Summary
The use of a commercially available AAS graphite tube atomizer as an electrode for the cathodic electrodeposition of element traces at constant-current in a hydrodynamic flow-through-system is described. After deposition the graphite tube is transferred into an atomizer unit for subsequent sensitive determination by atomic absorption spectrometry. The deposition yield of ≥99% (2 h; 1.5 A) for Co was verified, using60Co as a radioactive tracer, by monitoring the concentration fall in the electrolyte solution down to ≤5 pg/ml, and the deposited material. The efficiency of the system for the purification of electrolyte solutions was found to be very high. For the determination of the residual impurities, e.g. in very concentrated NH4F-solutions, a simple ion-exchange procedure was worked out for Cu, Mn, Ni, Pb, Zn. To get back the high purity solid NH4F, the solvent was evaporated partly and the precipitated crystals were sucked off in a PTFE-funnel. To avoid contamination, crystallization was carried out in a closed container system using the principle of subboiling distillation. The purity of the recrystallized NH4F-salt increased by a factor of 2 to 3 (crystallization yield 50–70%) so that a solid product with an impurity level below 0.5 ng/g was obtained.
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Broekaert JAC, Graule T, Jenett H, Tölg G, Tschöpel P (1989) Fresenius Z Anal Chem 332:825
Graule T, von Bohlen A, Broekaert JAC, Grallath E, Klockenkämper R, Tschöpel P, Tölg G (1989) Fresenius Z Anal Chem 335:637
Matousek JP (1981) Progr Anal At Spectrosc 4:247
Tschöpel P, Tölg G (1982) J Trace Microprobe Techn 1:1(1)
Tölg G, Tschöpel P (1987) Anal Sci 3:199
Keel TR, Tisue T (1988) J Environ Anal Chem 34:89
Thomassen Y, Larsen BV, Langmyhr FJ, Lund W (1976) Anal Chim Acta 83:103
Volland G, Tschöpel P, Tölg G (1977) Anal Chim Acta 90:15
Ciszewski A, Fish JR, Malinski T, Sioda RE (1989) Anal Chem 61:856
Sioda RE (1988) Anal Chem 60:1177
Woodriff R, Siemer D (1969) Appl Spectrosc 23:38(1)
Sioda RE, Batley GE, Lund W, Wang J, Leach StC (1986) Talanta 33:421(5)
Batley GE, Matousek JP (1977) Anal Chem 49:2031
Vidal JC, Monreal F, Castillo JR (1990) Analyst 115:539
Eller R (1986) Dissertation Mainz
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Hoppstock, K., Garten, R.P.H., Tschöpel, P. et al. Purification of reagents and separation of element traces by electrodeposition onto a graphite tube cathode. Fresenius J Anal Chem 343, 778–781 (1992). https://doi.org/10.1007/BF00633566
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DOI: https://doi.org/10.1007/BF00633566