699
GCCHROMATOGRAMS |
PHARMACEUTICAL
Organic Volatile Impurities/Residual Solvents
OrganicVolatile Impurities
Rtx®-200&Rtx®-WAX (GCxGC)
GC_PH00888
Columns:
Rtx
®
-200, 60m, 0.25mm ID, 1.0µm (cat.# 15056)
Rtx
®
-Wax, 2m, 0.18mm ID, 0.3µm (custom)
Sample:
0.2µLmix of 69 neat organic volatile impurities
Instrument:
Agilent 6890with LECO liquid nitrogen cryojet modulator
Inj.:
split/splitless, split ratio 600:1; gas saver: 20mL/min. after 1min.;
4mm ID split inlet liner w/wool (cat.# 20781); injectionwith band formation (fast injection)
Inj. temp.:
250°C
Carrier gas:
helium, constant flow
Flow rate:
1.5mL/min.
Oven temp.:
Rtx
®
-200: 35°C (9min.) to 220°C@ 3°C/min. (hold 1min.);
Rtx
®
-Wax: 65°C (9min.) to 250°C@ 3°C/min. (hold 1min.)
Modulation:
modulator offset: 30°C; 2nd dimension separation: 4 sec.; hot pulse: 0.3 sec.;
cool between stages: 1.7 sec.
Det:
FID@ 250°C; hydrogen: 40mL/min.; air: 450mL/min.; make-up gas: 45mL/min.; sampling rate: 200Hz
didyou
know
?
GCxGCSeparations
Separationof thecomplete listof International ConferenceonHarmonizationClass1, Class2,
andClass3organicvolatiles requiresat least two, andoften three, separateanalysesondiffering
capillaryGCcolumns.Whilemany laboratoriesdonotmonitor for thecomplete list, separationof
OVIs still isachallenge, oftencharacterizedby long run timesand incomplete separations.
UsingcomprehensiveGCxGC, it ispossible to resolveall of these target compounds, ina single
analysis,with less thana1-hour run time. In thisapproach, twocolumnsof differing selectivityare
used to separate thecompounds ina2-dimensional plot, as shownabove.Variousdetectorsalso
canbeemployed, including time-of-flightmass spectrometry, toyield reliable information for the
entire target compound list ina singleanalysis.
FormoreaboutGCxGC, visitourwebsiteand search forGCxGC.
Website :
E-mail :
TelNo : 03 9762 2034 . . . inAUSTRALIA
Mar 2011
