Determination of Ultratrace Amounts of Copper(Ⅱ) in Water Samples by Electrothermal Atomic Absorption Spectrometry After Cloud Point Extraction

A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry （ETAAS） after cloud point extraction （ CPE ）. 1-（ 2-Pyridylazo ） -2- naphthol was used as the chelating reagent and Triton X-114 as the mieellar-forming surfactant. CPE was conducted in a pH 8. 0 medium at 40 ℃ for 10 rain. After the separation of the phases by contrifugafion, the surfactant-rieh phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20μL of the diluted surfactant-rieh phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconeentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0 ng/mL, and the relative standard deviation was found to be less than 3. 1% for a sample containing 1.0 ng/mL Cu （ Ⅱ ）. This developed method was successfully applied to the determination of uhratraee amounts of Cu in drinking water, tap water, and seawater samples.

Flow Injection Semi-online Preconcentration Graphite Furnace Atomic Absorption Spectrometry for Determination of Cadmium,Copper and Manganese

A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements. The analytical performances of the prospsed method for determining Cd, Cu and Mn were studied. The analytes were preconcentrated with a thiol resin(Type 190, produced by Nankai University, China) whose active group is -SH. The elements to be determined were preconcentrated onto the column for 60 s and then rinsed with deionized water and eluted with 30 μL of 1 mol/L HCl. The graphite furnace atomic absorption spectrometry(GFAAS) determination of the concentrated analyte was carried out in parallel with the next preconcentration cycle. Enrichment factors 41, 22 and 20 and detection limits(3 σ , n =10) 0.36, 3.8 and 7.0 ng/L for Cd, Cu and Mn, respectively, along with a sampling frequency of 20 h -1 , were obtained with a 60 s loading time at a sample flow rate of 3.5 mL/min. The analytical results for a number of water samples show that the flow-injection semi-online column preconcentration can not only eliminate the effect of some concomitant elements, such as Li, Na, K, Ca and Mg, on the determination of the analyte, but also enhance the sensitivity.

Uncertainty in Detecting Copper and Zinc Contents in Maize Flour by Flame Atomic Absorption Spectrometry with Wet Digestion Method

[ Objective] This study aimed to evaluate the uncertainty in detecting copper and zinc contents in maize flour by flame atomic absorption spectrometry. [ Method] Combined with the actual inspection experience, the uncertainty in detecting copper and zinc contents in maize flour by tame atomic absorption spec- trometry was evaluated to establish the mathematical model. The uncertainty sources in the experimental process were investigated to analyze several components af- fecting the uncertainty in sample detection, including sample weighing, standard material transfer, solution dilution and volume setting, curve fitting, and repeat- ability of measurement instruments. [ Result] Standard curve fitting and repeatability test were two major factors that significantly affected the combined standard uncertainty. However, in the actual detection process, standard curve calibration and repeated detection procedures should be controlled strictly. Finally, the ex- panded uncertainty of copper and zinc contents in maize flour was （ 1.38 ± 0.08） mg/kg and （ 10.20 ± 1.20） mg/kg, respectively. [ Conclusion] This study provided reference for improving the accuracy and reliability of the detection method.

Determination of Copper and Lead Contents in Soil of the Yellow River Wetland in Shaanxi Province by Flame Atomic Absorption Spectrometry

[Objectives] The contents of copper and lead in the soil of the Yellow River Wetland were determined by flame atomic absorption spectrometry, which provides a theoretical basis for the treatment of soil pollution. [Methods] The soil was digested with a concentrated nitric acid-hydrofluoric acid-perchloric acid system, and the contents of heavy metals such as copper and lead in the Yellow River Wetland of Shaanxi Province were determined by flame atomic absorption spectrometry. [Results] The correlation coefficients reached 0.999 5 in the range of 0.00-1.00 mg/L, indicating good linearity. [Conclusions] The method is simple in operation, good in reproducibility, high in sensitivity to most elements, and can be widely used.

FLAME ATOMIC ABSORPTION DETERMINATION OF COPPER IN CEREALS FOOD SAMPLES WITH THE PRECONCENTRATION OF POTASSIUM TETRATITANATE WHISKER

A simple and reliable method has been developed for separation and preconcentration of trace amounts of copper ions in cereals food for subsequent measurement by flame atomic absorption spectrometry （FAAS）. The Cu^2＋ ions are adsorbed selectively and quantitatively during the passage. The retained copper ions were desorbed from the potassium tetratitanate whisker with 10.0mL of 2mol/L sulphuric acid solutions as eluent and were determined by FAAS. The linear range was 0.05μg/mL-0.20μg/mL in the original solution with a correlation coefficient of 0.9998. The detection limit of the proposed method is 2. lng/mL in the original solution （3σ, n=9）. Determination of copper in standard ions showed that the proposed method has good accuracy （recovery was more than 95%）. The method was successfully applied for recovery and determination of copper in cereals food samples

A novel method for the determination of trace copper in cereals by dispersive liquid-liquid microextraction based on solidification of floating organic drop coupled with flame atomic absorption spectrometry

A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop（DLLME-SFO） followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient（r） of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.

Determination of Copper by Flame Atomic Absorption Spectrometry after Preconcentration with Activated Carbon Impregnated with a New Schiff Base

A simple and reliable method for the extraction and determination of trace amounts of copper（Ⅱ） ions using activated carbon （AC） impregnated by a new Schiff base 5-[（4-heptyloxyphenyl）azo]-N-（4-propyloxyphenyl）-salicylaldimine （HPPS） and atomic absorption spectrometry is presented. Recovery efficiency and the influence of pH value, volume of sample solution, effect of different eluents, and interfering ions were evaluated. The limit of detection （3σ） was 2.62 ng.mL^-1 and the relative standard deviation （n=10） was 1.5%. Under optimum conditions, the copper ions were concentrated 25 fold using 250 mL of sample solution and 10 mL of eluent. This procedure has been successfully applied to the determination of copper in different water samples.

Preconcentration and Determination of Copper（Ⅱ） Using Octadecyl Silica Membrane Disks Modified by 1,5-Diphenylcarhazide and Flame Atomic Absorption Spectrometry

A simple and reproducible method for the rapid extraction and determination of trace amounts of copper（Ⅱ） ions using octadecyl-bonded silica membrane disks modified by 1,5-diphenylcarbazide （DPC） and atomic absorption spectrometry was presented, which was based on complex formation on the surface of the ENVI-18 DISK^TM disks followed by stripping of the retained species by minimum amounts of appropriate organic solvents. The elution was efficient and quantitative. The effect of potential interfering ions, pH, ligand amount, stripping solvent, and sample flow rate were also investigated. Under the optimal experimental conditions, the break-through volume was found to be about 1000 mL providing a preconcentration factor of 400. The maximum capacity of the disks was found to be （255±5） lag for Cu^2＋, and the limit of detection of the proposed method was 5 ng per 1000 mL. The method was applied to the extraction and recovery of copper in different water samples.

Solid Phase Extraction of Trace Copper（Ⅱ） Using Octadecyl Silica Membrane Disks Modified with N,N′-Disalicylideneethylenediamine

A simple and reproducible method for the rapid extraction and determination of trace amounts of copper（Ⅱ） ions using octadecyl-bonded silica membrane disks modified by N,N′-disalicylideneethylenediamine （DESDA） and atomic absorption spectrometry was presented. The method is based on complex formation on the surface of the ENVI-18 DISK^TM disks followed by stripping of the retained species by minimum amounts of appropriate organic solvents. The elution is efficient and quantitative. The effects of potential interfering ions, pH, ligand amount, stripping solvent, and sample flow rate were also investigated. Under the optimal experimental conditions, the break-through volume was found to about be 1000 mL providing a preconcentration factor of 500. The maximum capacity of the disks was found to be （389±4） μg for Cu^2＋. The limit of detection of the proposed method is 5 ng per liter. The method was applied to the extraction and recovery of copper in different water samples.

Ultrasound-assisted emulsification solidified floating organic drop microextraction for the determination of trace amounts of copper in water samples

A simple and efficient liquid-phase microextraction(LPME)technique was developed using ultrasound-assisted emulsification solidified floating organic drop microextraction(USAE-SFODME)combined with flame atomic absorption spectrometry,for the extraction and determination of trace copper in water samples.1-(2-Pyridylazo)-2-naphthol(PAN)was used as chelating agent.Microextraction efficiency factors(including extraction solvent type,extraction volume,time,temperature,and pH),the amount of the chelating agent,and salt effect were investigated and optimized.Under the optimum extraction conditions,figures of merit of the proposed method were evaluated.The calibration graph was linear in the range of 20–600 mg·L^(–1)with a detection limit of 0.76 mg·L^(–1).The relative standard deviation(R.S.D)for ten replicate measurements of 20 and 400 mg·L^(–1)of copper was 3.83%and 2.65%,respectively.Finally,the proposed method was applied to tap water,river water,and sea water,and accuracy was assessed through the analysis of certified reference water or recovery experiments.

火焰原子吸收光谱法测定岩石样品中铜、铅、锌的研究

主要研究火焰原子吸收光谱法测定岩石样品中的铜、铅、锌。采用石墨消解仪和HF-HCl-HNO3-HClO4酸系消解样品的前处理方法效果相对较好,酸性介质可用盐酸或硝酸溶液,浓度宜为2%~5%。通过实验得出:铜、铅、锌的检出限分别为0.012μg/mL、0.057μg/mL、0.009μg/mL,测定下限分别为0.048μg/mL、0.228μg/mL、0.036μg/mL,方法RSD值(精密度)1.0%~3.6%,加标回收率97.29%~101.0%,符合岩石矿物分析规范的要求。火焰原子吸收光谱法测定铜、铅、锌具有操作简便、实验用时短、干扰少及较好的准确度和精密度的特点。

火焰原子吸收光谱法、石墨炉原子吸收光谱法和电感耦合等离子体发射光谱法测定地表水样中铜的研究方法对比

采用火焰原子吸收光谱法(FAAS)、石墨炉原子吸收光谱法(GF-AAS)和电感耦合等离子体发射光谱法(ICP-OES)分别测定地表水中的铜,对检出限、精密度、正确度、低浓度环境样品测试等指标进行对比。实验结果表明,三种方法对于测定地表水中铜,测试结果无显著差异;与FAAS和ICP-OES法相比,GF-AAS法具有较低的检出限、较高灵敏度,对于测定低浓度环境样品具有较高的准确性。

Preparation and adsorption behaviors of Cu(Ⅱ) ion-imprinted polymers

Imprinted polymers were prepared for selective removal of Cu（Ⅱ） ions from metal solutions. Three ion-imprinted polymers were synthesized with methacrylic acid （MAA）, acrylamide （AA） and N,N＇-methylenebisacrylamide （MBAA） respectively as the functional monomers, ethleneglycoldimethacrylate （EGDMA） as the cross-linking agent, 2,2＇- azobisisobutyronitrile （AIBN） as the initiator and Cu （Ⅱ） ion as the imprint ion. The template Cu （Ⅱ） ion was removed from the polymer by leaching with a liquid of a 1：1 volumetric ratio of HCl to ethylenediaminetetraacetic acid （EDTA）. The capacity and selectivity of Cu（Ⅱ） ion adsorption were investigated with the three imprinted polymers and their non-imprinted counterparts. The polymers have a maximum adsorption capacity at pH 7.0. The isotherm of their batch adsorption of Cu（Ⅱ） ions shows a Langmuir adsorption pattern. Imprinted polymers all have a much higher capacity and higher selectivity of Cu（Ⅱ） adsorption than nonimprinted ones. MAA polymer benefits the most from imprinting. Imprinted MAA polymer has the highest selectivity when used to rebind Cu （Ⅱ） ion from an aqueous solution in the presence of other metal ions. Ion imprinting can be a promising technique of preparing selective adsorbents to separate and preconcentrate metal in a medium of multiple competitive metal ions through solid phase extraction （SPE）.

便携式钨丝电热原子吸收光谱仪测定水样中铜、铬、铅和镉

以钨丝原子化器和小型化CCD检测器为主要部件,组装了便携式钨丝电热原子吸收光谱分析仪,优化了载气(Ar/H2)流速、空心阴极灯位置、原子化器高度、灰化和原子化电流等主要仪器条件。最佳载气(Ar/H2)流速(mL/min)为600/300(Cd),800/200(Cu,Pb,Cr);灰化电流为2.9～3.2 A;原子化电流为8.5 A;CCD的积分时间为50 ms。并在优化的仪器条件下准确测定了环境水样中的铜(Cu)、铬(Cr)、铅(Pb)和镉(Cd),进样10μL时,其检出限分别为2、5、9和0.5μg/L。此便携式原子吸收光谱仪在环境水样痕量元素分析中可望有良好的应用前景。

微波消解-原子吸收法快速测定莼菜中铜、锌的含量

应用微波消解制备系统,对莼菜湿样中铜、锌元素进行了微波消解研究,并采用原子吸收法测定其元素的含量。通过L9(34)正交设计,讨论了HNO3/H2O2比、固液比、消解时间、微波功率对微波消解结果的影响。最佳的消解条件为:HNO3/H2O2(V/V)=1:1,固液比(g/ml)=1:12,消解时间为6min,微波功率为700W。在最佳微波消解条件下,进行了精密度实验、回收率实验和金属离子干扰实验。结果表明,所得铜的回收率在97.60%～102.80%之间,RSD为4.61%;锌的回收率在98.40%～101.80%之间,RSD为6.19%。微波消解法处理莼菜湿样,具有快速、简便、节约试剂、消解完全等特点,测定结果的精密度、准确度令人满意。

火焰原子吸收光谱法测定云冈石窟风化岩石中钙铜铁锰

采用HF-HNO3-HClO4混酸消化样品,HNO3溶解盐类,火焰原子吸收光谱法直接测定试液中钙、铜、铁、锰的含量。对共存离子的干扰情况进行了考察,发现大量的Si对测定有干扰,在处理样品时通过生成SiF4除去;磷、铝、钛等元素对钙的化学干扰,通过加入释放剂SrCl2消除。背景吸收使用氘灯扣除。采用标准曲线法测定,Ca、Cu、Fe、Mn的校准曲线的线性范围分别为0.00－20.00μg/mL、0.00－6.00μg/mL、0.00－10.00μg/mL、0.00~6.00μg/mL,检出限分别为0.000 3μg/mL、0.001 3μg/mL、0.002 6μg/mL、0.006 9μg/mL。方法用于云冈石窟风化岩石中钙、铜、铁、锰的测定,相对标准偏差分别为2.8%、3.0%、1.4%、2.9%,加标回收率在96%－110%之间。

导数-原子捕集-火焰原子吸收光谱法测定中草药中的微量铜

研究了在原有基础上对原子捕集装置的改进 ,并与导数原子吸收光谱法结合 ,使铜的测定灵敏度有较大提高。在 10mV min灵敏度档下 ,捕集时间为 2min时 ,方法的检出限和特征浓度分别为 0 .5 2和 0 .85μg L,分别较常规火焰原子吸收法改善 1和 2个数量级。利用该法成功测定了甘草、柴胡等 10味中药中的微量铜 ,平均回收率为 94.2 %～ 10 4%。

浊点萃取-火焰原子吸收光谱法测定微量铜

本文研究了浊点萃取 -火焰原子吸收光谱法测定微量铜。利用表面活性剂浊点特性实现胶束相分离 /富集微量待测离子。探讨了影响浊点萃取的因素。该方法用于自来水、河水及标准土壤中痕量铜的测定 ,具有低毒、高效、安全、简便等特点。

微波消解-火焰原子吸收光谱法测定铜精矿中银

以王水为消解体系,采用3步程序升温微波消解法处理样品,选择8%(体积分数)王水为测定介质,实现了火焰原子吸收光谱法(FAAS)对铜精矿样品中1.6~600.0g/t银的测定。干扰试验表明,样品中的铜和铁对银测定的干扰可忽略。在选定的实验条件下,以银质量浓度为横坐标,测得的吸光度为纵坐标绘制校准曲线,其线性相关系数为0.999 8。方法检出限为1.6g/t。采用实验方法对3个铜精矿标准物质分别测定11次,测定值与认定值一致,相对标准偏差(RSD)为0.23%~0.66%。选取5组不同银含量的铜精矿样品,按照实验方法测定,并根据测得银含量的不同范围,分别与国标方法 GB/T 3884.2—2012中的酸溶-FAAS和火试金-滴定法测得结果进行对比,结果表明,二者基本吻合。

火焰原子吸收光谱法连续测定钴矿中Co,Ni和Cu

用HCl HNO3 KClO3溶解试样,在几个相同量的试液中,分别加入浓度依次递增的3种元素的标准溶液,用空气 乙炔火焰原子吸收法连续测定Co,Ni和Cu的含量。建立了优化的仪器测定条件,并对可能存在的元素进行了干扰试验。钴、镍、铜的回收率为98 3%～101 0%,相对标准偏差为0 76%～2 31%。