流动注射在线分离富集-火焰原子吸收光谱法测定水中镍(Ⅱ)

应用D412螯合树脂作为富集柱填充物,将在线分离富集装置与火焰原子吸收光谱法联用测定水中镍(Ⅱ)的含量。优化的试验条件如下:1富集柱采用干法填充;2吸附介质的p H为6;3进样速率为5 m L·min-1;4 3 mol·L-1硝酸溶液(洗脱剂)用量为2.5 m L;5洗脱速率为7.5 m L·min-1。镍的质量浓度在50μg·L-1以内与其吸光度呈线性关系,检出限(3s)为0.35μg·L-1。方法用于自来水和河水样品的分析,加标回收率在96.0%~101%之间,测定值的相对标准偏差(n=7)在2.5%~3.1%之间。     

SPE and determination by FAAS of heavy metals using a new synthesized polymer resin in various water and dried vegetables samples

Firstly, poly[phenyl thiadiazole methacrylamide-co-divinylbenzene-co-2-acrylamido-2-methylpropane sulfonic acid] (PTMAAm-co-DVB-co-AMPS), a new polymer resin was synthesized. This polymer resin was characterized by elemental analyzer, X-ray diffractometer, scanning electron microscope (SEM) and IR spectrometer. The glass column packed with the synthesized polymer resin was used for solid phase extraction (SPE). At the same time, the analytes were separated and preconcentrated from various water, dried vegetables samples and standard reference material (CRM) with SPE and determined by flame atomic absorption spectrometer (FAAS). The experimental conditions of this method such as pH, flow rates of sample, flow rates of eluent, type / concentration / volume of eluent, sample volume and matrix ions were examined. The limits of detection (µg L^?1) were calculated (3s) 0.9 for Mn(II), 1.4 for Cd(II), Co(II) and Zn(II), 1.5 for Cr(III), 2.2. for Cu(II), 1.9 for Pb(II),1.5 for Ni(II) and 1.9 for Fe(III) (n = 21). The low relative standard deviation, ≤ 2% (n = 11) and preconcentration factor as 75 for analytes were obtained.     

On-line preconcentration and determination of Au(III) in various environmental/industrial samples by flame atomic absorption spectrometry

A rapid and simple on-line method is described for the determination of Au(III) in various samples. The method is based on the sorption of gold(III) on Lewatit MonoPlus TP207 chelating resin including the iminodiacetate group, which is used as sorbent material and packed in a minicolumn. The chemical variables such as the pH of the sample solution, eluent type, interfering ions and concentrations of reagents, and instrumental variables such as sample loading volume, reagents flow rates, and tubing length, which affect the efficiency of the method were studied and optimised. Au(III) was sorbed on the chelating resin, from which it could be eluted with 3 mol L^?1 HCl, and then introduced directly to the nebuliser-burner system of FAAS. The limit of detection of the method was 0.2 µg L^?1 while the relative standard deviation was <4.0% for 20 µg L^?1 Au(III) concentration. The preconcentration factor was found to be 106 while the optimised sample volume was 15.3 mL. The accuracy of the method was verified by analysing the certified reference material. The developed method was applied successfully for the determination of gold in different samples with satisfactory results.     

A new procedure for determination of nickel in some fake jewelry and cosmetics samples after dispersive liquid–liquid microextraction by FAAS

A new, simple and cheap dispersive liquid–liquid microextraction (DLLME) procedure was optimized for the preconcentration of trace amounts of Ni(II) as a prior step to its determination by flame atomic absorption spectrometry (FAAS). It is based on the microextraction of nickel, where appropriate amounts of the extraction solvent (CHCl₃), disperser solvent (ethanol) and chelating agent, name 5‐[(Z)‐isoxazol‐3‐yl‐diazenyl]‐2‐methyl‐quinolin‐8‐ol (MMD), were firstly synthesized/characterized and used. Various parameters that affect the extraction procedure such as pH, centrifugation rate and time, the chelating agent (MMD) concentration and sampling volume on the recovery of Ni(II) were investigated. The preconcentration of a 20 ml sample solution was thus enhanced by a factor of 80. The resulting calibration graph was linear in the range of 0.24–10 mg L⁻¹ with a correlation coefficient of 0.9998. The limit of detection (3 s/b) obtained under optimal conditions was 1.00 μg L⁻¹. The relative standard deviation for certified reference material determinations was 1.2%. The accuracy of the method was verified by the determination of Ni(II) in the certified reference material of wastewater (Waste water CWW TMD). The proposed procedure was successfully applied to the determination of Ni(II) in some fake jewelry and cosmetics samples.     

Application of Ni(II)-imprinted cross-linked poly(methacrylic acid) synthesised through double-imprinting method for the on-line preconcentration of Ni(II) ions in aqueous media

The present paper describes the feasibility of on-line preconcentration of nickel ions from aqueous medium on Ni(II)-imprinted cross-linked poly(methacrylic acid) (IIP) synthesised through a double-imprinting method and their subsequent determination by FAAS. The proposed method consisted in loading the sample (20.0 mL, pH 7.25) through a mini-column packed with 50 mg of the IIP for 2 min. The elution step was performed with 1.0 mol L^?1 HNO₃ at a flow rate of 7.0 mL min^?1. The following parameters were obtained: quantification limit (QL) – 3.74 µg L^?1, preconcentration factor (PF) – 36, consumption index (CI) – 0.55 mL, concentration efficiency (CE) – 18 min^?1, and sample throughput – 25 h^?1. The precision of the procedure assessed in terms of repeatability for ten determinations was 5.6% and 2.5% for respective concentrations of 5.0 and 110.0 µg L^?1. Moreover, the analytical curve was obtained in the range of 5.0–180.0 µg L^?1 (r = 0.9973), and a 1.64-fold increase in the method sensitivity was observed when compared with the analytical curve constructed for the NIP (non-imprinted polymer), thus suggesting a synergistic effect of the Ni(II) ions and CTAB on the adsorption properties of the IIP. The practical application of the adsorbent was evaluated from an analysis of tap, mineral, lake and river water. Considering the results of addition and recovery experiments (90.2–100 %), the efficiency of this adsorbent can be ensured for the interference-free preconcentration of the Ni(II) ions.     

Determination of Hg(II) in Environmental Water Samples by Dispersive Liquid Phase Microextraction Combined with Flame Atomic Absorption Spectrometry

In this study, a method of dispersive liquid phase microextraction combined with the flame atomic absorption spectrometry was proposed for the determination of trace Hg using diphenylthiocarbazone as chelating reagent. Several factors which have effect on the microextraction efficiency of Hg, such as pH, extraction and dispersive solvent type and their volume, concentration of the chelating agent, extraction time were investigated, and the optimized experimental conditions were established. After extraction, the enrichment factor was 68. The detection limit of the method was 45 ng mL^?1, and the relative standard deviation for eight determinations of 2 μg mL^?1 Hg was 1.7%. The results for the determination of Hg in environmental water samples (tap water, well water, mineral water and Caspian sea water) have demonstrated the applicability of the proposed method.     

微波消解-FAAS测定皖南茶园土壤中矿质元素含量

采用微波消解-FAAS测定了皖南休宁县茶园不同深度土壤中的矿质元素Cu、Cd、Mn、Zn、Fe、Pb的含量,分析了不同深度土壤中矿质元素的分布特征,结果表明,皖南土壤中矿质元素Cu、Cd、Mn、Zn、Pb 5元素含量随土壤深度呈递减趋势,土壤表层的矿质元素(Cu、Cd、Mn、Zn、Pb)含量高于深层的,这与施肥有关,土...     

火焰原子吸收光谱法测定臭牡丹中6种金属元素

采用火焰原子吸收光谱法直接对臭牡丹中的Fe、Cu、Ca、Mn、Zn、Mg 6种金属元素进行了测定.样品采用浓硝酸双氧水消解,应用校准曲线法测定.结果表明其富含上述6种金属元素,其中以钙、镁含量为高,方法回收率在95.00%-103.67%之间.     

超声波提取-火焰原子吸收光谱法测定金银花中的Fe、Cu和Pb

建立了湿法和超声波提取处理样品,火焰原子吸收光谱法测定金银花湿法消解液及超声波提取液中Fe,Cu和Pb元素含量的方法.金银花中3种元素的含量Fe＞Cu＞Pb,硝酸作为提取剂,提取元素的溶出率的大小:Cu＞Pb＞Fe,回收率为85％-107％,RSD为0.6-1.0％.结果表明,超声波提取能较好地提取金银花中微量元素,元...     

FAAS测定酒当归中的微量元素

采用硝酸-高氯酸（4＋1）混合酸消解样品,用火焰原子吸收光谱法（FAAS）测定了酒当归中Fe、Cu、Mg、Ca、Mn、Zn、Ni、Cr、Pb 9种微量元素的含量。结果表明,9种元素的质量浓度在一定的范围内均与其峰面积呈线性关系。该法用于酒当归样品分析,9种元素测定值的相对标准偏差（n=6）均小于3%,标准加入法测得9种元素回收率在91.2%—109.7%之间。采用火焰原子吸收光谱法测定酒当归中9种微量元素稳定性好,结果准确可靠。