Column Chromatographic Preconcentration of Copper in Alloys and Complex Materials Using 9,10 Phenanthrenequinone Monoxime Supported on Naphthalene

Abstract

A solid chelating compound phenanthrenequinone monoxime PQM) supported on naphthalene provides a rapid and economical means of preconcentration and separation of copper from the aqueous samples. Copper forms a complex with PC:: supported on naphthalene in the column at pH 6.1–8.4 with a flow rate of 1 ml/min. The metal complex and naphthalene are dissolved out from the column with 5 ml of DMF and the absorbance is measured at 470 nm against reacent blank. Beer's law is obeyed in the concentration range 0.6 9.6 μg of copper in 5 ml of DMF. The molar absorptivity and sensitivity are 6.3×10⁴ L mol^?1 cm^?1 and 0.001 μg cm^?2 respectively.     

Preconcentration and Determination of Trace Palladium with 1, 5-Diphenylcarbazone- Naphthalene as Adsorbent by Atomic Absorption Spectrometry

ABSTRACT|A highly selective, sensitive, rapid and simple atomic absorption spectrometric method has been developed for the determination of trace amounts of palladium in synthetic and real samples. Palladium can be adsorbed on naphthalene-1, 5-diphenyl-carbazone (DPCO) as adsorbent from the large volume of its aqueous solutions in the pH range 2.0 to 0. After filtration, the metal ion was desorbed with 5ml of 0.25M thiourea solution, and determined by AAS.

Alternatively, palladium can be adsorbed on this adsorbent packed in a column and determined similarly. The detection limit is 0.5 μg (signal to noise ratio=2) and the linearity is maintained in concentration range of 1.5-50μg of Pd with a correlation coefficient of 0.9992. Seven replicate determinations on samples containing 2.5 and 20μg of palladium gave the relative standard deviations of 3.6% and 0.81%, respectively. Various parameters such as effect of pH, volume of aqueous phase, shaking time and interference of number of ions on the determination of Pd have been studied in detail to optimize the conditions for its estimation in various synthetic and real samples.     

PVC-丁二酮肟复膜树脂分离富集原子吸收法测定地质样品中的钯

以包夹有丁二酮肟的PVC膜粘附在717强碱性阴离子交换树脂上为固定相,萃取色谱法分离富集矿样中的微量钯,以10％乙二胺-2％氢氧化钠溶液洗脱,用原子吸收光谱法测定。方法回收率在92．49,5～98．9％之间。     

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.     

微柱富集-原子吸收光谱法在线联用测定铅和钙

研究了“电化学前处理/微柱吸附顶浓缩/原子吸收在线检测”联用方法，利用自制的微型电化学富集柱对金属离子的吸附效应进行预富集，再瞬间解吸溶出直接进入原子吸收测定，极大的提高了测试灵敏度和降低了检出限，经对铅、钙离子的测定研究，可使特征浓度和检出限降低1-2个数量级以上，取得了令人满意的效果。     

盐酸苯海拉明的原子吸收法测定

探讨了盐酸苯海拉明在适当的酸性条件下与锌试剂、铜离子定量生成三元络合物,经ＭＩＢＫ萃取,以ＡＡＳ法测定萃取液听 铜来间接测定盐酸苯海拉明的量。本法与药典法相比,相对平均偏差小于０．４％,线性范围为５～５０μｇ．ｍＬ＾－１。回收率为９７％～１０２％。     

Atomic Absorption Spectrophotometric Investigation and Determination of Palladium

This work aims to achieve a determinate characterization of compound formation and to find out the resolution to overcome chemical interferences in atomic absorption spectrophotometric (AAS) determination of palladium. The effect of flame composition in producing a neutral palladium atoms was investigated. A new analytical procedure has been elaborated for the determination of palladium.     

Critical Study of the Determination of Palladium by Graphite Furnace- Atomic Absorption Spectrometry

Abstract

The atomic absorption spectroscopic behaviour of palladium in a graphite furnace has been investigated. The determination is several ordes of magnitude more sensitive than the flame technique. The use of Tantalum coated tubes does not improve considerably the sensitivity but prolongs the lifetime of the furnaces.     

流动注射在线萃取—石墨炉原子吸收光谱法测定地质样品痕量钯

应用流动注射在线萃取技术将ＰｄＣｌ＾２－６萃入２－巯基苯并噻唑－甲基异丁基酮直接进行石墨炉原子吸收测定。研究了流动注射在线萃取－石墨炉原子吸收光谱法测定地质样品中钯的实验条件、流路参数等。采样速率为２０样／ｈ,ＲＳＤ（ｎ＝１０）为４．８％,测定Ｐｄ的特征质量为２．６＊１０＾－１１。     

用X线荧光衍射法和原子吸收光谱法测定油漆中的铅含量

为勘查环境铅暴露的来源并评价其状况，应用K层X线荧光衍射法（XRF）对84张木制桌面表面油漆中的铅含量进行了测定。并应用原子吸收光谱法定量分析了8类18种液体油漆及12种内墙剥脱涂料中可溶性铅的含量。结果发现：所有桌面油漆的铅含量≤0．7mg／cm2，在正常范围内。但是，90年代以前生产的木质桌面表面油漆层中的铅含量明显高于90年代生产产品。液体油漆中铅含量为1．03×10－6～32800×10－6，其中超标者有3种，占16．7％，均为用于金属表面的防锈漆。内墙剥脱涂料中的铅含量为105×10－6～1430×10－6，均在正常范围内。结果提示：①应用便携式XFR检测桌面油漆中的铅含量，是一种快速、实用、准确的方法，非常有利于进行铅源的实地勘查；②除了少数几种工业用防锈漆以外，民用油漆，包括内墙涂料、家具、地板及桌面上用的油漆中的铅含量均未超标。但由于本调查未涉及80年代及更早时期的木质家具，老建筑中使用的油漆的铅污染情况如何，还有待进一步地勘查和研究。     

间接原子吸收光谱法测定药物制剂中的西米替丁

本文提出了流动注射原子吸收光谱法间接测定西米替丁的新方法。基于西米替丁与Ag（I）反应可以生成白色的沉淀,经流动注射在线过滤稀释,以原子吸收光谱法测定反应剩余银离子的量来间接测定西米替丁的量。在优化条件下西米替丁浓度在2～80mg／L范围内与吸光度呈良好的线性关系,回收率为97．0％～104．3％。方法用于片剂西米替丁的测定,结果满意。     

Sequential Injection On-Line Sorption Preconcentration Using PEEK-Turnings Packed Micro-Column for Ultra-Trace Cobalt Determination by Electrothermal Atomic Absorption Spectrometry

A novel sequential injection on-line column preconcentration method for ultra-trace cobalt determination by electrothermal atomic absorption spectrometry (ETAAS) using poly(etheretherketone) (PEEK) turnings as sorbent material was developed. The method was based on the on-line chelate complex formation and retention of target analyte with ammonium pyrrolidine dithiocarbamate (APDC) on the surface of PEEK-turnings and elution with methyl isobutyl ketone (MIBK). A 40 µL fraction of MIBK containing the bulk of analyte complex introduced directly into the transversely heated graphite tube atomizer of ETAAS for quantification. Acidity of sample solution, chelating reagent concentration, and preconcentration time were investigated and optimized separately, while all other factors were optimized by full factorial design optimization methodology. The significance of the variables and their interactions was estimated by employing analysis of variance (ANOVA) and Pareto chart. Under the optimum conditions the enhancement factor for cobalt determination was 60. The detection limit was 6 ng L^?1 and the precision expressed as relative standard deviation (RSD) was 3.5% at 0.1 µg L^?1 Co(II) concentration level, respectively. The proposed method was evaluated by analyzing water certified reference materials and spiked environmental samples.     

间接原子吸收法测定药物制剂中利血生的含量

提出了利血生的间接原子吸收法，该法基于利血生在碱性介质中的分离－产物半胱氨酸在适当的PH条件下与铜离子生成灰色沉淀，通过测定上清液中铜的含量来间接测定利血生的含量，在法在10－100mg/L范围内呈良好的线性关系（r=0.9992),回收率为98．5％－101．6％。该法可成功地用于药物制剂中利血生的测定。     

纳米氧化铝负载双硫腙分离富集-原子吸收法测定地质样品中的金、铂、钯的研究

金、铂、钯在地质样品中的含量甚微,国内外常采用ICP-AES,ICP-MS和ETAAS直接测定。FAAS法由于仪器便宜、操作方便,也广泛应用于预富集后的痕量贵金属的分析。目前,在测定贵金属的分析方法中,常采用固相萃取法富集分离样品,主要的固相萃取剂有:无机吸附剂,交联树脂[1],螯合树脂[     

Determination of Palladium by Graphite Furnace Atomic Absorption Spectrometry After Preconcentration with MCI GEL CHP 20P Resin as Sorbent

A solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of palladium with MCI GEL CHP 20P resin as sorbent was studied. Trace amounts of palladium was reacted with 2-ethylhexyl octyl sulfide followed by adsorption onto MCI GEL CHP 20P solid phase extraction column, and ethanol was used as eluent. The enrichment factor of this method for palladium was reached at 250. The detection limit in the original sample for palladium was found to be 0.0048 ng mL^?1. The proposed method has been successfully applied to the determination of trace amounts of palladium in different samples.     

Atomic Absorption Spectrometry Analysis of Silicates by the Absorption Tube Technique

Abstract

By the combined use of the absorption tube technique and solvent extraction, determination of cadmium, cobalt, copper, iron, lead and nickel in silicate rocks was investigated.

Applicable concentration range was from 0.1 to 1.Oppm for all the elements except cadmium, for which the range was from 0.005 to 0.025ppm. The accuracy and recovery determined by the use of standard samples from the United States National Bureau of Standards and Geological Survey were satisfactory for practical purposes.     

氢化物负压发生和真空无火焰原子化器的原子吸收光谱法测定铋

在负压发生器中用1% NaBH_4将Bi(Ⅲ)还原为铋化氢后,向发生器中加入一定量的空气。用真空泵将铋化氢和空气的混合物同时吸入到真空电热石英管中,用原子吸收仪器测定。在原子化器内,加入空气中的氧与硼氢化钠分解产生的氢反应,生成水分子。因而消除了氢对测定铋的干扰。     

Determination of Urinary Lead Levels in Normal Population by Graphite-Furnace Atomic Absorption Spectrophotometry Using Palladium Chloride as the Matrix Modifier

ABSTRACT|A direct method with graphite furnace atomic absorption spectrophotometry for determining low lead (Pb) levels in urine was described. The present method was based on wet-ashing digestion, 2-fold concentrated urine, and matrix modification with palladium chloride (PdCl²). The sensitivity (concentration at 0.0044 absorption units) of the proposed method is 0.18 ppb. Results were presented on the degree of accuracy and precision. Accuracy of the proposed method was checked by comparison with the values determined by the extracted method (conventional method). Precision of the proposed method was evaluated by within-run and between-run precision. Both of them were found to be satisfactory. Due to the high sensitivity, the proposed method could be applied to determine urinary Pb concentration in normal populations with no known Pb exposure.

Moreover, the method is simple, fast, and automatic.     

巯基壳聚糖富集火焰原子吸收光谱法测定天然水体中Pb2+和Cd2+ 的研究

利用自己研制的巯基壳聚糖对Pb^2 和Cd^2 具有良好的吸附效果这一特性，建立了巯基壳聚糖分离富集原子吸收光谱法测定天然水体中Pb^2 和Cd^2 的新方法，研究了最佳吸附和脱附条件，该法对Pb^2 和Cd^2 的准确检测下限可达到1.00μg/L和0.050μg/L。回收率分别达到96.5%和97.6%。该法灵敏度高，选择性好，用于实际水样的测定取得了满意的。