Use of packed-fiber solid-phase extraction for sample clean-up and preconcentration of vitamin B_(12) before determination

A rapid and simple preconcentration step applying packed-fiber solid-phase extraction columns has been investigated to vitamin B12. The extraction performance of the new method was investigated preliminarily on vitamin functional drink. The analysis used a reversed-phase C18 column, with a photo-diode array detector at 220 nm. The samples were preconcentrated with packed-fiber solid-phase extraction columns. Good linearity was observed in vitamin functional drink. The repeatability of extraction performance, expressed as relative standard deviations, was from 3.5% to 4.3%. The limit of detection （LOD） is 5 ng mL^-1 （S/N = 3）. Finally, the method had been applied for the determination of vitamin B12 in vitamin functional drink.

Sequential injection spectrophotometric determination of nanomolar nitrite in seawater by on-line preconcentration with HLB cartridge

The unstable state of nitrite results in its very low concentration in seawater, which is below the limit of detection （LOD） of conventional techniques of analysis. Some sensitivity-enhanced methods have been proposed for the determination of nitrite at nanomolar level to illustrate the role of nitrite in the marine nitrogen cycle. However, most of previous reports are not widely accepted, because of their complexity and cost equipment or intensive labor requirement. In this study, a simple automatic system for the determination of nanomolar level nitrite using on-line preconcentration with spectrophotometric detection was described..An Oasis HLB cartridge was adopted to quantitatively enrich the pink-colored azo compound, formed from nitrite via Griess reaction. The cartridge was rinsed with water and ethanol （volume fraction is 55%, the same below）, in turn, then eluted by an eluent containing 50% ethanol and 0.25 M（mol/dm^3） H2SO4, and determined at 543 nm with a 2 cm path-length flow cell. Under the optimized experimental conditions, the calibration curve showed a good linearity in the range of 1.4 85.7 aM, and the LOD （3a） was estimated to be 0.5 nM. The relative standard deviations of 7 measurements were 4.0% and 1.0% for the samples spiked at 7.1 and 28.6 nM, respectively. The recoveries for the different natural water samples were between 92.2%-108.4%. Each HLB cartridge could be reused for at least 50 times. As compared with other SPE methods, the advantages of this method included the free of interference from salinity variation and less sample consuming. The results of the application of the proposed method to natural water showed good agreement with liquid waveguide capillary cell detection method.

Iodine Determination by Microwave Plasma Torch Atomic Emission Spectrometer Coupled with Online Preconcentration Vapor Generation Technique

This article focuses on iodine determination by microwave plasma torch atomic emission spectrometry （MPT-AES） coupled with online preconcentration vapor generation method. A new desolvation device, multistrand Nafion dryer, was used as the substitute for condenser desolvation system. Some experimental conditions, such as preconcentration time, acidity of sample solution, rinsing solution acidity and dynamic linear range were investigated and optimized. The new desolvation system eliminates the problem of decreasing emission intensity of I（I） 206.238 nm line with the increase of working time on a conventional condenser desolvation system, thus greatly improving the reproducibility.

Flow Injection Semi-online Preconcentration Graphite Furnace Atomic Absorption Spectrometry for Determination of Cadmium,Copper and Manganese

A micro-flow injection sorbent extraction preconcentration system was combined with a graphite furnace atomic absorption spectrometry that formed an integrated system for the determination of trace amounts of elements. The analytical performances of the prospsed method for determining Cd, Cu and Mn were studied. The analytes were preconcentrated with a thiol resin(Type 190, produced by Nankai University, China) whose active group is -SH. The elements to be determined were preconcentrated onto the column for 60 s and then rinsed with deionized water and eluted with 30 μL of 1 mol/L HCl. The graphite furnace atomic absorption spectrometry(GFAAS) determination of the concentrated analyte was carried out in parallel with the next preconcentration cycle. Enrichment factors 41, 22 and 20 and detection limits(3 σ , n =10) 0.36, 3.8 and 7.0 ng/L for Cd, Cu and Mn, respectively, along with a sampling frequency of 20 h -1 , were obtained with a 60 s loading time at a sample flow rate of 3.5 mL/min. The analytical results for a number of water samples show that the flow-injection semi-online column preconcentration can not only eliminate the effect of some concomitant elements, such as Li, Na, K, Ca and Mg, on the determination of the analyte, but also enhance the sensitivity.

On-line Preconcentration of Trace Nickel from Electrolytic Manganese Using Minicolumn Packed Activated Carbon for Electrothermal Atomic Absorption Spectrometry

The online flow injection preconcentration and electrothermal atomic absorption spectrometry method were used for the determination of trace nickel in electrolytic manganese samples by sorption on a conical minicolumn packed with activated carbon at pH 9.0. The nickel was eluted from the minicolumn with 10%(v/v) nitric acid. An enrichment factor of 190-fold for a sample volume of 10mL was obtained. The detection limit (DL) of nickel with the use of the preconcentration method was 13ng·g -1in the original solid sample. The precision for 10 replicate determinations at 150ng·g -1 nickel concentration was 5.2% relative standard deviation (RSD). The calibration graph was linear with a correlation coefficient of r=0.9996 up to concentration of 660ng·g -1 nickel.

Preconcentration by Using Microcrystalline Phenolphthalein for Determining Trace Molybdenum(Ⅵ) in Water by GFAAS

Molybdenum（ Ⅵ ） is a biologically essential trace element and its role in an extremely wide variety of systems has been reported. Most common methods often fail to determine trace Mo （ Ⅵ ） in the analysis of molybdenum-containing samples, due to limitations such as inadequate detection limits and matrix interference, which make the direct determinations impossible. To solve this problem, various approaches are employed to concentrate and separate Mo（ Ⅵ ） to detectable levels. Concentration and separation methods play a main role in the analysis of trace Mo（Ⅵ）. Therefore, many separation and preconcentration procedures have been developed for the determination of Mo （ Ⅵ ）.

Preconcentration of Vanadium(Ⅴ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry

A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.

On-line Preconcentration and Determination of Trace Metals in Water Samples by Flow Injection Combined with Flame Atomic Absorption Spectrometry via Calix[4]arene Carboxylic Acid Packed Micro-column

An adsorbent calix[4]arene carboxylic acid was employed as the adsorption material for on-line flow in jection（FI） micro-column preconcentration coupled with flame atomic absorption spectrometry（FAAS） determination of trace heavy metals（Cu, Pb, Co, Ni and Cd）. Parameters such as the pH, loading time and flow rate of sample, and the concentration, volume and flow rate of eluent were optimized. The enrichment factors are 50.0, 56.5, 11.6, 12.1 and 19.1 for Cu, Pb, Co, Ni, and Cd, respectively, and a sample throughput of 20 h–1 was obtained. The limits of de tection for Cu, Pb, Co, Ni, and Cd were in a range of 1.56―3.91 μg/L, and the relative standard deviations（RSDs） were less than 2.76%（n=7）. Furthermore, the proposed method was successfully applied to the determination of Cu, Pb, Co, Ni, and Cd in certified reference materials and various water samples.

Flow-Injection Microcolumn on-Line Preconcentration for theDetermination of Chromium(Ⅵ)

A rapid and sensitive on-line preconcentration method for spectrophotometric determination of chromium (VI) in nature water is described. Preconcentration and determination are based on (i) the quantitative and fast adsorption of chromium (VI) on the high surface area nanometer-size TiO2 (anatase) powders, which prepared by a sol-gel method from hydrolysis of TiCI4 and (ii) the quantitative and reproducible elution of Cr (VI) by 2. 0 mol. L-1 HCI. A mini-column system for preconcentration is developed, Cr(VI)on the mini-column is eluted and merged with a stream water and DPCB (1, 5-diphenylcarbazide ) as the chromogenic reagent. The Proposed system permits throughputs of 6 sample h--l (0. 001 μg mL-1 Cr(VI) ) or 20 sample h-1 (0. 1 μg mL-1Cr (VI) . The preconcentration factor is 55. The detection limit is 0. 8 ng·mL-1 Cr(VI). The reproducibility is satisfactory with a relative standard deviation of less than 3. 35% (0. Of μg'mL-1Cr (VI), n = 5).

A New Thioamide Derivative for Separation and Preconcentration of Multi Elements in Aquatic Environment by Cloud Point Extraction

2-(pyridine-2-yl)-N-p-chlorohydrazinecarbothioamide (HCPTS) was synthesized, characterized and successfully applied for the preconcentration of Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II) in water, blood, and urine samples prior to graphite furnace atomic absorption determination (GFAAS);Hg was determined by cold vapor technique. Under the optimum experimental conditions (i.e. pH = 8, 10–4 M of HCPTS, 0.05% w/v of Triton X-114), calibration graphs were linear in the range of 0.02 to 200 ng?mL–1 for Co(II), Cd(II), Pb(II) and Ni(II);0.03 to 200 ng?mL–1 for Cu(II);0.07 to 200 ng?mL–1 for Fe(II) and Zn(II) and 0.02 to 150 ng?mL–1 for Hg(II). The enrichment factors were 43, 51, 41, 46, 54, 40, 45 and 52 for Cu(II), Ni(II),Zn (II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The limit of detection were found to be 0.019, 0.094, 0.0514, 0.052, 0.0165, 0.047, 0.068 and 0.041 ng?mL–1 for Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The developed method was applied to the determination of these metal ions in water, blood and urine samples with satisfactory results.

Determination of Trace Non Rare Earth Elements in High Purity Rare Earth Oxides by ICP－AES with Microcolumn Preconcentration in a Flow Injection System

A new method for the determination of trace non-rare earth elements in high purity rare earth oxides by ICP-AES with preconcentration on an active carbon-silica gel microcolumn in a flow injection system is described in this paper. Experimental parameters such as pH, flow rate,reagent concentration,length of reaction coil,eluent acidity,etc. were optimized. In the buffer solution of NH3. H2O/NH4Cl at pH 4. 6,Al,Cr,Cu,Fe, Pb, V and Zn can be preconcentrated and then eluted with 4. 5 mol/L nitric acid utilizing stop-flow technique. The enrichment factors were in range of 8. 1￣12. 6 with detection limits of μg/m level ,and the RSD with metals at μg/g level were 2. 3￣5. 0% (n= 7). The method proposed can reduce the matrix interference effectively , and has been applied to the determination of non-rare earth metals atμg/g level in high purity Eu2O3 with satisfactory results.

Preconcentration and determination of trace copper(II) in natural water using silica gel modified with 1-(2-pyridylazo)-2-naphthol

Trace copper (II) in water can be preconcentrated using silica gel modified with 1-(2-pyridylazo)-2-naphthol (PAN) and be determined spectrophotometri-cally. The conditions for the preconcentration were studied. The method was applied to both artificial and natural water samples and the results suggest that copper (II) of ppb level in water can be measured accurately after the preconcentration.

Separation,preconcentration and determination of Pb(Ⅱ) in water samples using microcrystalline triphenylmethane loaded with quinolin-8-olate

This paper described a novel method for the preconcentration of Pb（II） using microcrystalline triphenylmethane loaded with quinolin-8-olate prior to the determination by flame atomic absorption spectrometry. Pb（II） could be enriched by controlling appropriate condition. The preconcentration factor could reach to 200 and the detection limit of Pb（II） was 0.074 μg/L. The recovery was in a range of 93.5-103% with relative standard deviation of 1.0-2.2%. The proposed method had been successfully applied to the determination of trace Pb（U） in various water samples with satisfactory result.

Cobalt Determination by Means of Flow Injection On-line Sorbent Preconcentration-Flame Atomic Absorption Spectrometry with 1-Nitroso-2-naphthol as a Complexing Reagent

The suitability of 1-nitroso-2-naphthol(NN) as a complexing agent for on-line preconcentration of cobalt eluted on the C_(18) microcolumn by means of the FI-FAAS system was tested. Various parameters affecting the complex formation and its elution were optimized. A 2.3×10^(-3) mol/L reagent solution and the aqueous sample solution acidified with 0.1% (volume fraction) nitric acid were on-line mixed (6.4 mL/min) on a reaction coil set at (65±1)℃ and flowed through the microcolumn for 30 s. The pH of the mixed solution was adjusted to 3—4 with HNO_3(1 mol/L) or NaOH(1 mol/L). The adsorbed complexes in the microcolumn were eluted into the nebulizer of FAAS in 10 s with ethanol acidified with 1% HNO_3(3.0 mL/min). A good precision(1.6% for 100μg/L Co(Ⅱ), n=10), a high enrichment factor 17.2, with detection limit (3σ) 3.2μg/L, and sample throughput (90 h^(-1)) were obtained. The method was applied to the certified reference materials(CRMs), NBS-362 and NBS-364, for the determination of cobalt and the results were in good agreement with the certified values.

Preconcentration of Rare Earth Elements with 8-Hydroxyquinoline-5-sulfonic Acid Chelated Cellulose Filter Prior to Determination by Inductively Coupled Plasma Atomic Emission Spectrometry

Hydroxyquinoline 5 sulfonic acid, covalently bound to filter cellulose, was used for preconcentrating trace rare earth element(REE) ions from complex matrices and matrix separation, respectively. Multi REE ions were preconcentrated on the column filled with 8 hydroxyquinoline 5 sulfonic acid cellulose filter and analysed by ICP AES after being eluted with dilute HNO 3. In the given pH range, alkali and alkaline earth metal ions can be separated as matrix elements; a high concentration factor is obtained and the eluates can be measured without interference. The usefulness of the method is shown by the control analyses of standard reference materials. [WT5FZ]

PRECONCENTRATION OF TRACE ZINC IN SEAWATER ON CPPI RESIN BY FIA AND ON-LINE DETECTION BY ICP-AFS

A quite new type of chelating resin Carboxymethylated Polyethylenimine-Polymethylenepolyphenylene Isocyanate(CPPI)is used for the preconcentration of Zn from high salt water such as seawater. The preconcentration is controlled through the technique of Flow Injection Analysis(FIA).The concentrated sample solution is then directly transferred to an Inductively Coupled Plasma-Atomic Fluorescence Spectrometer(ICP-AFS)for determination.The detection limit of Zn by the technique is about 0.06 ppb.

DETERMINATION OF ANTIMONY IN WATER SAMPLES BY FLOW-INJECTION HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY WITH ON-LINE ION-EXCHANGE COLUMN PRECONCENTRATION

On-line ion-exchange separation and preconcentration were combined with flow-injection hydride generation atomic absorption spectrometry (HGAAS) to determine ultra-trace amounts of antimony in water samples. Antimony(Ⅲ) was preconcentrated on a micro-column packed with CPG-8Q chelating ion-exchanger using time-based sample loading and eluted by 4 mol l^(-1) HCl directly into the hydride generation AAS system. A detection limit (3σ) of 0.0015μg l^(-1) Sb(Ⅲ) was obtained on the basis of a 20 fold enrichment and with a sampling frequency of 60h^(-1). The precision was 1.0% r.s.d.(n=11) at the 0.5μg l^(-1) Sb(Ⅲ) level. Recoveries for the analysis of antimony in tap water, snow water and sea water samples were in the range 97-102%.

Modified monolithic silica capillary for preconcentration of catecholamines

Preconcentration of catecholamines by the modified monolithic silica in the capillary was investigated in this study. In order to achieve a microchip-based method for determining catecholamines in the saliva,the monolithic silica was fabricated in the capillary and the monolithic silica was chemically modified by on-column reaction with phenylboronate. Different modified methods were compared. The concentration conditions were optimized. This study indicates the applicability of the modified monolithic silica capillary when it was used to concentrate catecholamines.

Octa-<i>O</i>-Methoxy Resorcin [4] Arene Amberlite XAD-4 Polymeric Chelating Resin for Solid Phase Extraction, Preconcentration, Separation and Trace Determination of Ni(II), Cu(II), Zn(II) and Cd(II) Ions

Synthetic resin, Amberlite XAD-4 was linked covalently with the third generation supramolecule, octa-O-methoxy resorcin [4] arene through -N=N-group to form chelating resin, which has been characterized and effectively used for the separation and preconcentration of metal ions such as Ni(II), Cu(II), Zn(II) and Cd(II). Critical parameters such as pH, flow rate, sorption capacity, breakthrough studies, distribution coefficient, preconcentration factor, concentration of eluting agents responsible for quantitative extraction of metal ions were optimized. The synthesized resin showed good binding affinity towards Ni(II), Cu(II), Zn(II) and Cd(II) under selective pH conditions. Good breakthrough capacity and fast exchange kinetics of the resin lead to effective separation of metal ions from their binary and ternary mixture by column method on the basis of pH and eluting agents. The resin could be reused for about 8 -10 cycles. The proposed method having the analytical data with the relative standard deviation (RSD) 2% and with recoveries of analytes higher than 98%, reflects upon the reproducibility and reliability of the method which has been successfully applied in the separation and determination of Ni(II), Cu(II), Zn(II) and Cd(II) ions in synthetic, natural and ground water samples.

Determination of Heavy Metals at Sub-ppb Levels in Water by Graphite Furnace Atomic Absorption Spectrometry Using a Direct Introduction Technique after Preconcentration with an Iminodiacetate Extraction Disk

A direct analysis method combining an iminodiacetate extraction disk (IED) with graphite furnace atomic absorption spectrometry was developed for the determination of Co, Ni, Cu, Cd, Sn, Pb, and Bi at sub-ppb levels in water. A 100 mL water sample was adjusted to pH 5.6 with nitric acid and a 1 mol?L–1 ammonium acetate solution, and then passed through an IED (diameter, 47 mm;effective filtering diameter, 35 mm) at a flow rate of 80 - 100 mL?min–1 to preconcentrate seven analytes. The IED was dried at 100?C for 20 min in an electric oven, and 110 - 145 small disks, each 2 mm in diameter, were punched out from the IED. A small disk was introduced into the graphite furnace and atomized according to a heating program. For Cd, Sn, Pb, and Bi measurements, Pd was used as a chemical modifier to enhance the absorbances. Calibration was performed using aqueous standard solutions. The detection limits, corresponding to three times the standard deviation (n = 5) of the blank values, were 0.092 μg·L–1 for Co, 0.12 μg·L–1 for Ni, 0.40 μg·L–1 for Cu, 0.077 μg·L–1 for Cd, 0.92 μg·L–1 for Sn, 0.61 μg·L–1 for Pb, and 0.80 μg·L–1 for Bi with an enrichment factor of 140 using a 100-mL water sample. A spike test for the seven analytes in tap water, rainwater, river water, and mineral drinking water showed quantitative recoveries (93% - 108%).