ICP-MS法与石墨炉原子吸收法测定矿山废水中铊含量的比较

通过对比测定矿山废水中铊含量的ICP-MS法与石墨炉原子吸收法,为选矿废水中铊的测定提供可靠的方法,在确定ICP-MS法与石墨炉原子吸收法工作曲线的基础上,对矿山选矿废水中铊进行测定并确定最佳测定方法,检测结果中石墨炉原子吸收法的测定结果 1.57μg/L,加标回收率为94%~108%;ICP-MS法的测定结果为1.92μg/L,加标回收率为86%~98%;结果表明,对于复杂水体中铊的测定,石墨炉原子吸收法具有较高的抗干扰能力、重现性、准确度和精密度,即矿山选矿废水中铊的含量检测石墨炉原子吸收法优于ICP-MS方法。     

原子吸收分光光度计测定地表水铝含量浅析

对地表水中铝含量的测定采用原子吸收法的两种方公式（即石墨炉原子吸收法和火焰原子吸收法）分别进行了试验,其中石墨炉原子吸收法测定中采用石墨管涂锆,基体改进剂为硝酸镁,准确度符合要求。火焰原子吸收法测定中采用空气-乙炔间接火焰原子吸收法,在调整了PAN用量下,标准曲线的相关系数r达到了0.9996,取得了良好的效果。     

碘化钾络合MIBK萃取富集石墨炉原子吸收法测定水中的铅

本文研究了石墨炉原子吸收测定水中铅的方法。用硝酸和高氯酸溶解水中的铅,经碘化钾和MIBK络合萃取富集,用原子吸收石墨炉法测定。该方法相对标准偏差(RSD)为3.77%,检测限(DL)为0.6μg/L-1,方法回收率在92.5%-107.3%,结果令人满意。     

石墨炉原子吸收法测定废水中铅的不确定度分析

对石墨炉原子吸收法测定废水中铅的不确定度进行评定,系统分析不确定度的来源,计算出该方法的不确定度,为评价方法的可靠性和分析的准确性提供参考。     

原子吸收光度法测定空气中的镉、镍

试验中用王水消解样品,分别采用火焰原子吸收光度法测定空气污染固定源中镉、镍;石墨炉原子吸收光度法测定散源中镉、镍。方法的精密度及准确度都较好。     

石墨炉原子吸收分析中的基体改进技术及其应用研究

石墨炉原子吸收法灵敏度高、吸收效果好、测定速度快,因此在工业、农业、生物、食品等领域应用广泛。但是由于石墨炉原子吸收分析过程中,会有其他因素的干扰,对分析结果有一定的影响。所以还需要对石墨原子吸收分析中的基体改进技术进行探讨。本文主要阐述了基体改进剂的类型、基体改进及降低干扰的途径,以及在基体改进技术的应用。     

石墨炉原子吸收法与ICPMS法测定皮革中镉的比较

石墨炉原子吸收法和电感耦合等离子体质谱法（ICPMS）是测定皮革中镉元素的主要方法。本文针对这两种测定方法进行了分析,并将两种方法所测结果进行了比较,探讨了用电感耦合等离子体质谱法测定时如何选择内标元素的,阐述了在内标元素选择正确的情况下,电感耦合等离子体质谱法与石墨炉原子吸收法测定结果保持一致。     

吸收型冷原子测汞仪检出限检定的问题讨论及建议

本文介绍了根据JJG 548-2004《测汞仪》检定规程对吸收型冷原子测汞仪检测限检定中遇到的问题和解决方案。建议用JJG 694-2009《原子吸收分光光度计》检定规程中对石墨炉原子化法原子吸收分光光度计检出限计算方法计算吸收型冷原子测汞仪检测限。     

石墨炉原子吸收法测定水中铅的能力验证实验

采用石墨炉原子吸收法测定水之中的Pb,确定了测定的线性范围及检出限。对同一厂家或不同厂家的标准物质的不同浓度基准溶液进行Pb内控样比对,并与原子吸收火焰法的方法比对,确定石墨炉法测定Pb的结果可靠。     

石墨炉原子吸收在土壤微量元素测试中的应用

本文阐述了用石墨炉原子吸收分光光度法测定土壤中铅、镉,改进了样品的处理方法,分析过程中的灯电流、灰化温度、原子化温度等因素对灵敏度的影响,确定了石墨炉的最佳条件,取得了可靠结果。     

Speciation of chromium in water samples with cloud point extraction separation and preconcentration and determination by graphite furnace atomic absorption spectrometry

A novel method has been developed for the speciation of chromium in natural water samples based on cloud point extraction (CPE) separation and preconcentration, and determination by graphite furnace atomic absorption spectrometry (GFAAS). In this method, Cr(III) reacts with 1-phenyl-3-methyl-4-benzoylpyrazol-5-one (PMBP) yielding a hydrophobic complex, which then is entrapped in the surfactant-rich phase, whereas Cr(VI) remained in aqueous phase. Thus, separation of Cr(III) and Cr(VI) could be realized. Total chromium was determined after the reduction of Cr(VI) to Cr(III) by using ascorbic acid as reducing reagent. PMBP was used not only as chelating reagent in CPE procedure, but also as chemical modifier in GFAAS determination of chromium. The detection limit for Cr(III) was 21 ng L(-1) with an enrichment factor of 42, and the relative standard deviation was 3.5% (n=7, c=10 ng mL(-1)). The proposed method has been applied to the speciation of chromium in natural water samples with satisfactory results.     

Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni2+ with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni2+ with 10 mL solution. Under the optimal conditions, the detection limit of Ni2+ is 0.12 ng mL(-1) with R.S.D. of 4.3% (n = 10, c = 100 ng mL(-1)). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.     

Determination of trace aluminum in biological and water samples by cloud point extraction preconcentration and graphite furnace atomic absorption spectrometry detection

A cloud point extraction (CPE) method for the preconcentration of trace aluminum prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) has been developed. The CPE method is based on the complex of Al(III) with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP), and then entrapped in non-ionic surfactant Triton X-114. PMBP was used not only as chelating reagent in CPE preconcentration, but also as chemical modifier in GFAAS determination. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PMBP and Triton X-114, equilibration temperature and time, were investigated in detail. An enrichment factor of 37 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of this method for Al(III) is 0.09 ng mL(-1), and the relative standard deviation is 4.7% at 10 ng mL(-1) Al(III) level (n=7). The proposed method has been applied for determination of trace amount of aluminum in biological and water samples with satisfactory results.     

Characterization of arsenic (V) and arsenic (III) in water samples using ammonium molybdate and estimation by graphite furnace atomic absorption spectroscopy

Arsenic (V) is known to form heteropolyacid with ammonium molybdate in acidic aqueous solutions, which can be quantitatively extracted into certain organic solvents. In the present work, 12-molybdoarsenic acid extracted in butan-1-ol is used for quantification of As (V). Total arsenic is estimated by converting arsenic (III) to arsenic (V) by digesting samples with concentrated nitric acid before extraction. Concentration of As (III) in the sample solutions could be calculated by the difference in total arsenic and arsenic (V). The characterization of arsenic was carried out by GFAAS using Pd as modifier. Optimization of the experimental conditions and instrumental parameters was investigated in detail. Recoveries of (90-110%) were obtained in the spiked samples. The detection limit was 0.2 microg l(-1). The proposed method was successfully applied for the determination of trace amount of arsenic (III) and arsenic (V) in process water samples.     

Determination of trace lead in water samples by continuous flow microextraction combined with graphite furnace atomic absorption spectrometry

A new method of continuous flow microextraction (CFME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of trace lead in water samples. A drop of 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) dissolved in benzene is injected into a glass chamber by a microsyringe and held at the outlet tip of a PTFE connecting tube, the sample solution flows right through the tube and the glass chamber, the solvent drop interacts continuously with the sample solution, and the analyte was extracted into the drop and concentrated. After extracting for a period of time, the drop was retracted into the microsyringe and directly injected into graphite furnace for determination of Pb. Several factors affecting the extraction efficiency, such as solution pH, sample flow rate, drop volume and extraction time, were optimized. Under the optimized conditions, a concentration factor of 45 was achieved, and the detection limits for Pb were 12 pg mL(-1). The relative standard deviation for six replicate analyses of 10 ng mL(-1) Pb was 6.8%. The proposed method was applied to determine of trace Pb in water samples with satisfactory results.     

柠檬酸-硝酸作基体改进剂石墨炉原子吸收法测定水中的铯

本文提出了以柠檬酸—硝酸作为基体改进剂,石墨炉原于吸收法测定水中的铯,系统地研究了 Cs 的实验条件,重点探讨了基体改进剂的选择及干扰的消除。该法特征量为22pg,检出限(3S)为0.93ng/mL,方法简便、快速、准确。本法应用于实际样品的分析,获得满意的结果,可满足水质分析的要求。     

原子吸收石墨炉法快速测定饮用水中钛

本文针对用化学方法测定水中钛的不足,提出用原子吸收石墨炉法塞曼背景校正进行测定,并进行相应的条件试验。试验结果表明:在控制一定的条件下即可快速、方便、准确地测定钛的含量,而且检出限和精密度都令人满意。     

分散液液微萃取浮动溶剂固化——原子吸收光谱法测定环境水体样品中的重金属

采用了十一醇为萃取剂,吡咯烷二硫代甲酸铵(APDC)为络合剂的分散液液微萃取浮动溶剂固化-石墨炉原子吸收光谱法(DLLME-SFO-GFAAS)测定水体样品中痕量金属离子的分析方法,对实验条件进行了优化,改进了传统萃取方法中试剂用量大、手续繁琐、易交叉感染等不足。同时对方法测量检出限及回收率进行试验,结果表明在优化的实验条件下铜、镉、铅的检出限分别0.03μg/L、0.03μg/L和0.01μg/L,加标回收率在95.3%--102.4%,方法准确、可靠。     

Determination of trace lead in water samples by graphite furnace atomic absorption spectrometry after preconcentration with nanometer titanium dioxide immobilized on silica gel

Nanometer titanium dioxide immobilized on silica gel (immobilized nanometer TiO2) was prepared by sol-gel method and characterized using X-ray diffraction (XRD) and scanning electron microscope (SEM). The adsorptive capability of immobilized nanometer TiO2 for lead was assessed in this work using column method. It was found that lead can be quantitatively retained by immobilized nanometer TiO2 in the pH range 4-7, then eluted completely with 1.0molL(-1) HCl. The adsorption capacity of immobilized nanometer TiO2 for Pb was found to be 3.16mgg(-1). A new method has been developed for the determination of trace lead based on preconcentration with a microcolumn packed with immobilized nanometer TiO2 prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS). The detection limit of this method for Pb was 9.5ngL(-1) with an enrichment factor of 50, and the relative standard deviations (R.S.D.s) was 3.2% at the 10ngmL(-1) Pb level. The method was validated using a certified reference material, and was applied for the determination of trace lead in water samples.