ertec, 2-theta, march 2009 microwave digestion of …microwave digestion of samples ertec, 2-theta,...
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Microwave Digestion of Samples
Ertec, 2-Theta, March 2009
Wroclaw, Tesin 2009
Edward Reszke, ERTEC-PolandVasek Helan , 2 THETA, CZ
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High pressure MW systems
Ethos plus from Milestone
digestion vessel Ethos
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Ertec console Reactor/mineralizer Ertec
High pressure digestion system with water cooled steel jacket
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Cross-section of Magnum digestion vessel
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Recovery at microwave and conventional
dissolution of ceramics
Table7. Dissolution speed of „conventional” and
microwave closed approaches
Conventional Teflon bomb Microwave digestor
Matrix (h) (min) (min)
Al2O3 24 1440 20
AlN 2 120 15
BN 5 300 15
Si3N4 6 360 15
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TOC
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Solution of reagents Matrix Uwagi
HNO3 Biological materials incompletye digestion at atrmospheric pressure
HNO3 + H2O2 Biological materials Effective digestion of small samples
HNO3 + H2SO4 general use Frequently used but promotes losses of easili volatile elements such as As, Ge, Hg, Se
HNO3 + HCl general use aqua regia
HNO3 + HClO3 Biological materials High oxidation potential, low loss of As, Hg, Se, In and so on .., safe
HNO3 + HClO4 Biological materials Effective decomposition , low loss of Pb
HNO3 + HCl + HF general use -
HNO3 + HF general use -
HNO3 + HClO4 + H2SO4 general use Temperature regime must be controlled , loss of As, Hg, Fe Sb
HF innorganic materials -
H2SO4 + HClO4 general use Small samples , denger of explosion
H2SO4 + H2O2 general use Losses of As, Hg, Ge, Ru, Se and many other volatile elements
HClO4 Biological materials Strong oxidizer, denger of explosion
H2O2 + Fe3+ Biological materials except oils, fats and grees Decomposition with OH* radicals, low temperature of decomposition, good for large
samples, no loss of elements
Digestion reagents
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Useful Glassware Accessories
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A glance at the new system from the front
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Dwójka
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Czwórka
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Digestion of difficult organic samples with dry mass over 1g
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PRÓBKI WYMAGAJĄCE SZCZEGÓLNEGO PODEJŚCIA
TABLETKI POWLEKANEPOLIMERY PRÓBKI „NIESPODZIANKI” – OLEJ „TRANSFORMATOROWY”
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GRAFIT Z ELEKTROWNI JĄDROWEJ MOCHOWCE – SŁOWACJA
Masa próbki – 0,1gOdczynniki : 5 ml Perchloric acid 70 % + 2 ml H2O
Procedura rozkładu:
Krok 1 – Czas 5 min, Moc: 60 %, Pmax 20 atm, Pmin 17 atm, Tmax 300 ° C Tmin 295 ° C
Krok 2 – Czas 5 min, Moc: 80 %, Pmax 30 atm, Pmin 27 atm, Tmax 300 ° C Tmin 295 ° C
Krok 3 – Czas 10 min, Moc: 100 %, Pmax 45 atm, Pmin 42 atm, Tmax 300 ° C Tmin 295 ° C
Bardzo dobry klarowny roztwór
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Kind of aSample
Drymass[g](up to)
System ERTEC2 modules Magnum(samples/day)
Microwave furnaces with 6 vessel carouselle (samples/day)
Organic 0.5 g1.0 g2.0 g5.0 g
65 50 25 12
50 sometimes impossibleimpossible!!impossible!!!
Mixed 0.5 g1.0 g2.0 g5.0 g
50 38 19 11
36 24
usually impossibleimpossible!!
Non-organic(dissolution only)
0.5 g1.0 g2.0 g5.0 g
35 25 13 6
30 18
sometimes impossible impossible!!
Capability of different digestion systems
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Power efficiency as an and point detection of digestion procedures
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Perhydrol 30ml
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Olej z SEMTEXU 0,4 ml + 6ml HNO3
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Temperature control Temperature control ––A new low A new low -- temperature Kjeldahl temperature Kjeldahl procedureprocedure
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Bułka sucha 1,5g próbka druga
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Olej z SEMTEXU 0,5g – zadziałanie bezpiecznika ciśnieniowego
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Advantages of the new digestion system
1. A new more efficient coupling between the magnetron and the digestion vessel
2. Built-in reflectometer enabling measurements of microwave power reflected from the sample
3. Indication of the ‘well closed” digestion vessel’s head
4. Reduced more ergonomic hight of the digestor
5. A new user-friendly software with more useful data
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Thank you for your attention