radionica - university of belgradechem.bg.ac.rs/zf/lect/zf2018_ljesevic_gcxgc_practice.pdf ·...
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Radionica
Dan III
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SVEOBUHVATNA DVODIMENZIONALNA GASNA
HROMATOGRAFIJA SA MASENIM
SPEKTROMETROM
(GCXGC-MS)
Marija Lješević,
Istraživač pripravnik, Institut za hemiju, tehnologiju i metalurgiju Univerziteta u Beogradu
U Beogradu, 23.11.2018.
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PUSTANJE UZORAKA
Adekvatna priprema
(ekstrakcija, clean-up- florisil, aluminijum oksid,
silika gel, natrijum sulfat)
Rastvarči
Koncentracija uzoraka
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EKSTRAKCIJA DIZELA
U uzorak se doda 30 mL heksana, pa se propusti kroz filter papir u levak za odvajanje. Izmućka
se i sačeka da se odvoje faze. Heksanska faza se ispusti u erlenmajer u kome je 25 g Na2SO4, a vodena faza
se dva puta reekstrahuje sa po 30 mL heksana. Heksanski ekstrakti se spoje. Nakon pola sata (da se
uzorak osuši natrijum sulfatom), procedi se kroz filter papir u čist balon i upari na vakuum uparivaču do
zapremine od 1-2 mL. Kvantitativno (uz dodatak par mL heksana) uzorak se prebaci u prethodno
odmerene penicilinke i upari do suva strujom azota. Izmeri se količina suvog ostatka.
Cleanup:
Suvi ostatak se rastvori u 8 mL heksana i propusti kroz kolonu fluorisil- natrijum sulfat. Kolona
se pravi: vata, 2g fluorisila, 2 g natrijum sulfata (ili u staklenim Pasterovim pipetama: vata, 0.3 g
fluorisila, 0.3 g natrijum sulfata). Neophodno je da se fluorisil i natrijum sulfat aktiviraju pre pravljenja
kolona (fluorisil na 1500C preko noći, natrijum sulfat na 5500C preko noći). Uzorak se skuplja u prethodno
odmerene penicilinke, pa upari do suva pod strujom azota. Izmeri se količina suvog ostatka.
Suvi ostatak se rastvori u 1 mL heksana, i od tog rastvora pripreme se uzorci za snimanje na GCxGC-MS
(finalna koncentracija u vialama treba da bude do 50 ppm).
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UKLJUČIVANJE
MS
GC
Racunar
He GCS Real time
Vacuum (Auto stratup)
3h
Generator azota
Zoex modulator
Function
Direct Operation
-3
Execute
T=-80
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UZORCI
Real time
Open method
Aquisition
Download intial
parametersTunning
Auto tune
Check tuning results
Save tune file
Sample login
Sample name
Data file
Tune file Start
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AUTOTUNING RESULTS
FWHM (full width at half maximum) vrednosti: 0,5-0,7
Detektor ≤ 2 kV
Relative intensity ratios:
m/z 502 min 2%
m/z 69 min duplo veći od m/z 28
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KREIRANJE METODE
Injektovanje:
split/splitless
GCxGC
Temperaturni program
Hot jet program
MS
Solvent cut time
Acquisition mode (SCAN/SIM)
Event time
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OBRADA HROMATOGRAMA
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GSMS SOLUTION
POSTRUN ANALYSIS
Eurodizel
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CHROMSQUARE
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