吡咯烷二硫代氨基甲酸铵及其氧化产物共沉淀分离富集氯化物中的痕量铅及原子吸收光谱测定

研究了吡咯烷二硫代氨基甲酸铵 (APDC)及其氧化产物 (DPTD)在pH 3.5条件下定量共沉淀氯化物中的痕量铅 ,用FAAS测定 ,检出限可达 1.2× 10 - 2 mg/L。标准加入的回收率在 97.2 %～ 10 6 .2 %之间 ,克服了基体干扰 ,取得了较为满意的结果。     

共沉淀分离富集原子吸收光谱法测定氯化物中痕量镉

研究了吡咯烷二硫代氨基甲酸铵 (APDC)及其氧化产物 (DPTD)体系在 pH3.5条件下定量共沉淀氯化物中痕量镉 ,用FAAS测定 ,检出限可达 1.3× 10 - 3mg·L- 1。加标回收率在 97%～ 10 3%之间 ,克服了基体干扰 ,取得了较满意的结果。     

Zn-DDTC共沉淀预富集火焰原子吸收光谱法测定水中微量镍

探讨了以Zn DDTC为共沉淀载体,共沉淀富集水中微量镍的方法,用火焰原子吸收光谱法测定镍,提高了灵敏度,选择性高,操作简便,方法检出限为3.78μg·L-1,相对标准偏差为3 92%～6.47%,回收率为95.8%～103.0%,用于测定自来水和其水源水中微量镍,结果满意。     

共沉淀富集—火焰原子吸收光谱法测定饮料中铅

饮料中铅含量测定,无法直接用火焰原子吸收光谱法测出其含量。因为饮料中铅含量低于仪器检出浓度,故必须预富集。氢氧化镁胶状沉淀能同时共沉淀一些重金属离子,在梨形分液漏斗内产生共沉淀,然后将沉淀从漏斗下部分离出来。以此达到富集目的。方法简便,富集效果好。经试验,方法相对标准偏差为6.47％,回收率在90.5％～112％,检出限为0.05mg·L~(-1)。     

铬(Ⅵ)-二乙基二硫代甲酸钠共沉淀-原子吸收光谱法测定环境水样中铁、锰、锌、镉

提出了以二乙基二硫代甲酸钠螯合铬(Ⅵ)作为载体共沉淀富集水体中铁、锰、锌和镉的方法。沉淀经离心分离,甲基异丁酮溶解后,以微量进样300μL火焰原子吸收光谱法测定铁、锰、锌,以石墨炉原子吸收光谱法测定镉。用水样10.0 mL,在pH 4.6的邻苯二甲酸氢钾缓冲介质中加入20 g.L-1重铬酸钾溶液150μL,20 g.L-1DDTC溶液1.0 mL可达到完全共沉淀分离,所得沉淀经离心分离后用甲基异丁酮2.0 mL溶解,并用于AAS分析。在优化的条件下,铁、锰、锌和镉的检出限(3σ)分别为9.0,6.8,1.8,0.03μg.L-1,相对标准偏差(n=6)在1.8%~3.8%之间。方法用于实际水样的测定,用标准加入法测得回收率在93.7%~105.0%之间。     

火焰原子吸收光谱法测定污泥中铜锌铅镉镍

污水处理厂污泥进行自然风干，筛分制备污泥样品，经烘干、硝酸－氢氟酸－高氯酸消解后，用火焰原子吸收光谱法测定污泥中铜、锌、铅、镉、镍含量。方法简便、快速、实用，具有较高的精密度和准确度。相对标准偏差为0．8％－6．0％，加标回收率为95％－103％。     

PVC-PP树脂分离富集/火焰原子吸收光谱法测定海水中痕量铜镍钴

采用自制的聚氯乙烯多乙烯多胺（PVC-PP）树脂,在pH值为5．0的条件下,分离富集海水中的痕量铜、镍、钴,以1．2mol／L盐酸溶液洗脱．火焰原子吸收光潜法测定,富集倍数最大可达100倍（回收率大于90％）。研究了吸附与洗脱的最佳条件,方法检出限分别为铜0．81μg/L、镍0．98μg/L、钴0．57μg/L（富集倍数100,S／N=3）,相对标准偏差小于5％（n=7）,样品加标回收率在90％-105％之间。     

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。     

萃取富集-火焰原子吸收光谱法测定水中镍

探讨了有机溶剂萃取和有机相经加热蒸发相结合在富集分离水中镍的应用,结合火焰原子吸收光谱法,提高了灵敏度,设备简单,操作简便,方法检出限为4.10μg·L-1。     

Ni(Ⅱ)-PAR共沉淀-原子吸收光谱法测定水样及奶茶粉中的锌

研究了用4-(2-吡啶偶氮)-间苯二酚(PAR)为沉淀剂,以Ni(Ⅱ)为载体离子的共沉淀体系快速共沉淀分离富集水样和奶茶粉中的锌,并用火焰原子吸收光谱(FAAS)测定。共沉淀过程受体系酸度、载体镍、沉淀剂PAR的用量及陈化时间的影响。结果显示,在pH 5.0的条件下,能够定量共沉淀试样中的锌。方法检出限为3.77μg/L,用于水样及奶茶粉的加标回收率为97.0%～99.1%,相对标准偏差为1.3%～4.1%。     

壳聚糖富集火焰原子吸收法测定水中痕量铜

采用壳聚糖修饰钨丝基质螺旋卷，直接浸入含有痕量铜的pH5．0的Brltton-Robinson缓冲溶液中，经电磁搅拌富集一定时间后，将其转移至空气／乙炔火焰燃烧器上，利用火焰原子吸收光谱法简便快速测定水中痕量铜。方法的线性范围为2—75μg／L；检出限为0．98μg／L。同一支钨丝螺旋卷重复涂敷壳聚糖富集Cu，RSD(n=6)为2．7％。     

Preconcentration,Determination and Speciation of Chromium(III) Using Solid Phase Extraction and Flame Atomic Absorption Spectrometry

A facile, reliable and reproducible method for speciation and determination of the traces amounts of chromium(III) in waste water has been developed. The method was based on complex formation on the surface of the ENVI‐18 DSK^? disks followed by stripping of the retained species by minimum amounts of appropriate organic solvents. The elution was 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 be about 1500 mL providing a preconcentration factor of 300. The maximum capacity of the disks was found to be 225 ± 3.9 μg for Cr³⁺. A limit of detection of 0.02 ng.mL ^?1 was obtained, and the method was applied for determination of chromium in electroplating industries waste water located in the eastern regions of Tehran.     

胞外高聚物分离富集-火焰原子吸收法测定水样中镍

以胞外高聚物PF-2作为镍的分离富集新材料,利用扫描电镜(SEM)、X射线能量色散分析仪(EDX)和傅里叶变换红外光谱(FTIR)对其进行表征.以火焰原子吸收法为检测手段,研究了胞外高聚物PF-2对水中Ni(Ⅱ)的吸附性能.结果表明:在pH 5.0,此吸附剂对水中的Ni(Ⅱ)具有很强的吸附能力.高聚物PF-2对Ni(Ⅱ...     

Determination of Silver with On-Line Preconcentration Using Dithiozone Chelate and Carbon Nanotubes for Preconcentration with Detection by Flame Atomic Absorption Spectrometry

A novel flow injection system incorporating a micro-column packed with carbon nanotubes (CNTs) as an adsorbent has been applied to the on-line preconcentration of trace silver with detection by flame atomic absorption spectrometry. Silver is first chelated by dithizone (H₂Dz), then retained on the CNTs surface and afterward quantitatively eluted by methanol. Influencing parameters, including the concentration of reaction reagent, enrichment variables, and elution variables were investigated. The adsorption mechanisms of Ag-H₂Dz chelate retained onto the CNTs surface have also been studied. By loading 6.9 mL sample solution, a linear calibration graph is obtained within the range of 3–120 µg L^?1 with R of 0.9996, and a detection limit (3σ) of 0.8 µg L^?1 is achieved, along with a precision of 1.6% R.S.D. at the 30 µg L^?1 level (n = 7). The dynamic sorption capacity of CNTs for silver is 122 mg g^?1. The procedure is demonstrated by measurement of spike recovery in a series of water samples, giving rise to spike recoveries in the range of 96.8–99.7%.     

火焰原子吸收法测定植物叶片中Pb、Cd、Cu、Zn含量

对八种植物叶片 (糖胶树、榕树、红花羊蹄甲、银合欢、垂叶榕、白玉兰、蟛蜞菊、大花紫薇 )中Pb、Cd、Cu、Zn的测定方法进行了研究 ,采用炭化—灰化—硝酸溶解方法进行样品处理 ,火焰原子吸收法测定Pb、Cd、Cu、Zn四种重金属元素。结果表明 ,该法准确 ,回收率高。各元素的回收率分别为 :铅 88%～ 1 0 5 %、镉 90 %～ 1 0 3 %、铜 90 %～ 1 0 5 %、锌 91 %～ 1 0 5 %。     

纳米硅羟基磷灰石分离富集-火焰原子吸收法测定水样中痕量铅

提出了纳米硅羟基磷灰石(Si-HAP)分离富集,火焰原子吸收光谱法(FAAS)测定水样中痕量铅的新方法。考察了铅在纳米Si-HAP上的吸附动力学、最佳酸度和吸附容量。实验结果表明:在最佳实验条件下,纳米Si-HAP能定量、快速地吸附水中的痕量Pb2+,其静态吸附容量24.33 mg/g;吸附在纳米Si-HAP上的Pb2+可用0.01mol/L EDTA-Ca完全洗脱。本法对Pb2+的检出限为1.33 ng/mL,相对标准偏差为4.0%(n=11,c=1μg/mL),加标回收率在94.9%~102.0%之间。方法用于实际水样中铅的测定,结果满意。     

流动注射-在线富集火焰原子吸收分光光度法测定痕量铅

本文报道在流动注射分析体系中用装有黄原脂棉的微型柱对溶液中Pb2 进行在线富集后,用3.0 mol/L盐酸洗脱柱上富集的Pb2 ,然后采用火焰原子吸收光谱法在线测定痕量Pb2 ,方法的线性范围为0.5～100μg/L。与未富集前相比,测定的灵敏度可提高65倍。方法用于环境水样中痕量Pb2 的测定,回收率在97.0%～102%之间,相对标准偏差小于4.0%,分析结果满意。     

活性炭微柱在线流动注射预富集-火焰原子吸收快速顺序测定铜、钴、镍、镉、铅的研究

采用双柱富集的流动注射在线预富集系统与220FS顺序多元素原子吸收分光光度计联用，使用圆锥型活性炭微柱为预富集柱，在pH4～5．5范围内，以吡咯啶二硫代氨基甲酸铵(APDC)为络合剂，6mol／L HNO3为洗脱剂，实现了Cu、Co、Ni、Cd、Pb5种元素的快速顺序测定。该体系对以上5种元素的富集倍数为9．8～15．5之间，34s富集的检出限(3σ)Cu为1．81，Co为3．10，Ni为1．66，Cd为0．28，Pb为4．90μg/L；相对标准偏差Cu 1．13％；Co1．24％；Ni2．26％；Cd0．95％；Pb1．77％。     

Determination of Silver by Flame Atomic Absorption Spectrometry after Preconcentration on Naphthalene Modified with Dithizone

A solid‐phase extraction method for preconcentration of silver and consequent determination by atomic absorption spectrometry is described. The method is based on the adsorption of silver on naphthalene modified with dithizone in a column. The adsorbed silver is eluted from the column with a thiourea solution and determined by flame atomic absorption spectrometry. The adsorption conditions including pH, reagent concentration, eluent volume, flow rate and interfering ions were investigated. The calibration graph was linear in the range 10–1000 ng mL^?1 of Ag in the initial solution with r = 0.9998. The limit of detection based on 3S_b was 3.9 ng mL^?1. The relative standard deviation for ten replicate measurements of 40 and 600 ng mL^?1 of Ag was 4.4% and 0.9%, respectively. The method was applied to the determination of silver in mineral, radiology film and wound dressing samples.     

螯合树脂在线富集火焰原子吸收法测定痕量铅和镉

在pH=4.88的乙酸-乙酸钠缓冲溶液中,用螯合离子交换树脂富集铅和镉,以1.50mol/L HNO3作洗脱液,火焰原子吸收法测定洗脱液中痕量铅和镉。该方法对铅和镉的线性范围分别是4.0～80.0μg/L和2.0～30.0μg/L,检出限分别为1.3μg/L和0.7μg/L。该方法用于地表水中痕量铅和镉的测定,分析结果满意。