University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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Pyrrolidine dithiocarbamate

Citations 5

"Determination Of Copper, Manganese And Nickel In Biological Samples And Sea-water By Flow Injection Online Sorption Preconcentration In A Knotted Reactor Coupled With Electrothermal Atomic Absorption Spectrometry"
J. Anal. At. Spectrom. 1998 Volume 13, Issue 6 Pages 527-531
Elissaveta Ivanova, Karima Benkhedda and Freddy Adams

Abstract: A flow injection system with online sorption pre-concentration of copper, nickel and manganese with ammonium pyrrolidinedithiocarbamate (APDC) or 8-hydroxyquinoline (HQ) in a knotted reactor (KR) coupled with electrothermal atomic absorption spectrometry was developed. APDC offered better performance characteristics than HQ for the pre-concentration of copper and nickel but could not be employed for manganese. The performance characteristics of the determination of copper and nickel with APDC were: detection limits (3s), 6.0 and 7.6 ng L-1, precision (relative standard deviation) 2.5% for 0.2 µg L-1 and 1.5% for 0.2 µg L-1 and enhancement factors 44 and 21 using a 30 s pre-concentration time. The corresponding parameters for the determination of manganese with HQ were detection limit 29.0 ng L-1, precision (relative standard deviation) 2.9% for 0.4 µg-1 manganese and enhancement factor 8 with a 30 s pre-concentration time. The sampling frequency was 26 h-1. The accuracy of the method was demonstrated by the anal. of certified reference materials and by recovery measurements on spiked samples.
Copper Manganese Nickel Biological Sea Spectrophotometry

"Flow Injection Online Sorption Preconcentration Of Platinum In A Knotted Reactor Coupled With Electrothermal Atomic Absorption Spectrometry"
Fresenius J. Anal. Chem. 1998 Volume 361, Issue 5 Pages 445-450
E. Ivanova and F. Adams

Abstract: A flow injection online sorption pre-concentration method for the electrothermal AAS determination of Pt was developed. The pyrrolidine dithiocarbamate complexes of either Pt4+ or Pt2+, formed in 0.7 mol L-1 HNO3, are online adsorbed on the inner walls of a PTFE knotted reactor and subsequently eluted with MeOH. An enhancement factor of 112 and a detection limit (3s) of 10 ng L-1 along with a sampling frequency of 21 h-1 were achieved with a 90 s pre-concentration time at a sample flow rate of 8.8 mL min-1. The RSD is 2.5% for 0.4 µg L-1 Pt. The method was applied to the determination of Pt in blood samples.
Platinum Blood Spectrophotometry

"Mercury Speciation By Coupling Cold Vapor Atomic Absorption Spectrometry With Flow Injection Online Preconcentration And Liquid Chromatographic Separation"
Fresenius J. Anal. Chem. 1998 Volume 361, Issue 8 Pages 761-766
Xuefeng Yin, Wolfgang Frech, Erwin Hoffmann, C. Lüdke, Jochen Skole

Abstract: A fully automated system for the direct determination of methylmercury (MeHg), ethylmercury (EtHg), phenylmercury (PhHg), and inorganic mercury (Hg(II)) at the ng/L level is described. It is based on solid phase extraction pre-concentration incorporated in a flow injection (FI) system, high performance liquid chromatography (HPLC) separation, reduction combined with thermolysis and determination by cold vapor atomic absorption spectrometry (CVAAS). For pre-concentration a microcolumn of bonded silica with octadecyl functional groups (C18 reversed phase material) was used as a sorbent for the Hg complexes formed online with ammonium pyrrolidine dithiocarbamate. Retained mercury species are eluted with a methanol-acetonitrile-water mixture and subjected to separation on an octadecyl silane (ODS) column before determination by CVAAS. The sensitivity of organo-mercury determination could be improved by NaBH4 as a reductant combined with a thermolysis step. To perform online measurements the pre-concentration microcolumn was mounted in a pressure-tight casing. Limits of detection for MeHg, EtHg, PhHg, and Hg(II) employing a sample volume of 58.5 mL were 9, 6, 10, and 5 ng/L, respectively. The RSD calculated from 9 repeated measurements was 3.6, 5.5, 10.4, and 7.6% for MeHg, EtHg, PhHg, and Hg(II), respectively. Finally, the application of this method for speciation of Hg in fish and human urine is described.
Mercury(II) Methylmercury ion Phenylmercury Ethylmercury Marine Urine Spectrophotometry HPLC

"Preconcentration Of Trace Metals For Their Determination With ICP-AES"
Fortschr. Atomspektrom. Spurenanal. 1984 Volume 1, Issue 1 Pages 491-499
Vos, Gerrit; Van Dordrecht, Peter; Ten Bras, Petrus W. (SFS)

Abstract: Trace metals were determined in natural waters by inductively coupled plasma atomic emission spectroscopy (ICP-AES) after pre-concentration by ion exchange or solvent extraction Chelex 100 [11139-85-8] gave better recoveries of Mn, Co, Ni, Cu, Zn, Cd, and Pb than Amberlite IR 120 [9002-23-7] or 8-hydroxyquinoline [148-24-3] immobilized on SiO2. However, CHCl3 extraction with 4-ethyl-1,2,4-triazole [43183-55-7]/Na diethyldithiocarbamate (I) [148-18-5] or ammonium pyrrolidinedithiocarbamate [5108-96-3]/I gave better results. (SFS)
Metals, trace Manganese Cobalt Copper Nickel Zinc Cadmium Environmental Ion exchange Spectrophotometry Sample preparation

"Robotic Sample Pretreatment Coupled With Flow Injection Online Sorption Preconcentration-electrothermal Atomic Absorption Spectrometry For The Determination Of Copper In Environmental And Biological Materials"
Lab. Rob. Autom. 1998 Volume 10, Issue 5 Pages 293-298
Alfredo Velasco-Arjona, María Dolores Luque de Castro, Elissaveta Ivanova, Freddy Adams

Abstract: An automated robotic method for sample pretreatment was developed for copper determination in environmental and biological materials at the low microgram per g level. The robotic station performing the preliminary operations as weighing of sample and acid digestion was coupled with the flow injection (FI) online sorption pre-concentration. of the pyrrolidine dithiocarbamate chelate of copper on the walls of a PTFE knotted reactor (KR) and subsequent electrothermal atomic absorption spectrometry (ETAAS) determination of copper. The accuracy of the method was demonstrated by the anal. of environmental and biological certified reference materials. The precision is 1.4-2.5% relative standard deviation in the 4-50 µg/g concentration. range.
Copper Environmental Biological Spectrophotometry