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Linear chrono-amperometry using re-dissolution: application to halides; La chronoamperometrie lineaire par redissolution: application aux halogenures

Abstract

The possibility of applying linear chrono-amperometry to analysis was studied using a falling-drop mercury electrode. Measurements of the cations were carried out by direct reduction or by prior formation of an amalgam, which is then oxidized. Using the first technique, the minimum concentration that can be attained is about 10{sup -6} M and the reproducibility of the results is of the order of 2%. With the second method the sensitivity is much improved: in the concentration range of 10{sup -7} to 10{sup -8} M, the scatter of the results is less than 10% if the agitation and temperature conditions are kept constant. The halides are determined by re-dissolving the mercurous halide deposit formed by electrolysis. From the analytical point of view, the sensitivity is limited in the domain where the phenomena can be interpreted and used. In the case of the chloride ion the lower limit of this zone is close to 10{sup -5} M; it is 10{sup -6} M for the bromide and less than 10{sup -7} M for the iodide. For lower concentrations, simple laws that might be applied in analysis are no longer valid. However, the splitting of the peak observed during the reduction of the mercurous  More>>
Authors:
Perchard, J -P; Buvet, M; Molina, R [1] 
  1. Commissariat a l'Energie Atomique, Centre d'Etudes Nucleaires de Fontenay-aux-Roses, 92 (France)
Publication Date:
Jun 01, 1966
Product Type:
Technical Report
Report Number:
CEA-R-3030
Resource Relation:
Other Information: 18 refs; PBD: Jun 1966
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; AMPEROMETRY; ELECTROCHEMISTRY; ELECTROLYSIS; MERCURY BROMIDES; MERCURY CHLORIDES; MERCURY IODIDES
OSTI ID:
20468576
Research Organizations:
Commissariat a l'Energie Atomique, Centre d'Etudes Nucleaires de Fontenay-aux-Roses, 92 (France)
Country of Origin:
France
Language:
French
Other Identifying Numbers:
TRN: FR04R3030044286
Availability:
Available from INIS in electronic form
Submitting Site:
FRN
Size:
[76] pages
Announcement Date:

Citation Formats

Perchard, J -P, Buvet, M, and Molina, R. Linear chrono-amperometry using re-dissolution: application to halides; La chronoamperometrie lineaire par redissolution: application aux halogenures. France: N. p., 1966. Web.
Perchard, J -P, Buvet, M, & Molina, R. Linear chrono-amperometry using re-dissolution: application to halides; La chronoamperometrie lineaire par redissolution: application aux halogenures. France.
Perchard, J -P, Buvet, M, and Molina, R. 1966. "Linear chrono-amperometry using re-dissolution: application to halides; La chronoamperometrie lineaire par redissolution: application aux halogenures." France.
@misc{etde_20468576,
title = {Linear chrono-amperometry using re-dissolution: application to halides; La chronoamperometrie lineaire par redissolution: application aux halogenures}
author = {Perchard, J -P, Buvet, M, and Molina, R}
abstractNote = {The possibility of applying linear chrono-amperometry to analysis was studied using a falling-drop mercury electrode. Measurements of the cations were carried out by direct reduction or by prior formation of an amalgam, which is then oxidized. Using the first technique, the minimum concentration that can be attained is about 10{sup -6} M and the reproducibility of the results is of the order of 2%. With the second method the sensitivity is much improved: in the concentration range of 10{sup -7} to 10{sup -8} M, the scatter of the results is less than 10% if the agitation and temperature conditions are kept constant. The halides are determined by re-dissolving the mercurous halide deposit formed by electrolysis. From the analytical point of view, the sensitivity is limited in the domain where the phenomena can be interpreted and used. In the case of the chloride ion the lower limit of this zone is close to 10{sup -5} M; it is 10{sup -6} M for the bromide and less than 10{sup -7} M for the iodide. For lower concentrations, simple laws that might be applied in analysis are no longer valid. However, the splitting of the peak observed during the reduction of the mercurous iodide deposit was interpreted as showing that the mono-molecular Hg{sub 2}I{sub 2} layer formed on the drop has particular electrochemical properties. (authors) [French] Les possibilites analytiques de la chronoamperometrie lineaire ont ete etudiees en utilisant une electrode de mercure a goutte pendante. Le dosage des cations a ete effectue par reduction directe ou par formation prealable d'un amalgame puis oxydation de celui-ci. Par la premiere technique la concentration minimale que l'on peut atteindre est d'environ 10{sup -6} M et la reproductibilite des resultats est de l'ordre de 2%. Par la seconde methode la sensibilite se trouve grandement amelioree; dans une zone de concentration comprise entre 10{sup -7} et 10{sup -8} M, la dispersion des determinations est inferieure a 10% si les conditions d'agitation et de temperature sont maintenues constantes. Le dosage des halogenures est realise par redissolution d'un depot d'halogenure mercureux constitue par une electrolyse prealable. Du point de vue analytique, la sensibilite est limitee au domaine de concentrations ou les phenomenes sont interpretables et exploitables. Dans le cas de l'ion chlorure la limite inferieure de ce domaine est voisine de 10{sup -5} M; elle est de 10{sup -6} M pour le bromure et inferieure a 10{sup -7} M pour l'iodure. Pour des concentrations inferieures, les lois simples susceptibles d'applications analytiques ne sont plus verifiees. Cependant, le dedoublement du pic observe lors de la reduction de l'iodure mercureux depose a ete interprete en mettant en evidence les proprietes electrochimiques particulieres de la couche mono-moleculaire de Hg{sub 2}I{sub 2} formee sur la goutte. (auteurs)}
place = {France}
year = {1966}
month = {Jun}
}