GC

The world’s most advanced

INVERSE GAS CHROMATOGRAPH
 s
m GC

s
SURFACE
MEASUREMENT
Advanced instrumentation for the characterisation
of particulates, fibres and thin-films.
Opening up a whole new world of
SYSTEMS sorption solutions.

W H A T I S I N V E R S E G A S C H R O M A T O G R A P H Y (I G C) ?

I nverse Gas Chromatography (IGC)

is a gas-phase technique for
characterising surface and bulk
ANALYTICAL GAS CHROMATOGRAPHY

properties of solid materials. The

principles of IGC are very simple,
being the reverse of a conventional
gas chromatographic (GC)
experiment. Sample gas pulse Standard analytical Separated sample peaks
column packing
A cylindrical column is uniformly
packed with the solid material
of interest, typically a powder,
fibre or film. A pulse or constant
concentration of gas is then injected INVERSE GAS CHROMATOGRAPHY (IGC)
down the column at a fixed carrier
gas flow
rate, and the time taken for the pulse
or concentration front to elute down
the column is measured by a detector.
A series of IGC measurements with
different gas phase probe molecules Single probe Packed sample column Single peak
then allows access to a wide range
of gas pulse (particulate or fibre) (Retention time t R )
physico-chemical properties of the solid
sample.
I N T R O D U C I N G T H E R E V O L U T I O N A R Y S M S iG C

T
Column
he revolutionary iGC from SMS SMS iGC SCHEMATIC
is the world’s first commercial Packed sample

inverse gas chromatograph.

The unique SMS flow control
CONTROL PC
technology* provides the state-
of-the-art in humidity control
together with unrivalled accuracy
and reproducibility. The standard
instrument configuration comes
with a thermal conductivity detector FID

(TCD) and a flame ionization detector Carrier gases

(FID): this combination allows

differentiation between moisture TCD

and organic solvent elutants. Further Flow

control
detectors may be added module Probe gas and Flow
humidifier switching
(e.g. Mass Spectrometer)
according to customer module module Column Detector
module modules
requirements.

* patent applied for PROBE GAS OVEN COLUMN OVEN

 iG C I N S T R U M E N T K E Y B E N E F I T S

 Unprecedented Accuracy and Repeatability  Quick and Easy Sample Preparation

The combination of 6 electronic mass flow
controllers, a fixed volume injection loop and
isothermal vapour generation means that the SMS
IGC provides an experimental reproducibility
never before possible with conventional GC
injection systems.
The use of straight 300mm glass columns with the
unique SMS column packer means that a typical
sample can be packed reproducibly in less than
5 minutes. The specially designed quick-change
column fittings allow rapid changeover of samples
while ensuring the integrity of the column seals.

 Fully Automated Analysis  Flexible and Powerful Characterisation Tool

The instrument is operated using IGCWin PC
software allowing the selection of up to 10
different probe molecules in one experiment and
the consecutive analyses of 2 separate columns.
Comprehensive data analysis software brings the
results to your desktop with a few clicks of a mouse.
The SMS IGC instruments are designed with
flexibility in mind. A wide range of experimental
possibilities is available in the standard
configuration including both pulsed and frontal
probe molecule injection, and the independent
control of humidity (%RH) in the carrier gas stream.

iG C S O R P T I O N S O L U T I O N S

The SMS iGC has been designed as a powerful  Bulk Properties

research and QA tool, providing access to many
Diffusion Coefficients
important physicochemical properties of materials.
e.g. Controlled Release Polymers
These properties can provide valuable insight into
particular process or performance-related issues.
Phase Transition Temperatures
e.g. Amorphous recrystallisation
 Surface Chemistry
in Pharmaceuticals
Dispersive Surface Energy
e.g. Pharmaceutical Inhalation Formulation Solubility Parameters
e.g. Stability of Drug
Specific Polar Interactions Polymorphs
FL
A

e.g. Filtration Characteristics of Activated

VO

Carbons
URINGS

Acid-Base Properties
e.g. Surface Characterisation of Catalysts

 Surface Adsorption N
A

D
PE
Isotherms at Low Concentration RFU
MES
e.g. Adsorption on Porous Materials

Surface Heterogeneity
e.g. Effect of Surface Modification Treatments

Competitive Adsorption
PH

e.g. Persistence of Perfumes on Cotton

A

M
R

A
C
EU
TICA
LS

FI
BR
ES
S
L

A
E R
M IN
 CASE STUDY 1: BATCH-TO-BATCH VARIABILITY

IGC may be used to determine batch-to-batch

variations in surface chemistry which may impact
upon the processing or final performance of a
material. In this example IGC was successfully used
to correlate differences in specific polar interactions
for three batches of a pure drug material with their
corresponding dissolution rates. Batch A gave a
good dissolution profile whereas batch C did not
and batch B was just outside the accepted tolerance.
In this case the much higher specific free energies
measured for 1,4 Dioxane and Ethyl Acetate on batch
A indicates an increased availability of hydrophilic
acidic sites on the surface. This information can be
used to explain the differences in surface chemistry
and therefore dissolution behaviour of the different
batches. In this case, the processing of the material
is shown to modify the surface chemistry and hence Specific interactions on three batches of a pure drug
the observed dissolution rates. measured by IGC

CASE STUDY 2: SURFACE HETEROGENEITY IN BINARY MIXTURES

IGC may also be used to determine the surface

heterogeneity (distribution of surface sites) of
single phases or multicomponent mixtures. Surface
heterogeneity can have a significant impact upon
the performance and handling of particulate
solids. In this case IGC was used to determine the
heterogeneity profiles of lactose monohydrate,
magnesium stearate and a 98%:2% mixture of the
two materials. The data shows that by adding 2%
by weight of magnesium stearate the distribution of
surface sites available for interaction is significantly
altered, even though the highest energy sites remain
unchanged. These results may be correlated with
process properties such as powder handling or Surface heterogeneity profiles for lactose,
performance properties such as aerosol dispersion for
magnesium stearate and a 98%:2% mixture of the
example.

CASE STUDY 3: HUMIDITY DEPENDENCE OF GLASS TRANSITION TEMPERATURE

As well as surface properties IGC may also be used

to measure properties of the bulk material such
as glass transition temperatures. In this case the
variation in glass transition temperature (Tg) with
relative humidity (%RH) has been measured by
IGC for the complex sugar maltose. The observed
lowering of the Tg with increasing %RH can have
a dramatic impact upon the storage and processing
stability of polymeric materials, in particular those
with some degree of amorphous character.

Variation of the Tg of Maltose as a function of %RH

 iG C C O N T R O L S O F T W A R E

 Easy to Learn and Use

 Realtime Display Of Experiment Progress

 Quick-set Methods

 Save and Restore Methods

 Batch Running of up to 10 Methods

 Preconditioning Methods

 Wide Range of Method Variables;

Probe Molecule, Temperature, %RH,
Flow Rate and Probe Molecule Concentration
 User Programmable Probe Molecule Database

iG C A N A L Y S I S S O F T W A R E

 Quick and Easy Data Plotting

 Raw Data Analysis

 Dead-Time Correction

 Surface Energy

 Heat of Sorption

 Isotherm Plotting

 %RH / Flow Rate Plot

 Performance Test

 Elutant Properties Database

Example plots generated using the IGC analysis software running under Microsoft Excel
 S M S iG C I N S T R U M E N T S P E C I F I C A T I O N S
 Standard Column Oven
Dual column aluminium block with thermoelectric
heating and sub-ambient cooling.
Temperature range 5°C – 120°C with 0.1°C stability
 Sample Columns
300mm x 6mm o.d. dimethyldichlorosilane treated
glass. Internal diameters 2mm, 3mm and 4mm
 Probe Molecule Oven
Forced air circulation type.
Temperature range ambient+5°C – 50°C
(dependent upon probe molecules used)
 Probe Molecule Injection
Fixed volume injection loop with electronic mass
flow controllers. Concentration range 0.02 – 0.95
p/pº (dependent upon probe molecules used)
Fig. A SMS iGC Instrument Reproducibility
For more information on any of the following please contact us:
 iGC Sample Analysis
 iGC Literature Database
 iGC Application Notes
 iGC Product Demonstration
WORLDWIDE
Surface Measurement Systems Ltd
3 Warple Mews, Warple Way
London W3 0RF
Tel: +44 (0)20 8749 4900
Fax: +44 (0)20 8749 6749
email: igc@smsuk.co.uk
www.smsuk.co.uk
Design: Kingfisher Design • Photography: Michael Owen • Illustrations: Andrew Green
 Customised Column Oven on request
 Standard Detectors
Thermal Conductivity (TCD) and Flame Ionisation
(FID) in series.
 Instrument Reproducibility
Specific component of surface energy <3% standard
deviation.
(See Fig. A below for 12 consecutive measurements
on the same column packed with paracetamol)
 Column-to-Column Reproducibility
Specific component of surface energy <4% standard
deviation.*
(See Fig. B below for single measurements on
22 different columns packed with paracetamol)
* For a homogeneous material
Fig. B SMS iGC Column-to-Column Reproducibility
 SMS Seminars and Workshops
 DVS – Dynamic Vapour Sorption
 VGI – Vapour Generator Instrument
 Confidential Consultancy
USA and CANADA
Surface Measurement Systems, NA
s
m
s
2222 South 12th Street, Suite D
Allentown, PA 18103
Tel: (610) 798 8299
Fax: (610) 798 0334
email: igc@smsna.com SURFACE
www.smsna.com MEASUREMENT
SYSTEMS