title: Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry.
abstract: An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be <5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L(-1) and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples.
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan. Electronic address: naeemullah433@yahoo.com.
authors.lastname: Naeemullah
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
authors.forename: Tasneem Gul
authors.initials: TG
authors.lastname: Kazi
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
authors.forename: Hassan Imran
authors.initials: HI
authors.lastname: Afridi
authors.affiliation: Department of Chemistry, COMSATS Institute of Information Technology, Abbottabad 22060, Pakistan.
authors.forename: Faheem
authors.initials: F
authors.lastname: Shah
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
authors.forename: Sadaf Sadia
authors.initials: SS
authors.lastname: Arain
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
authors.forename: Salma Aslam
authors.initials: SA
authors.lastname: Arain
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
authors.forename: Abdul Haleem
authors.initials: AH
authors.lastname: Panhwar
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
authors.forename: Mariam Shahzadi
authors.initials: MS
authors.lastname: Arain
authors.affiliation: Center for Pure and Applied Geology, University of Sindh, Jamshoro 76080, Pakistan.
authors.forename: Muhammad Kashif
authors.initials: MK
authors.lastname: Samoon
mesh_terms: D056831:Coordination Complexes / Q000737:chemistry*; D004867:Equipment Design; D005618:Fresh Water / Q000032:analysis*; D057230:Limit of Detection; D011759:Pyrrolidines / Q000737:chemistry*; D015203:Reproducibility of Results; D012834:Silver / Q000032:analysis* / Q000302:isolation & purification; D052617:Solid Phase Microextraction / Q000295:instrumentation*; D013054:Spectrophotometry, Atomic / Q000295:instrumentation; D013594:Syringes; D013859:Thiocarbamates / Q000737:chemistry*; D062065:Wastewater / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D056831:Coordination Complexes; D011759:Pyrrolidines; D012834:Silver; D013859:Thiocarbamates; D062065:Wastewater; D014874:Water Pollutants, Chemical; C020972:pyrrolidine dithiocarbamic acid
keywords: Activated carbon cloth; Electrothermal atomic absorption spectrometry; Micropipette tip; Silver(I); Solid phase microextraction; Syringe