Skip to main content
U.S. Department of Energy
Office of Scientific and Technical Information

Flow Injection Electrochemical Quartz Crystal Microbalance with ICP-OES Detection: Electroprecipitation and Stripping of Lanthanum and Neodymium in a Flow Cell

Journal Article · · Journal of the Electrochemical Society
 [1];  [2];  [3];  [3]
  1. Washington State Univ., Pullman, WA (United States); University of Notre Dame
  2. Univ. of Florida, Gainesville, FL (United States)
  3. Washington State Univ., Pullman, WA (United States)

We used an improved version of our hyphenated analysis technique, flow injection electrochemical quartz crystal microbalance (EQCM) with inductively coupled optical emission spectroscopy, to investigate the electroprecipitation of lanthanum and neodymium from flowing solutions. The improved version has two independent flow injection circuits, allowing different conditions for electrochemical precipitation (pH=4.3 or 2.6) and quick stripping (2% HNO3) with EQCM mass detection and ICP-OES elemental analysis. Lanthanum or neodymium ions in a 500 uL sample were injected into a carrier stream and deposited onto an EQCM housed in a micro flow cell, owing to a localized high-pH layer. The deposits are subsequently stripped from the electrode using HNO3 and analyzed downstream using an ICP-OES. We found that using acidic solutions without supporting electrolyte leads to an increase of the amount of lanthanum detected by 4-fold. The enhanced deposition can be attributed to enhanced mass transfer by migration. Furthermore, we showed that by applying chronopotentiometry, we can detect a change in the hydrogen evolution reaction mechanism that enables the precipitation of lanthanides on the surface of the electrode. Understanding and enhancing the deposition of lanthanides is relevant for elemental or isotopic detection in nuclear forensics.

Research Organization:
Univ. of Notre Dame, IN (United States)
Sponsoring Organization:
USDOE National Nuclear Security Administration (NNSA), Office of Defense Nuclear Security
Grant/Contract Number:
NA0003763
OSTI ID:
1962373
Journal Information:
Journal of the Electrochemical Society, Journal Name: Journal of the Electrochemical Society Journal Issue: 3 Vol. 170; ISSN 0013-4651
Publisher:
IOP PublishingCopyright Statement
Country of Publication:
United States
Language:
English

References (47)

Investigation of Electron Transfer by Geobacter sulfurreducens Biofilms by using an Electrochemical Quartz Crystal Microbalance journal August 2014
Electrodeposition of actinides for alpha-spectrometry journal December 1999
A robust, field-deployable method for the electrodeposition of actinides journal May 2008
Electrochemical precipitation of neptunium with a micro electrochemical quartz crystal microbalance journal April 2020
Chronopotentiometry of solutions containing sodium iodide and iodine in dimethylsulphoxide journal June 1967
Experimental aspects of use of the quartz crystal microbalance in solution journal October 1985
The conditions for electrodeposition of insoluble hydroxides at a cathode surface: A theoretical investigation journal December 1959
The electrodeposition of insoluble hydroxides —An experimental investigation journal June 1961
Photochemical separation and co-precipitation of lanthanides in nitric acid solution journal June 1997
Inside solid-liquid interfaces: Understanding the influence of the electrical double layer on alkaline hydrogen evolution reaction journal September 2021
Dynamics of bubble formation on submerged capillaries in a non-uniform direct current electric field journal December 2020
Electrodeposition from a binary electrolyte: new developments and applications journal November 2007
In-situ activation of hydrogen evolution in pH-neutral electrolytes by additions of multivalent cations journal June 2012
Preconcentration mechanism of trivalent lanthanum on eQCM electrodes in the presence of α-hydroxy isobutyric acid journal January 2020
Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials journal May 2017
Self-Enhancement of Voltammetric Waves of Weak Acids in the Absence of Supporting Electrolyte journal April 1994
Electrochemical applications of the quartz crystal microbalance journal October 1989
Cathodic Preconcentration of f-Elements on a Mercury Film Carbon Fiber Disk Microelectrode journal June 2011
Rheology of the Electric Double Layer in Electrolyte Solutions journal May 2020
Direct Identification and Analysis of Heavy Metals in Solution (Hg, Cu, Pb, Zn, Ni) by Use of in Situ Electrochemical X-ray Fluorescence journal April 2015
Electrochemical Induced Calcium Phosphate Precipitation: Importance of Local pH journal September 2017
Elucidating the Cathodic Electrodeposition Mechanism of Lead/Lead Oxide Formation in Nitrate Solutions journal March 2017
Standardized Benchmarking of Water Splitting Catalysts in a Combined Electrochemical Flow Cell/Inductively Coupled Plasma–Optical Emission Spectrometry (ICP-OES) Setup journal April 2017
Polarographically Controlled Syntheses, with Particular Reference to Organic Chemistry journal July 1943
U1 snRNP regulates cancer cell migration and invasion in vitro journal January 2020
Hydration and ion pair formation in common aqueous La( iii ) salt solutions – a Raman scattering and DFT study journal January 2015
Electrochemical deposition for the separation and recovery of metals using carbon nanotube-enabled filters journal January 2018
Kinetics of viscoelasticity in the electric double layer following steps in the electrode potential studied by a fast electrochemical quartz crystal microbalance (EQCM) journal January 2021
What is the trigger for the hydrogen evolution reaction? – towards electrocatalysis beyond the Sabatier principle journal January 2020
In situ observation of pH change during water splitting in neutral pH conditions: impact of natural convection driven by buoyancy effects journal January 2020
Flow injection on-line group preconcentration and separation of (ultra)trace rare earth elements in environmental and geological samples by precipitation using a knotted reactor as a filterless collector for inductively coupled plasma mass spectrometric determination journal January 1999
Anomalous behaviour of the quartz crystal microbalance in the presence of electrolytes journal January 2000
Viscoelasticity in the diffuse electric double layerElectronic supplementary information (ESI) available: QCM impedance measurements. See http://www.rsc.org/suppdata/an/b2/b206305k/ journal September 2002
Viscoelastic, mechanical, and dielectric measurements on complex samples with the quartz crystal microbalance journal January 2008
126. Concentration polarisation in acid solutions journal January 1945
Increasing the rate of the hydrogen evolution reaction in neutral water with protic buffer electrolytes journal December 2020
III. On the concentration at the electrodes in a solution, with special reference to the liberation of hydrogen by electrolysis of a mixture of copper sulphate and sulphuric acid journal January 1901
Application of piezoelectric quartz crystals to the analysis of trace metals in solution: a review journal January 2001
Optimization of Actinides Trace Precipitation on Diamond/Si PIN Sensor for Alpha-Spectrometry in Aqueous Solution journal August 2014
Hydrolysis constants of tervalent lanthanum and lanthanide ions in 0.1 M KNO3 solution journal June 2012
Migration Considerations in Chronopotentiometric Analysis journal September 1988
Flow Injection Electrochemical Quartz Crystal Microbalance with ICP-OES Detection: Recovery of Silver by Electrodeposition with Redox Replacement in a Flow Cell journal May 2021
Design and Finite Element Model of a Microfluidic Platform with Removable Electrodes for Electrochemical Analysis journal January 2019
Electrochemical Preconcentration Mechanism of Trivalent Lanthanum journal January 2018
EQCM and Surface pH Studies on Lanthanum Accumulation on Electrodes in Aqueous Solution journal January 2016
Microfluidic-Based Sample Chips for Radioactive Solutions journal March 2015
Electro-Precipitation of Actinides on Boron-Doped Diamond Thin Films for Solid Sources Preparation for High-Resolution Alpha-Particle Spectrometry journal April 2019

Similar Records

Flow Injection Electrochemical Quartz Crystal Microbalance with ICP-OES Detection: Recovery of Silver by Electrodeposition with Redox Replacement in a Flow Cell
Journal Article · Mon May 24 00:00:00 EDT 2021 · Journal of the Electrochemical Society · OSTI ID:1835440

In situ ellipsometric study of the electroprecipitation of nickel hydroxide films
Journal Article · Tue Mar 31 23:00:00 EST 1998 · Journal of the Electrochemical Society · OSTI ID:624297