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
Website: @unf

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Classification: Industrial -> electroplating solution

Citations 16

"Flow Injection Extraction Spectrophotometric Determination Of Nickel Using Bis(acetylacetone)ethylenediimine"
Anal. Chim. Acta 2000 Volume 408, Issue 1-2 Pages 123-127
N. Chimpalee, D. Chimpalee, P. Keawpasert and D. Thorburn Burns

Abstract: Nickel was determined by flow injection spectrophotometry at 370 nm after extraction of nickel(II) bis(acetylacetone)ethylenediiminate chelate into chloroform. The carrier stream was deionized water and the reagent streams were phosphate buffer (pH 7.0) and 1.5% (w/v) bis(acetylacetone)ethylenediimine solutions. The reaction stream was heated to 60degC and then cooled to room temperature prior to extraction into chloroform. The sampling rate was 18 h-1. The calibration graph was linear up to 25 µg mL-1 nickel, based on injection volumes of 250 µL. The relative standard deviation (n=10) was 0.98% for 20 µg mL-1 nickel. The system has been applied to the determination of nickel in nickel-copper alloys and in synthetic electroplating solutions.
Nickel Spectrophotometry Extraction Complexation Heated reaction

"Novel Use Of Doublet Peaks In Flow Injection Analysis. Simultaneous Spectrophotometric Determination Of Nickel(II) And Iron(II)"
Anal. Chim. Acta 1988 Volume 214, Issue 1-2 Pages 197-205
David A. Whitman, Gary D. Christian and Jaromir Ruzicka

Abstract: For the determination of Ni (0.17 to 0.24M) and Fe(II) (2.7 to 5.4 mM) in the same solution, e.g., electroplating bath solution, a flow injection system was used in which the absorbance was measured at 395 nm of Ni(II) and of Fe as Fe(III) after reaction in a 25-cm knotted coil with freshly (online) mixed 2% KSCN and 1% K2S2O8, which served as both reagent and carrier stream (1.5 mL min-1). Two different detector cell configurations were used (descriptions given) according to required sample size (20 to 200 or 200 to 500 µL). Individual elements could be monitored by much weaker peaks at 675 nm (Ni) and 505 nm (Fe(II)). Rectilinear calibration graphs were obtained within the cited ranges, and the general utility of the doublet-peak technique was assessed.
Iron(2+) Nickel(II) Spectrophotometry Calibration Detector Doublet peaks Gradient technique Simultaneous analysis Knotted reactor

"Stoichiometric Measurements In Nickel/hypophosphite Baths For Electroless Deposition"
Anal. Chim. Acta 1994 Volume 290, Issue 3 Pages 287-293
Nima K. Dirjal, Kenneth A. Holbrook* and Peter B. Wells

Abstract: Titrimetric methods and 31P NMR were compared for the determination of hypophosphite (I) and phosphite (II) in both alkaline and acid solution used in the electroless deposition of Ni-P alloys. For accuracy and precision the iodometric method was preferred. To determine I, 5 mL of test solution was added to 28 mL of 6 M HCl, >1 g of KI and 50 mL of 0.02 M KIO3. After standing in the dark for 30 min, the solution was titrated against 0.1 M thiosulfate. The recoveries of I from alkaline plating baths were 92-95%. To determine II, 5 mL of test solution was added to 25 mL of phosphate buffer (pH 7; 0.34 g of KH2PO4 and 0.355 g of Na2HPO4 in 1 l) and 20 mL of 0.05 M I2. After standing in the dark for 1 h, 5 mL of 6 M acetic acid were added and the solution was titrated as above. The recoveries of II from alkaline plating baths were 96-97%. P was determined in the deposited film as 12-molybdophosphate blue (detection at 660 nm) by FIA following dissolution in HNO3 (details given).
Hypophosphite Phosphite Sample preparation Spectrophotometry

"Tubular Detectors For Flow Injection Potentiometric Determination Of Tetrafluoroborate In Electroplating Baths"
Anal. Chim. Acta 1994 Volume 293, Issue 1-2 Pages 35-41
A. N. Araújo, M. B. Etxebarria, J. L. F. C. Lima, M. C. B. S. M. Montenegro,* and R. Pérez Olmos

Abstract: A tubular detector for the determination of tetrafluoroborate was evaluated in a single line FIA system. The detector was described previously by Lapa et. al., (Il Farmaco, 1990, 45, 901), and consisted of an active PVC membrane containing immobilized tetra-octylammonia (as the ion exchanger) and 2-nitrophenyl octyl ether (as the mediator solvent.). The detector exhibited a linear response from 4 µM to 10 M tetrafluoroborate from pH 2.7-11.5 and the detection limit was 2.3 µM. The standard deviation (n = 22) of the analytical signal was 1 mV within the calibration range. The response time was short and enabled a sampling rate of 360/h and the detector life was 36 months. The detector was used in a high dispersion FIA system for the analysis of plating baths. The FIA system allowed a 7 µL volume of plating bath solution to be dispersed in a water carrier stream (8.5 ml/min). The resulting stream was merged with 33 mM sodium sulfate/10 µM-sodium tetrafluoroborate (0.45 ml/min) and passed through the detector cell. The response was linear for 1-6 M tetrafluoroborate. The mean recovery (n = 7) was 98.8% and a RSD of 1.9%.
Tetrafluoroborate Electrode Electrode Potentiometry Apparatus

"Direct Spectrophotometric Determination Of Chromium By Microwave-oven Induced Flow Injection Analysis"
Anal. Chim. Acta 1998 Volume 374, Issue 1 Pages 61-66
Xiaoyuan Wu, Hui Zhao, Xingguo Chen, Zhide Hu*, Zhengfeng Zhao and Martin Hooper

Abstract: Two sensitive flow injection methods were developed for the determination of traces of Cr(VI), based on the very efficient microwave-accelerated reactions of Cr2O72- with dibromocarboxyarsenazo (DBM-AsA, in System 1) and dibromo-o-carborylchlorophonazo (DBOK-CPA, in System 2). The reactions are followed spectrophotometrically by measuring the decrease in the absorbance of DBM-AsA at 535 nm or DBOK-CPA at 556 nm. The sampling frequency for both systems is 40 h-1. The calibration graphs are linear at 1.62-27.0 µg mL-1, and 0.40 and 10.80 µg mL-1 for Systems 1 and 2, respectively. The respectively. detection limits are 0.087 and 0.10 µg mL-1. The methods were applied to determine traces of Cr in a steel sample and electroplating solutions with satisfactory results.
Chromium(VI) Spectrophotometry Microwave Heated reaction Indirect

"Spectrophotometric Determination Of Nickel(II), Iron(II), Boric Acid And Chloride In Plating Baths By Flow Injection Analysis"
Analyst 1988 Volume 113, Issue 12 Pages 1821-1826
David A. Whitman, Gary D. Christian and Jaromir Ruzicka

Abstract: In one set-up, a two-line system was used for the flow injection determination of Ni(II) and Fe(II); Ni(II) (0.17 to 0.24M) was determined directly by spectrophotometry at 675 nm in the presence of 2.7 to 5.4 mM Fe(II). Bivalent Fe was determined after oxidation by S2O82- to Fe(III) which was then caused to react with SCN- with absorbance measurement of the product at 505 nm. In a second set-up, H3BO3 was introduced to 0.1 M Tris buffer (pH 9.7) and was then caused to react with 0.25% azomethine H in aqueous 2% ascorbic acid for absorbance measurement at 420 nm with a two-fold online dilution. The calibration graph was rectilinear from 0.05 to 0.8 M H3BO3. The Cl- concentration. (1.7M) was determined in one of two other set-ups in a reagent stream of aqueous 15% methanol containing 2.4% HNO3, 75 mM Fe(NO3)3 and 2 mM Hg(SCN)2. The absorbance of the Fe(SCN)2+ complex formed after Cl- - Hg(SCN)2reaction, was measured at 480 nm. The methods were applied to the determination of Ni(II), Fe(II), H3BO3 and Cl- in electroplating solutions.
Iron(2+) Nickel(II) Chloride Boric acid Spectrophotometry Dilution Merging zones Simultaneous analysis Complexation

"Voltammetric Determination Of High Concentrations Of Metal Ions In A Continuous-flow System At Vitreous-carbon Electrodes"
Fresenius J. Anal. Chem. 1985 Volume 322, Issue 3 Pages 334-335
B. Lendermann Contact Information und U. Giese

Abstract: The determination of 1 to 100 g L-1 of Pb or Cd in aqueous solution is effected with use of a microprocessor-controlled polarograph and a flow cell with a vitreous-carbon electrode vs. silver - AgCl. The mobile phase (0.8 mL min-1) was 0.1 M KNO3 and the scan rate was 600 mV s-1 starting at -0.45 and -0.60 V for Pb and Cd, respectively. The calibration graph for Pb was not rectilinear. The method may be applied to the analysis of electroplating solution and waste liquors.
Palladium Cadmium Electrode Voltammetry

"Flow Injection Analysis Of High Chloride Levels In Electroplating Baths Using Online Dialysis And Potentiometric Detection"
Fresenius J. Anal. Chem. 1995 Volume 351, Issue 7 Pages 614-617
A. N. Araújo, M. B. Etxebarria, J. L. F. C. Lima, M. C. B. S. M. Montenegro and R. Pérez Olmos

Abstract: Electroplating bath solution (80 µL) was injected into a carrier stream (0.5 ml/min) of water which merged with a stream (2 ml/min) of 2 M Na2SO4 in a mixing coil (56 cm x 0.8 mm i.d.). The stream passed to a dialysis unit (3.5 cm long) with an acceptor stream (2 ml/min) of 0.8 mM HNO3/0.1 M KNO3 to a tabular chloride electrode with a homogeneous crystalline membrane as previously described (Ferreira et al., Ibid., 1993, 347, 314) for potentiometric measurement. The calibration graph was linear for 1.4-2.5 M chloride. Sample throughput was 30/h.
Chloride Electrode Potentiometry Dialysis Membrane

"Flow Injection Titration Of Chloride In Electroplating Baths With A Silver Tubular Electrode As A Detector"
Anal. Sci. 1997 Volume 13, Issue 1 Pages 89-92

Abstract: A single-channel FIA manifold of high dispersion was used (schematic given). Sample was injected into a 1.5 mM AgNO3 carrier stream containing 1 M KNO3 to increase the conductivity and adjust the ionic strength through a 390 cm coil to create the exponential concentration gradient required in FIA 'pseudo-titrations'. The optimum flow rate was 3.6 ml/min. Ag tubular electrodes with a homogeneous crystalline membrane was used as the indicator electrode (cf. Ferreira and Lima, J. Flow Injection Anal., 1993, 10, 17). The method was suitable for chloride concentrations of 0.06-2.5M. The RSD was ~5% and the sampling rate was ~78 samples/h.
Chloride Electrode Potentiometry Titrations Dispersion Optimization Gradient technique

"An Automated Ion Analyzer"
Am. Lab. 1985 Volume 17, Issue 2 Pages 92-97
Ranger, C.B.

Abstract: An automated system is described that incorporates flow-injection anal. and ion chromatography, allowing both techniques to be performed either sequentially or simultaneously using a single instrument. Several examples, including anion determination in acid rain sample, Fe determination in presence of Pu, Ni and Zn determination in phosphate bath, are given to illustrate the performance of the system. Several levels of sample preparation can be incorporated in-line to provide complete automation. (SFS)
Anions Iron Automation Review

"Development And Application Of Graphite-teflon Composite Coating Electrode"
Gaodeng Xuexiao Huaxue Xuebao 1997 Volume 18, Issue 4 Pages 535-537
Xu, H.D.;Luo, Y.J.;Zou, M.Z.

Abstract: In this paper, the procedure of preparation of graphite-Teflon composite electrode (GTE) by coating was investigated. The coating consisted of a solid mixture 2.5 g(graphite 45%, Teflon 45% and PVC 10%) mixed with a solvent(THF: DMF = 1:4 in volume) 0.8 mL. Copper wires(phi = 0.7 mm) were coated by the coating and heated at 200°C for 5 min, and the GTEs were finished. They could be modified and changed into other metallic Teflon composite electrode only by electroplating in correspondent plating bath, such as mercury- cobalt- or copper- Teflon composite electrode. They had been applied to flow injection analysis by techniques of electrochemistry successfully. 8 References
Electrode Electrode Voltammetry Apparatus Detector

"Studies On Flow Injection Analysis Automatic Dilution Techniques And Their Applications"
Fenxi Shiyanshi 1991 Volume 10, Issue 3 Pages 56-58
Lin, S.;Lu, L.;Li, Y.

Abstract: Three types of automatic dilution techniques, viz., small-volume injection sampling, sequental-injection zone sampling and sample splitting, were investigated, with regard to simplicity, flexibilty, dilution factors and precision. Dilution factors were from 50 (for small-volume injection sampling) to 1000 (for sample splitting). The techniques were highly efficient with excellent precision over a wide range of dilution. The sample-splitting method was applied to ores and electroplating solution; coefficient of variation were 0.3%.
Automation Dilution Precision Small sample Sample splitting Zone sampling

"Determination Of Highly Concentrated Zinc In Zinc Plating Passivating Solutions By A Zone-sampling Flow Injection Analysis Method"
Fenxi Shiyanshi 1996 Volume 15, Issue 4 Pages 73-75
Liu, P.;Zhou, D.;Su, D.L.

Abstract: Sample (30 µL) was injected into a a carrier stream of water at 3.6 ml/min in a flow injection system (schematic shown) and dispersed before entering a second sampling loop. A 50 µL portion of the diluted sample was carried by a stream of aqueous 0.012% xylenol orange at 4.2 ml/min to a reactor (250 cm long) and the absorbance was measured at 570 nm. The concentrated sample was diluted more than 1000-fold automatically by this zone-sampling technique and variation of manifold factors. Little interference was observed from the main components of CrO3 and Cr(III) in the solution, whereas the other ions including Fe(III), Cd(II) and Cu(II) did not interfere. The RSD (n = 20) was 1% for 16 g/l Zn(II). Sampling frequency was 84 runs per h. In practice, recoveries were 92.8-104.7%. Results were compared with those obtained by the EDTA method and by AAS.
Zinc Spectrophotometry Zone sampling Method comparison Interferences

"Flow Injection Determination Of Copper(II) In Chemical And Electrochemical Baths With A Potentiometric Differential Microdetector"
Lab. Rob. Autom. 1997 Volume 9, Issue 6 Pages 305-308
Liliana Olenic*, Elena Hopîrtean, Liviu Olenic, Daniela Crisan

Abstract: A differential microdetector with two similar Cu(II) selective membranes was used for discontinuous flow potentiometric determinations of Cu(II). The influence of some factors (temperature, medium, etc.) is eliminated. The method is very simple and sensitive. The results obtained show that the errors are below 1%, thus fully meeting the practical requirements. The method correlates well with the results of the titration determination of Cu(II). The throughput was 60 samples/h. The method proposed has an important utilization in the regeneration of the baths considering the decrease in their concentrations during the metal-coating process.
Copper(II) Potentiometry Detector

"Flow Injection Spectrophotometric Determination Of Manganese In Electroplating Solutions"
Lihua Jianyan, Huaxue Fence 1989 Volume 25, Issue 4 Pages 207-208
Tao, S.;Hu, X.;Wang, H.;Lin, S.

Abstract: A 2 mL sample, obtained by tenfold dilution of the electroplating solution, is mixed with 3 mL of aqueous NH3 and 3 drops of 3% H2O2 solution and then heated in a water bath (at 80°C) for 2 min before addition of 3 drops of 0.2% Na2OsO4 solution. After being cooled, the mixture is centrifuged at 4000 rpm, and the ppt. is dissolved in 3 mL of 2 M H3PO4 and 0.5 mL of 1 M KI. The solution is diluted with water to 25 mL. The I3- produced (stable for 24 h) is determined by flow injection spectrophotometry, with water as carrier stream and detection at 400 nm. Beer's law is obeyed for 0 to 1.6 mg mL-1 of Mn. Recovery was 100 to 103%. Results agreed well with those by ICP-AES. For determination of 0.4 mg of Mn, NaCl (200 mg), Ni (100 mg), Co or BO33- (10), Cu (5), and Fe(III), Cr(III), Cd or Sn(II) (1) did not interfere.
Manganese Spectrophotometry Interferences Indirect Method comparison

"Flow Injection Analysis - Spectrophotometric Determination Of Cobalt In Electroplating Solution"
Lihua Jianyan, Huaxue Fence 1989 Volume 25, Issue 4 Pages 227-230
Hu, X.;Tao, S.;Liao, Q.;Lin, S.

Abstract: A 4 mL sample of Ni - Co - Mn electroplating solution (containing >0.1 mg mL-1 of Co) is heated to 75°C with 4 mL of aqueous NH3 and drop of H2O2 solution for 3 min, followed by addition of 1 drop of Na2O5O4 solution (0.2 mg mL-1) and heating for 5 min more. A portion of this mixture is introduced into a flow injection analyzer. with 23% Na2SO4 as carrier stream to react with H2SO4 (1:5) during which Ni(NH3)62+ is decomposed. The absorbance of the solution containing Co(NH3)63+ is measured at 500 nm. Beer's law is obeyed for 0 to 14 mg of Co in 25 mL of solution For determination of 4 mg of Co, 200 mg of Ni does not interfere; other elements (e.g. Mn, precipitated as MnO2) do not interfere. Results are similar to those obtained by ICP-AES.
Cobalt Spectrophotometry Method comparison Interferences