共查询到20条相似文献,搜索用时 31 毫秒
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Domínguez-González R Moreda-Piñeiro A Bermejo-Barrera A Bermejo-Barrera P 《Talanta》2005,66(4):937-942
A new method using diluted reagents (nitric and hydrochloric acids and oxygen peroxide) and ultrasound energy to assist metals acid leaching with from edible seaweed was optimized. The method uses a first sonication at high temperature with hydrochloric acid as a previous stage to an ultrasound-assisted acid leaching with 7 ml of an acid solution containing nitric acid, hydrochloric acid and hydrogen peroxide at concentrations of 3.7, 3.0 and 3.0 M, respectively. Optimum conditions for the first sonication step were ultrasound energy at 17 kHz, sonication temperature at 65 °C, an acid volume of 2 ml, an hydrochloric acid concentration of 6.0 M and a sonication time of 10 min. It has been found that the first sonication stage at high temperature with hydrochloric acid is necessary to obtain quantitative recoveries for As, Ba, Fe and V. Otherwise quantitative recoveries were reached for the other elements investigated (Ca, K, Na, Mg, Cd, Cr, Cu, Mn, Ni, Pb and Zn). The repeatability of the ultrasound-assisted acid leaching method was around 10% for all elements. Adequate limit of detection and limit of quantification were reached by using inductively coupled plasma-optical emission spectrometry (ICP-OES) for measurements. The method resulted accurate after analysing several seaweed certified reference materials (IAEA-140/TM, NIES-03 and NIES-09). The method was finally applied to the multi-element determination in edible seaweed samples. 相似文献
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铜精矿试样利用HCl和HNO3混酸于微波消解仪中进行溶解,电感耦合等离子体发射光谱(ICP-OES)法测定铜精矿中的银含量。试验了不同比例消解体系的消解效果,研究了不同浓度铁、铜基体的影响,结果表明王水体系消解效果最佳,1 000mg/L以下的铁、铜或铁、铜的混合基体对银的测定没有影响,10%HCl体系作为测定酸度。该方法对银的线性范围为0.73~1 500g/t,标准物质测定值与标准值无显著性差异。该方法前处理试剂消耗少、速度快,分析浓度范围宽,可用于铜精矿中银的快速测定。 相似文献
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Afshin Rajabi Khorrami Tahereh Hashempur Ali Mahmoudi Ali Reza Karimi 《Microchemical Journal》2006,84(1-2):75-79
A highly sensitive and accurate method for preconcentration and determination of ultra trace amounts of cobalt and nickel ions in water samples is proposed. The preconcentration is achieved using C18-silica extraction disks modified with 5-(6-methoxy-2-benzothiazoleazo)-8-aminoquinoline (MBTAQ). The retained ions on the prepared solid phase was eluted with 10 ml of 0.01 M nitric acid and measured by inductively coupled plasma-optical emission spectrometry (ICP-OES). The influence of the type and amount of eluent used, pH, sample and eluent flow rates, amount of MBTAQ and the effect of other ions on extraction efficiency were investigated. The limits of detection of the method were 0.08 and 0.06 μg l− 1 for cobalt and nickel, respectively, and provide an enrichment factor of 100. The results obtained on 10 successive extractions and elution cycles revealed relative standard deviations of 1.5 and 1.0% for cobalt and nickel, respectively. The proposed method has been applied to the determination of ultra trace amounts of cobalt and nickel ions in natural and synthetic water samples with satisfactory results. 相似文献
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浊点萃取-流动注射电感耦合等离子体原子发射光谱法同时测定水中镉钴铜镍锌 总被引:3,自引:1,他引:2
本文提出了浊点萃取-流动注射电感耦合等离子体原子发射光谱(FI—ICP—AES)法同时测定水中镉、钴、铜、镍、锌的新方法。利用5-Br—PADAP将待测金属离子转化为水不溶性的螯合物,并萃取到表面活性剂Triton X-114的浓缩相,以乙醇-硝酸溶液稀释含富集离子的浓缩相,并以FI—ICP-AES法测定。考察了流动注射进样体积、积分时间、萃取体系介质酸度、螯合剂和表面活性剂用量等实验条件的影响。在折衷条件下,镉、钴、铜、镍和锌的浓缩倍率可达18、10、16、10和8,检出限分别为0.7μg/L、1.6μg/L、1.3μg/L、5.7μg/L、3.2μg/L。方法成功应用于自来水、河水和海水中痕量镉、钴、铜、镍和锌的分析。在0.02mg/L和0.10mg/L二个水平进行加入回收试验,回收率在80%与118%之间。 相似文献
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In this study, dispersive liquid-liquid microextraction (DLLME) combined with inductively coupled plasma optical emission spectrometry (ICP-OES) was developed for simultaneous preconcentration and trace determination of chromium, copper, nickel and zinc in water samples. Sodium diethyldithiocarbamate (Na-DDTC), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. The effective parameters of DLLME such as volume of extraction and disperser solvents, pH, concentration of salt and concentration of the chelating agent were studied by a (2f−1) fractional factorial design to identify the most important parameters and their interactions. The results showed that concentration of salt and volume of disperser solvent had no effect on the extraction efficiency. In the next step, central composite design was used to obtain optimum levels of effective parameters. The optimal conditions were: volume of extraction solvent, 113 μL; concentration of the chelating agent, 540 mg L−1; and pH, 6.70. The linear dynamic range for Cu, Ni and Zn was 1-1000 μg L−1 and for Cr was 1-750 μg L−1. The correlation coefficient (R2) was higher than 0.993. The limits of detection were 0.23-0.55 μg L−1. The relative standard deviations (RSDs, C = 200 μg L−1, n = 7) were in the range of 2.1-3.8%. The method was successfully applied to determination of Cr, Cu, Ni and Zn in the real water samples and satisfactory relative recoveries (90-99%) were achieved. 相似文献
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以氢氟酸、硝酸消解样品,然后加入硫酸络合钛避免其在低酸度介质中水解,并且加热至产生三氧化硫烟以驱赶氢氟酸,以水稀释定容后采用电感耦合等离子体原子发射光谱法(ICP-OES)直接测定含钒尾渣中钒的含量。试验考察了在共存含有铁、钛、铝、铬、锰、钒等元素的含钒尾渣复杂基体中,基体效应、光谱干扰以及背景噪音等影响因素对钒测定的干扰,方法通过优选元素分析谱线、背景校正区域以及光谱仪工作条件,并且采用基体匹配法和同步背景校正法相结合方式,消除了构成复杂且变化无常的样品基体对测定的影响。结果表明:方法可用于测定0.01~6.0%范围的钒,并且样品基体在铁20~40%、钛5~30%、铝铬锰钠硅钙镁各1~10%的范围变化对测定无影响;检测下限可达0.0009%; 精密度:RSD<3%;回收率94%~106%;方法与高锰酸钾氧化-硫酸亚铁铵滴定化学分析法的测定结果对照一致。 相似文献
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Summer N. Hanna Clifton P. Calloway Jr. Jason D. Sanders Ronald A. Neslon Jamaal Cox Bradley T. Jones 《Microchemical Journal》2011,99(2):165-169
A new compact, aluminum electrothermal vaporization cell was constructed for inductively coupled plasma-optical emission spectrometry analysis. This cell is compact enough to fit within the space occupied by the spray chamber and fits directly to the quartz torch without extraneous tubing through the use of a simple Compression fitting. Sample volumes as low as 10 μL were analyzed with an automated control program for efficient vaporization. Twelve elements were analyzed utilizing a time resolved acquisition method so that real-time data could be generated over a period of 10 s with an average improvement factor of 14 for elements over a wavelength range of 193–445 nm. 相似文献
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C. Bosch Ojeda 《Talanta》2007,71(1):1-12
Rh is contained in catalyst in much smaller quantities than Pt. For this reason, the database for this metal with respect to emissions from catalytic converters is much smaller than that for platinum, thus precluding a quantitative risk assessment.Accurate determinations of the rhodium have always been difficult tasks. The metal is often present at trace levels in sample types of complex composition. This situation has improved recently due to developments of instrumental methods and their applications to analyses of rhodium in a variety of matrices. The purpose of this review is to describe the analytical sensitive methods by inductively coupled plasma spectrometry. 相似文献
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罗海霞 《中国无机分析化学》2019,9(1):8-10
用HCl-HNO3混和酸溶解金精矿样品,用电感耦合等离子体发射光谱法(ICP-OES)测定。在选定的操作条件下,砷的检出限0.018μg/mL。相对标准偏差( n=11),RSD<2%,加标回收率在98.2%-103.0%之间。用该法测定金精矿中砷元素的含量,操作简单易行,能够满足日常生产需要。 相似文献
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应用电感耦合等离子体原子发射光谱(ICP-AES)法对球化剂中镧、铈、钇进行测定,通过硝酸、氢氟酸和盐酸分解试料,高氯酸冒烟驱走硅和氟,最后用盐酸溶解盐类,能准确、快速地测定其含量,加标回收率在97%~100%,精密度实验取得了满意的结果。 相似文献
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A new method for solid-phase extraction and preconcentration of trace amounts Hg(II) from environmental samples was developed by using sodium dodecyle sulphate-coated magnetite nanoparticles (SDS-coated Fe3O4 NPs) as a new extractant. The procedure is based on the adsorption of the analyte, as mercury-Michler's thioketone [Hg2(TMK)4]2+ complex on the negatively charged surface of the SDS-coated Fe3O4 NPs and then elution of the preconcentrated mercury from the surface of the SDS-coated Fe3O4 NPs prior to its determination by flow injection inductively coupled plasma-optical emission spectrometry. The effects of pH, TMK concentration, SDS and Fe3O4 NPs amounts, eluent type, sample volume and interfering ions on the recovery of the analyte were investigated. Under optimized conditions, the calibration curve was linear in the range of 0.2-100 ng mL−1 with r2 = 0.9994 (n = 8). The limit of detection for Hg(II) determination was 0.04 ng mL−1. Also, relative standard deviation (R.S.D.) for the determination of 2 and 50 ng mL−1 of Hg(II) was 5.2 and 4.7% (n = 6), respectively. Due to the quantitative extraction of Hg(II) from 1000 mL of the sample solution an enhancement factor as large as 1230-fold can be obtained. The proposed method has been validated using a certified reference materials, and also the method has been applied successfully for the determination of Hg(II) in aqueous samples. 相似文献
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Eva María Seco-Gesto 《Talanta》2007,72(3):1178-1185
Studies on the application of a short microwave irradiation cycle and the use of diluted acids to extract trace elements from raft mussel samples were developed. Multi-element determinations (Al, Ba, Cd, Cr, Cu, Fe, Mn, Pb, Sn, V and Zn) were carried out by inductively coupled plasma-optical emission spectrometry (ICP-OES). Parameters such as acid/oxidizing reagents (diluted nitric acid, hydrochloric acid and hydrogen peroxide) concentrations, acid/oxidizing solution volume, temperature, ramp time and hold time for the microwave heating were simultaneously studied by using an experimental design approach. The optimum conditions have showed the sample pre-treatment of 10 mussel samples to less than 3.0 min when a microwave power of 600 W and a controlled temperature of 65 °C were used. This time (hold time plus ramp time) is quite shorter than those reported for conventional microwave-assisted acid digestion procedures. Since temperature inside the reactor is not high, the venting time can be shorted to 15 min. In addition, the concentration of acid/oxidizing reagents needed to complete the acid leaching (2.5 M, 3.0 M and 0.5 % (m/v) for nitric acid, hydrochloric acid and hydrogen peroxide, respectively) is lower than the required concentration for a conventional microwave-assisted acid digestion (concentrated acids). The proposed method has showed a good repeatability of the overall method, and relative standard deviations between 11 and 2% were reached for 12 replicate microwave-assisted acid leaching and ICP-OES measurements. The method was finally validated by analyzing TORT-1 and GBW-08571 certified reference materials and it was successfully applied to fast multi-element determinations in several raft mussel samples. 相似文献
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Maria Cruz Zuluaga Ainhoa Alonso-Olazabal Xabier Murelaga Luis Angel Ortega 《Microchemical Journal》2011,99(2):443-448
Pottery tempered with former pottery fragments (named grogs) is very common during the Bronze Age in the Cantabrian Cornice (North Spain). Grog tempered pottery from two coeval archaeological sites Santa Maria de Estarrona and Peracho are studied in order to establishes pottery provenance. Chemical analyses of pottery are used to discriminate locally from imported pottery under the assumption that different geological regions exhibit a distinctive chemical fingerprint. However, the pottery-maker usually transforms the original clay by tempering and prepares the material suitable for firing modifying the raw material chemical fingerprint. The problem increases when grogs are used as tempering agent. In these cases the chemical input is clearly contaminated with foreign materials making impossible to assign a source area. SEM-EDX has been applied to both the matrix and the different types of grog tempers and the results have been compared to the whole potsherd analysis performed by ICP-OES. Chemometric analysis of matrices enable to discriminate different raw materials that can be attributed to locally produced pottery. This chemical characterization of the matrices by SEM-EDX is more effective than the chemical composition determined for the whole potsherd by ICP-OES. The occurrence of grogs within grog tempers and various types of grogs indicates modes of production based on intensive recycling. The presence of some pottery vessels at the Estarrona site with chemical features similar to those of Peracho is indicative of the transport of pieces during the migrations of semi-sedentary groups and/or the exchange of pieces between different groups of humans. 相似文献
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《Analytical letters》2012,45(9):1623-1632
Abstract A new procedure based on closed vessel Microwave-Induced Combustion (MIC) technique is proposed for the decomposition of petroleum coke and further determination of sulfur by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). The procedure is based on sample ignition by microwave radiation using closed quartz vessels pressurized with oxygen and use of NH4NO3 as an ignition aid. The nature and concentration of absorbing/refluxing solution were studied, as well as the operational parameters related to MIC technique. Results were compared with those obtained by conventional wet digestion in closed vessels, certified reference materials (agreement was better than 98%), and also using ion chromatography for S determination. 相似文献