699
GC CHROMATOGRAMS |
PHARMACEUTICAL
Organic Volat i le Impur i t ies/Residual Solvents
Organic Volatile 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:
0.2µL mix of 69 neat organic volatile impurities
Instrument:
Agilent 6890 with LECO liquid nitrogen cryojet modulator
Inj.:
split/splitless, split ratio 600:1; gas saver: 20mL/min. after 1 min.;
4mm ID split inlet liner w/wool (cat.# 20781); injection with band formation (fast injection)
Inj. temp.:
250°C
Carrier gas:
helium, constant flow
Flow rate:
1.5mL/min.
Oven temp.:
Rtx
®
-200: 35°C (9 min.) to 220°C @ 3°C/min. (hold 1 min.);
Rtx
®
-Wax: 65°C (9 min.) to 250°C @ 3°C/min. (hold 1 min.)
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
did you
know
?
GCxGC Separations
Separation of the complete list of International Conference on Harmonization Class 1, Class 2,
and Class 3 organic volatiles requires at least two, and often three, separate analyses on differing
capillary GC columns. While many laboratories do not monitor for the complete list, separation of
OVIs still is a challenge, often characterized by long run times and incomplete separations.
Using comprehensive GCxGC, it is possible to resolve all of these target compounds, in a single
analysis, with less than a 1-hour run time. In this approach, two columns of differing selectivity are
used to separate the compounds in a 2-dimensional plot, as shown above. Various detectors also
can be employed, including time-of-flight mass spectrometry, to yield reliable information for the
entire target compound list in a single analysis.
For more about GCxGC, visit our website and search for GCxGC.
Website :
E-mail :
TelNo : 03 9762 2034 . . . in AUSTRALIA
Mar 2011
