beinrohr-trace analysis.ppt [režim kompatibility]
TRANSCRIPT
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Trace Analysis of Concentrated Sulphuric Acid and Zinc Sulphate by
Flow-Through Coulometry
Ernest Beinrohr, Pavol Beinrohr and Stanislava Hlubikova
Department of Analytical ChemistrySlovak Technical University, Bratislava
ISTRAN, s.r.o., Bratislava
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Tasks for analytical chemists:
Raw materials
Products
Bulk analysis
Surface analysis
Wastes
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Bulk analysis
Robust system
Automation
Low cost/analysis
Requirements:
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Theory
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Chronopotentiometry
Pb0 – 2 e- ⇒ Pb2+
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Chronopotentiometry
Pb0 – 2 e- ⇒ Pb2+
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Experimental
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The cell and electrode
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Results
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Fe in sulphuric acid
Electrode: microporous E-53C
Electrolyte: diluted HCl
Method: in-electrode coulometric titration (reduction)
Parameters:
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Fe3+ + e- ⇒ Fe2+
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Fe in zinc sulphate
Electrode: macroporous E-104N
Electrolyte: diluted HCl
Method: in-electrode coulometric titration (oxidation)
Parameters:
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Fe2+ - e- ⇒ Fe3+
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Cd, Pb, Cu in zinc sulphate
Electrode: macroporous E-104L
Electrolyte: diluted HCl
Method: stripping coulometry
Parameters:
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Cd Pb Cu
1st step: Cd2+ + 2 e- ⇒ Cd0
2nd step: Cd0 - 2 e- ⇒ Cd2+
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As, Sb in zinc sulphate
Electrode: E-T/Au and E-CA/Au
Electrolyte: diluted HCl
Method: stripping coulometry
Parameters:
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As
Sb
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Chlorides in zinc sulphate
Electrode: E-CA/Ag
Electrolyte: diluted HNO3
Method: coulometric titration
Parameters:
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1st step: Cl- + Ag0 - e- ⇒ AgCl2nd step: AgCl + e- ⇒ Ag0 + Cl-
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Conclusions:
Fe in sulphuric acid can be measured down to 0.1 mg/L
Cd, Pb, Cu, As, Sb, Mn in zinc sulphate can be measured down to 0.01 mg/L
Chlorides in zinc sulphate can be measured in the range of to 1 to 1000 mg/L
and more …
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Metals:Fe, Ni, Cr, Pb, Cd, Bi, Hg …
Semimetals:As, Se, Sb
Non-metals:S2-, Cl-, NO3
-, PO43- …
Organics:EDTA …
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Thank you