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.     

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.     

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.     

火焰原子吸收分光光度法测定水泥中的铁和锰的研究

对火焰原子吸收分光光度法定水泥中的铁和锰的方法进行了研究.结果表明,在选定的最佳仪器条件下,测定水泥中铁和锰的RSD分别为0.45％和2.68％,回收率分别为97.0％～99.0％和98.0％～102.0％,该法操作简单、测试快速、结果准确稳定.     

火焰原子吸收光谱法测定铸铝合金中的铜

建立了火焰原子吸收光谱法测定铸铝合金中的铜含量,并研究了酸度、干扰元素、干扰抑制剂的加入量对测定结果的影响.通过大量实验的反复验证,确定了测定铸铝合金中铜元素含量的最佳工作条件,并在最佳工作条件下测定标准试样,测定结果的相对标准偏差小于5％,回收率为99.2％～102.2％,从而证明了方法的可行性.该方法测定铜含量的范...     

长链脂肪酸及溶剂对浮选富集锶的效果影响

试验了4种有机溶剂(苯、氯仿、正丁醇和甲基异丁基酮)和作为捕集剂的4种长链脂肪酸(十二烷基磺酸钠、十四酸、十六酸和十八酸)对浮选法富集锶效率的影响。试验中,于含锶(Ⅱ)的溶液(约10mL)中加入2g·L~(-1)脂肪酸的乙醇溶液(4种脂肪酸中的任一种),将溶液的酸度调至pH 8,并移入自制浮选柱中,加入任一有机溶剂10mL,通入流量为8～12L·min~(-1)的空气浮选5min,按预选的仪器工作条件用火焰原子吸收光谱法测定有机相中锶的含量。根据所测得结果,选择十八酸作为捕集剂和甲基异丁基酮作为有机溶剂进行浮选富集效果最好,回收率在90%以上。     

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。     

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...     

火焰原子吸收光谱法测定鸭粪中铜和锌的含量

采用火焰原子吸收光谱法测定白洋淀生态养鸭场中饲料及鸭粪中的铜和锌含量,测定结果为饲料中的铜含量范围在9.7-61.55mg/kg,锌含量范围在63.14-149.07mg/kg,在禽类饲料中铜、锌含量属于较低的类型;鸭粪中铜含量范围在13.71-94.74mg/kg,锌含量范围在156.98-346.31mg/kg,参...