2-乙基己醇萃取-原子吸收光谱法测定微量镓

在７．０ｍｏｌ／Ｌ盐酸介质中,在抗坏血酸存在下,用２－乙基己醇萃取试样溶液中的酸性铬蓝Ｋ－镓的络合物,然后用３０ｇ／Ｌ的硫脲将络合物反萃取到水相中,用ＦＡＡＳ法测定镓,据此建立了萃取反萃取－ＦＡＡＳ法测定微量镓的新方法。方法线性范围为０～６０．０ｍｇ／Ｌ,灵敏度为０．２８ｍｇ／Ｌ／１％,已用于铝酸钠溶液中微量镓的测定。     

金属有机化合物中过渡金属的原子吸收分光光度法测定

本文报导应用火焰原子吸收分光光度法对金属有机化合物中过渡金属铜、镍、钴、铁、钼及铬的定量测定。我们将金属有机化合物溶解在适当的有机溶剂或水中,不必分离基体,即可用标准加入法直接进行测定。操作简单,速度快,相对误差<0.4％。     

盐酸苯海拉明的原子吸收法测定

探讨了盐酸苯海拉明在适当的酸性条件下与锌试剂、铜离子定量生成三元络合物,经ＭＩＢＫ萃取,以ＡＡＳ法测定萃取液听 铜来间接测定盐酸苯海拉明的量。本法与药典法相比,相对平均偏差小于０．４％,线性范围为５～５０μｇ．ｍＬ＾－１。回收率为９７％～１０２％。     

间接原子吸收法测定药物制剂中利血生的含量

提出了利血生的间接原子吸收法，该法基于利血生在碱性介质中的分离－产物半胱氨酸在适当的PH条件下与铜离子生成灰色沉淀，通过测定上清液中铜的含量来间接测定利血生的含量，在法在10－100mg/L范围内呈良好的线性关系（r=0.9992),回收率为98．5％－101．6％。该法可成功地用于药物制剂中利血生的测定。     

Coprecipitation Behavior of Some Metals with Chitosan and Their Determination by Graphite Furnace Atomic Absorption Spectrometry

Chitosan is derived from chitin by deacetylation. Chitosan forms a complex with metal ions and is soluble an organic acid. The metal ions were concentrated in the precipitates of chitosan when the sample solution containing metal ions was adjusted to neutral after the chitosan solution was added. These properties are applied to the preconcentration of metal ions in water samples and their determination by graphite furnace atomic absorption spectrometry. Metal ions,such as ruthenium, indium, vanadium, strontium,rhodium were collected in the chitosan precipitates.     

Determination of Gold in Biological Materials by Atomic Absorption Spectroscopy

Abstract

A method for the determination of gold in biological materials such as serum, urine, synovial fluid and tissues was investigated. After the dry ashing of the samples, gold was extracted from 6 M HCL into MIBK. The amount of gold was determined directly in the organic phase by the atomic absorption spectrometry. The range of the working curve was from 0.1 to 5.0 μg and the accuracy and recovery of the present method were satisfactory for practical purposes.     

间接原子吸收光谱法测定药物制剂中的西米替丁

本文提出了流动注射原子吸收光谱法间接测定西米替丁的新方法。基于西米替丁与Ag（I）反应可以生成白色的沉淀,经流动注射在线过滤稀释,以原子吸收光谱法测定反应剩余银离子的量来间接测定西米替丁的量。在优化条件下西米替丁浓度在2～80mg／L范围内与吸光度呈良好的线性关系,回收率为97．0％～104．3％。方法用于片剂西米替丁的测定,结果满意。     

海水中铜锌铅镉的萃取-反萃取法同时提取-原子吸收光谱法测定

采用萃取-反萃取法同时提取出海水中Cu、Zn、Pb、Cd,Cu、Pb、Cd石墨炉法测定,Zn用火焰法测定.对样品的前处理方法和最佳仪器条件进行了研究,并通过加标实验验证了方法的可靠性.结果表明:萃取-反萃取法能完全满足海水中Cu、Zn、Pb、Cd的前处理要求,可节省一半前处理时间,有溶液稳定、环保、节省试剂等优点.     

Column Solid-Phase Extraction with 2-Acetylmercaptophenyldiazoaminoazobenzene (AMPDAA) Impregnated Amberlite XAD-4 and Determination of Trace Heavy Metals in Natural Waters by Flame Atomic Absorption Spectrometry

A column solid-phase extraction (SPE) preconcentration method was developed for the determination of Cd, Co, Cu, Ni and Zn ions in natural water samples by flame atomic absorption spectrometry. The procedure is based on the retention of analytes in the form of 2-acetylmercaptophenyldiazoaminoazobenzene (AMPDAA) complexes on a short column of AMPDAA-XAD-4 resin from buffered sample solution and subsequent elution with hydrochloric acid plus sodium chloride. Important SPE parameters were optimized using model solutions. The loading half-time, t_1/2, for Cd, Co, Cu and Zn was found to be less than 5min, and for Ni the value was 12min. The detection limit for Cd, Co, Cu, Ni and Zn was 0.028, 0.064, 0.042, 0.023 and 0.16µgL^–1, respectively, and the quantification limit was 0.043, 0.11, 0.099, 0.044 and 0.29µgL^–1, respectively. The AMPDAA-XAD-4 resin has good selectivity for Cd, Co, Cu, Ni and Zn over several electrolytes, especially over earth alkaline metals with tolerance limits of 0.05molL^–1. The method was validated by analysing a standard reference material (GBW 08301), and it was found that the results agree with those quoted by the manufactures. The developed method was applied to the determination of trace metal ions in tap water and river water samples with satisfactory results.     

磷酸三丁酯萃取火焰原子吸收法间接测定植物和煤灰中的痕量锗

本文报道了磷酸三丁酯萃取-火焰原子吸收法间接测定植物及煤灰样品中痕量锗的新方法。锗与钼酸铵在0．3mol／L的硝酸介质中形成稳定的锗钼杂多酸,被磷酸三丁酯萃取,有机相直接进样测定钼而间接测定锗;特征浓度为21．8ng／mL／1％吸光度,RSD(n=11)为4．6％,加标回收率为97．6％～101．2％。     

原子吸收光谱法测定香烟烟气中重金属的含量

用原子吸收、荧光光谱法测定了不同品种香烟烟气的水吸收液中铅(Pb)、镉(Cd)、铬(Cr)、汞(Hg)的含量,并用等离子体发射光谱法进行比较测定。结果表明,原子吸收光谱法具有灵敏度高、干扰小、快捷的优点。方法回收率为98%～100%,相对标准偏差小于5.0%。实际样品测定结果令人满意。     

固相萃取-火焰原子吸收光谱法测定金

将多孔石墨化炭黑与5-硫代-15-冠-5的乙醚溶液混合后,蒸干溶剂乙醚.将所得的混合物填入聚四氟乙烯柱中,制得固相萃取柱.萃取柱经0.1 mol·L-1的硫代硫酸钠和pH 3.5的乙酸盐缓冲溶液洗涤后,用0.1 mol·L-1的硫代硫酸钠溶液反向洗脱小柱上富集的金,洗脱液供火焰原子吸收光谱法测定.方法用于矿石和环境水样中金的实际测定,结果与电感耦合等离子体质谱法的结果一致,相对标准偏差(n=5)在2.4%～3.4%之间,回收率在92.6%～97.8%之间.     

浊点萃取-氢化物发生原子吸收光谱法测痕量汞

提出了浊点萃取预富集氢化物发生-原子吸收光谱法测定痕量汞的新方法。详细探讨了溶液pH值、表面活性剂浓度、平衡时间等因素对浊点萃取效果的影响。在优化的实验条件下,该法对汞的富集倍数为20倍,检出限为0.039μg/L,相对标准偏差(RSD)为4.8%(n=11)。所建立的方法用于天然水中痕量汞的测定,分析结果满意。     

High-Resolution Continuum Source Atomic Absorption Spectrometry with Microwave-Assisted Extraction for the Determination of Metals in Vegetable Sprouts

The goal of this study was to investigate the enrichment of garden cress (Lepidium sativum), mung beans (Vigna radiata), and soybeans (Glycine max) with minerals. Hydroponic nutrient solutions were enriched with Zn²⁺,Cr³⁺, Ca²⁺, Mg²⁺, and Se²⁺. Morphological assessment was based on monitoring changes that occurred as a function of the concentrations of elements in the medium. The growth of the plant, as a result of a stimulating or inhibitory effect of the identity and concentration of elements on the germination process, was characterized. Microbiological contamination was identified and catabolic profiles of two bacterial strains were performed. High-resolution continuum source atomic absorption spectrometry (HR-AAS) was used to determine Zn²⁺, Cr³⁺, Ca²⁺, Mg²⁺, and Se²⁺ in dried plant material after sample pretreatment using microwave-assisted extraction. The limits of detection were 0.010, 0.029, 0.013, 0.151, and 0.030 milligram per liter for Ca²⁺, Cr³⁺, Mg²⁺, Se²⁺, and Zn²⁺, respectively. Recoveries were higher than 98 percent and the relative standard deviation was less than 5 percent. The accuracy of the procedure was estimated by analyzing certified reference materials. The results showed that biofortification of garden cress by zinc holds the highest promise for the creation of designer foods. Garden cress was found to have the highest bioconcentration factor among the investigated plants; at 50 parts per million, plant growth was stimulated without contamination by microorganisms.     

Kinetics and Determination of Some Transition Metals with Peri-Dihydroxynaphthindenone

Abstract

A simple sensitive and selective spectrophotometric method has been developed for determination of some transition metal ions. It is based on the reaction of the metal ions with excess peri-dihydroxynaphthindenone in 80% v/v ethyl alcohol-water mixture at 30°C. The colored products obtained display maximum absorption band at 560–590 nm depending upon the type of transition metal ion used, and E_{1 cm} ^1% in the range 70–480. Under the optimum conditions results with an average recovery of 96%, (mean standard deviation ±3% are obtained for 6 different transition metal ions without any significant interference from Li⁺, Na⁺, K⁺, Cs⁺, Rb⁺, Ba²⁺, Sr²⁺, Ni²⁺, Bi³⁺, Co²⁺, Mn⁺², Cd⁺² and Al⁺³. Kinetic data reveal that the reaction proceeds via a second order route (first order with respect to either the metal cation or ligand). The activation parameters and a suggested mechanism have been presented, and the nature of bonding in the solid chelate products has been verified.     

微乳相萃取分离富集-原子吸收光谱法分析铬形态

建立了一种微乳相萃取分离-石英双缝管原子捕集火焰原子吸收光谱法(STAT-FAAS)分析环境水样中铬形态的新方法。该方法中,Cr(Ⅲ)与8-羟基喹啉反应形成的疏水性配合物,经萃取进入微乳相,Cr(Ⅵ)留在水溶液中,从而实现Cr(Ⅲ)与Cr(Ⅵ)的相互分离。Cr(Ⅵ)含量的测定通过过氧化氢溶液将Cr(Ⅵ)还原为Cr(Ⅲ),按同样方法分析。实验对微乳相萃取的主要影响因素进行了优化。结果表明,经优化后实验条件为:平衡温度80℃,平衡时间10min,溶液酸度pH=9.0,NH3-NH4Cl缓冲溶液用量2.0mL,8-HQ用量0.05mmol;TritonX-100微乳液组成:m(TritonX-100):m(正戊醇):m(正己烷):m(水)=3.0:15:1.5:4.0。在此条件下,萃取的富集倍数达到25倍(50mL起初样品溶液/2mL最终测定液),线性范围为2.5～500μg/L,检出限为0.62μg/L,相对标准偏差(RSD)为3.8%(n=10,c=10μg/L)。本方法已成功地应用于电镀废水中铬形态分析。     

溶剂萃取-石墨炉原子吸收光谱法测定水样中的痕量铅

本文采用2-(5-溴-2-吡啶偶氮)-5-二乙氨基苯酚(5-Br-PADAP)为络合剂,辛醇为提取剂,提出了有机溶剂萃取-石墨炉原子吸收光谱测定水样中痕量铅的分析方法。对萃取和石墨炉升温条件进行了优化。在本实验条件下,方法的线性范围在0.5~5.0μg/L之间,检出限为0.067μg/L,相对标准偏差(RSD)为3.9%(n=7),回收率在89%~97%范围。本法与未经溶剂萃取的方法相比,线性斜率提高了约20倍。本法已用于环境水样中痕量Pb的测定,测定结果与ICP-MS的分析结果具有良好的一致性。     

Selective Determination of Copper in Water Samples by Atomic Absorption Spectrometry after Cloud Point Extraction

A preconcentration methodology utilizing the cloud point phenomenon is described for the determination of copper by flame atomic absorption spectrometry. The reagent Sulfathiazolylazo resorsin was used as a complexing agent. The preconcentration factor of 25-fold was obtained. The calibration curve is linear in the range of 4–400 µ g L^?1 with a limit of detection of 0.64 µ g L^?1. The relative standard deviation (n = 5, 12 µ g L^?1) was 3.5%. The cloud point is formed in the presence of phenol at room temperature. The method was successfully applied to the determination of copper in water samples and a standard reference material.     

Determination of Iron in Zirconium by Electrolytic Dissolution and Atomic Absorption Spectroscopy

Abstract

A simple method for the determination of iron in the range of 0.01–1.00% in zirconium metal and its alloys is described. The method is based on the electrolytic dissolution of zirconium into an organic solvent and the subsequent measurement of iron by atomic absorption spectroscopy. The method is rapid, requiring 30 minutes for one measurement.     

间接原子吸收法测定苯并三氮唑

乙酸钠介质中 ,加入过量的铜 (Ⅱ )与苯并三氮唑生成沉淀 ,用火焰原子吸收法测定上清液中剩余的铜(Ⅱ ) ,工作曲线法测定了工业合成样品及内燃机冷却水中的苯并三氮唑。该方法测定苯并三氮唑线性范围为1 2mg/L～ 30mg/L ,回收率 (n =5)为 98.9～ 1 0 1 .0 %。文中还测定了难溶化合物的溶解度、溶度积和化合物的组成比。