的检出限为1.1 ng/mL(3σ),对浓度为0.1μg/mL的Cu(II)溶液平行测定6次,相对标准偏差为1.9%。方法已用于小米和水样中痕量铜的测定。     

火焰原子吸收光谱法测定锰电解液中铜锌镉铅

在酸性和低温条件下,用适量乙醇使锰电解液中的ＭｎＳＯ４沉淀分离,用火焰原子吸收光谱法直接测定锰电解液中铜,锌、镉和铅含量。方法简便、快速,实用,具有较高的精密度和准确性。相对标准偏差３．８％－４．５％,回收率９０．５％－１０６．５％,特征浓度铜为０．４９μｇ．ｍｌ＾－１／１％,锌为０．００８μｇ．ｍｌ＾－１／１％,镉为０．０１５μｇ．ｍｌ＾－１／１％,铅为０．１８μｇ．ｍｌ＾－１／１％。     

浊点萃取-火焰原子吸收光谱法测定食品和饮料中的痕量铜

研究了基于非离子表面活性剂TritonX-114和螯合剂二乙基氨基二硫代甲酸钠(DDTC)的浊点萃取-火焰原子吸收光谱法测定痕量铜的分析方法.考察了影响浊点萃取效率的参数,包括pH值、DDTC浓度、TritonX-114用量、平衡温度及时间等.在优化条件下,本法的检出限(3σ)为1.55μg/L,相对标准偏差RSD为3.4%(n=7,c=100μg/L),线性范围为0～250μg/L.将该法应用于茶叶标准样品(GBW07605)、奶粉和矿泉水等样品中痕量铜的测定,其回收率在96.7%～113.5%之间.     

浊点萃取-火焰原子吸收光谱法测定人尿液中的痕量铅

以双硫腙作为络合剂、聚乙二醇辛基苯基醚(TritonX-100)为非离子表面活性剂,建立浊点萃取-火焰原子吸收光谱测定尿液中痕量铅的方法。探讨了络合剂用量、平衡时间、pH值、TritonX-100用量、冰浴时间等因素对萃取效率的影响。结果表明:该方法对铅的最大富集倍数约为40倍,检出限为0.06μg·L-1(n=11)。回收率在96.7%~101%,线性范围为0~1.00μg·mL-1。利用该方法测定尿液中痕量铅的含量,结果令人满意。     

表面活性剂在火焰原子吸收法中的增敏作用研究

本文研究了火焰原子吸收法测定人发中铜含量时,表面活性剂十二烷基硫酸钠（SDS）的增敏作用.实验表明,在0.80%（V/V）HNO3存在下,0.08%（m/V）SDS可以提高吸收值约2～3倍.本法测定痕量铜的RSD≤2.1%（n=5）,回收率在88.8%～97.5%之间.     

螯合树脂在线富集火焰原子吸收法测定痕量铅和镉

在pH=4.88的乙酸-乙酸钠缓冲溶液中,用螯合离子交换树脂富集铅和镉,以1.50mol/L HNO3作洗脱液,火焰原子吸收法测定洗脱液中痕量铅和镉。该方法对铅和镉的线性范围分别是4.0～80.0μg/L和2.0～30.0μg/L,检出限分别为1.3μg/L和0.7μg/L。该方法用于地表水中痕量铅和镉的测定,分析结果满意。     

Sensitivity Enhancement for Slotted Quartz Tube Flame Atomic Absorption Spectrometry Using a Gas Screen

Slotted Quartz Tube (SQT) is a simple device that provides a sensitivity enhancement of 2–5 times in Flame Atomic Absorption Spectrometry (FAAS) depending on the element. A Gas Screen-Slotted Quartz Tube (GS-SQT) was designed to further increase sensitivity. For this purpose, two slotted gas chambers were fixed on the left and right sides of a burner head and Ar gas was supplied into these chambers perpendicular to the light path to produce two thin layers of gas screen. It was observed that these Ar screens can move up the flame tails in two ends of SQT. In addition to an increase in sensitivity by the use of SQT, Ar screen resulted in a further improvement in characteristic concentrations, C₀, by a factor of 1.60 for Cd, 2.01 for Co, 1.42 for Cu, 1.94 for Mn, 1.86 for Ni, 1.78 for Pb, 1.62 for Se, and 1.09 for Zn. In addition to the enhancement in sensitivity, gas screen also helps by protecting the spectrometer from the adverse effect of using slotted quartz tube. The system is very simple and low-cost; it can be produced and applied easily.     

Determination of Melamine Based on the Formation of an Insoluble Copper-Melamine Complex and Flame Atomic Absorption Spectrometry

A copper-melamine complex was optimally synthesized by heating excess copper(II), as 50 m mol L^?1 copper(II) chloride in 50% (v/v) methanol, and melamine at 80°C. The amount of residual copper(II) in solution after removal of the copper-melamine complex was then measured by flame atomic absorption spectrometry. The concentration of depleted copper was proportional to the concentration of melamine, with a linear calibration curve (melamine concentration against copper absorbance) between 0.5 and 2.5 m mol L^?1 (R² = 0.9943) and with a limit of detection of 0.50 m mol L^?1. Although external standard calibration provided poor recoveries in fortified fish flesh (40% to 74% for 5 to 10 mg melamine/g), the method of standard addition provided acceptable values (90% to 93%), with a relative standard deviation of 3% to 10%. The results obtained with the standard addition method were in broad agreement with those obtained by high performance liquid chromatography.     

Determination of Silver by Flame Atomic Absorption Spectrometry after Preconcentration on Naphthalene Modified with Dithizone

A solid‐phase extraction method for preconcentration of silver and consequent determination by atomic absorption spectrometry is described. The method is based on the adsorption of silver on naphthalene modified with dithizone in a column. The adsorbed silver is eluted from the column with a thiourea solution and determined by flame atomic absorption spectrometry. The adsorption conditions including pH, reagent concentration, eluent volume, flow rate and interfering ions were investigated. The calibration graph was linear in the range 10–1000 ng mL^?1 of Ag in the initial solution with r = 0.9998. The limit of detection based on 3S_b was 3.9 ng mL^?1. The relative standard deviation for ten replicate measurements of 40 and 600 ng mL^?1 of Ag was 4.4% and 0.9%, respectively. The method was applied to the determination of silver in mineral, radiology film and wound dressing samples.     

流动注射-在线富集火焰原子吸收分光光度法测定痕量铅

本文报道在流动注射分析体系中用装有黄原脂棉的微型柱对溶液中Pb2 进行在线富集后,用3.0 mol/L盐酸洗脱柱上富集的Pb2 ,然后采用火焰原子吸收光谱法在线测定痕量Pb2 ,方法的线性范围为0.5～100μg/L。与未富集前相比,测定的灵敏度可提高65倍。方法用于环境水样中痕量Pb2 的测定,回收率在97.0%～102%之间,相对标准偏差小于4.0%,分析结果满意。     

缝式石英管捕集技术的改进

试验了各种条件对Ag、Au、Cu、Pb和Zn灵敏度影响.结果表明,分别用不同火焰条件进行原子捕集与释放可获得最佳灵敏度。捕集1min,测得Ag、Au、Cu、Pb和Zn的特征浓度分别为8.1×10、1.7×10~(-3)、1.8×10~(-3)、2.4×10~(-3)和1.3×10~(-4)μg/ml,比常规火焰原子吸收光谱法的灵敏度分别提高62、106、28、83和77倍。Ag、Au、Cu、Pb和Zn的相对标准偏差依次为2.8％、3.1％、2.6％、2.7％、5.4％。本法测定了牡蛎中Ag和Cu。     

流动注射在线液-液萃取火焰原子吸收法测定水中痕量铅

提出了一种流动注射在线液－液萃取火焰原子吸收直接测定水中痕量铅的分析方法。实验以APDC为螯合剂,用MIBK为萃取剂,研究了在线萃取中各种实验参数、酸度条件的影响,考察了共存元素的干扰。方法的RSD（n=12)为2．7％,测定检出限为3．1μg/L,回收率为96％－106％。     

Coprecipitation for the Determination of Copper(II), Zinc(II), and Lead(II) in Seawater by Flame Atomic Absorption Spectrometry

A TiO(OH)₂ precipitate was used for the preconcentration of copper(II), zinc(II), and lead(II) in seawater prior to determination by flame atomic absorption spectrometry. The influence of pH, sample volume, amount of precipitate, and centrifugation time were optimized for quantitative recoveries of the analytes. Under the optimum conditions, the detection limits of copper(II), lead(II), and zinc(II) were 4.3, 9.7, and 9.6 micrograms per liter, respectively. The recoveries of analytes were between 95.00 and 103.00 percent with the relative standard deviation below 6 percent. The procedure was validated by the analysis of NASS-5 and SPS-WW1 Batch 109 standard reference materials and the procedure was successfully applied to seawater.     

Determination of Cadmium in Fruit and Vegetables by Ionic Liquid Magnetic Microextraction and Flame Atomic Absorption Spectrometry

An ionic liquid-linked dual magnetic microextraction procedure is reported for cadmium(II) with flame atomic absorption spectrometry. Cadmium was complexed with pyrolidine dithiocarbamate and the chelate was extracted into the fine droplets of 1-butyl-3-methylimidazolium hexafluorophosphate by using a vortex mixer with Fe₃O₄ nanoparticles. Plackett–Burman design was used to optimize relevant parameters of the method, including the pH, the volume of ionic liquid, the amount of ammonium pyrolidine dithiocarbamate, the mass of magnetic nanoparticles, and the vortex time. The pH, volume of ionic liquid, and mass of ammonium pyrolidine dithiocarbamate significantly affected the recovery. The limit of detection, preconcentration factor, and relative standard deviation were 0.32 µg L^?1, 80, and 3.4%, respectively. The procedure was validated by the analysis of spinach leaves standard reference material 1570a and recovery measurements. Practical application of the method involved the determination of cadmium in fruit and vegetables.