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Gas Chromatography
Ray E. Clement*
Ontario Ministry of the Environment, Laboratory Services Branch, P.O.Box 213, Rexdale, Ontario, Canada M9W 5L1
Francis I. Onuska
National Water Research Institute, Canada Centre for Inland Waters, Burlington, Ontario, Canada L9R 4A6
Gary A. Eiceman
Department of Chemistry, New Mexico State University, Las Cruces, New Mexico 88003
Herbert H. Hill, Jr.
Department of Chemistry 4630, Washington State University, Pullman, Washington 99164
INTRODUCTION
This review of fundamental developments in the field of
As for
the previous review of this series, the principal method of
literature review was by use of the biweekly Chemical Abstracts Service CA Selects for GC. Added to the coverage this
time are recent developments in GC/MS. Again, CA Selects
for Mass Spectrometry were employed for the literature review. To reflect the increasing work in serially coupled column
GC and in HPLC/GC, these areas are discussed with multidimensional GC under the new heading of multicolumn
chromatography.
The principal developments in liquid phases and solid
supports relate to their manufacture and use to improve selectivity for more directed separations, while liquid crystals
have gained acceptance as unique phases for certain applications. Liquid phase theory was used to develop predictive
tools for PTGC based on isothermal data bases. Less work
was reported concerning structure prediction from retention
data, while surprisingly little work was performed in the area
of solution thermodynamics. Supercritical fluids continue to
be extensively studied as were detectors for SFC,including
gas chromatography (GC) covers the years 1986-1987.
0003-2700/88/0360-279R108.50/0
SFC/MS. Important new work was also performed in the
areas of serially connected columns and in GC optimization
on a theoretical basis. As observed in the previous review in
this series, FT-IR continuesto receive a great deal of attention
as a GC detector. Although extensive applications of GC/MS
were reported, especially to biomedical and biochemical
problems, there were few fundamental developments in the
now well-established GC/MS technique.
COLUMN THEORY AND TECHNIQUES
A monograph describing the properties of adsorbents and
catalysts has been published by Paryjczak (Al), an excellent
text covering quantitative analysis of gas chromatographywas
written by Novak and Leclercq (A2), and a practical volume
by Grob (A3) describes methodological aspects of making and
manipulating capillary columns for gas chromatography. New
developments in gas chromatography and open tubular column chromatography have appeared (A4, A5).
The retention mechanism was studied for n-alkanes with
cross-linked poly(dialkylsi1oxane)stationary phases having
different alkyl chain lengths (C8to C18). Model stationary
phases were prepared with these phases and the specific re0 1988 American
Chemical Society
279 R
GAS CHROMATOGRAPHY
tention volumes of the analytes measured within the range
of 8 to 160 "C. The thermodynamic calculations indicate that
bulk dissolution appears to be the dominant mechanism for
their retention within these stationary phases (A6). The
distribution of elution peaha e ressed in Gram-Charlier series
were derived by means of M3ing's transformation for OTC
gas chromatography. The effect of pressure drop on parameters such as skewness was also discussed. For a linear nonideal chromatographic process, the skewness of a peak is
inversely proportional to the square root of the number of
theoretical plates ( A n . Dose (A8) investigated the computational simulation of temperature programmed GC behavior
of two series of analytes. The approach presented accounts
for both retention time and peak width behavior over diverse
temperature programs, Simulation accuracies are generally
1%for retention time data and 10-15% for peak width data.
The isothermal retention time data used as input are most
conveniently reduced to two quantities S, and H,,which are
proposed as a new claw of retention indices. A technique using
inverse GC for accurately measuring polymer-solute diffusion
coefficients was developed by Pawlisch (A9). The validity of
the technique was demonstrated by measuring the diffusivity
and activity of benzene, toluene, and ethylbenzene in polystyrene between 110 and 140 "C. The diffusion coefficients
obtained were consistent with existing va or sorption measurements. Leclercq and Cramers (AIO)gmonstrated that
for a given separation problem, vacuum outlet operation of
columns with a constant inner diameter always yields the
shortest analysis times under minimum plate height conditions. The comparison of vacuum vs atmospheric outlet operation is broadened to columns with different dimensions.
It appears that vacuum outlet operation is beneficial only in
terms of speed of analyses, if low maximum plate numbers
are required. The gain in speed of analysis is more pronounced
for wide-bore than for narrow-borecolumns. Characterization
of peak asymmetry with overloaded capillary columns based
on the solution of the mass-balance equations with a parabolic
expansion of the isotherm equation is in ood agreement with
the experimental peak profiles observe! ( A l l ) . The asymmetry depends greatly on the magnitude of the second derivative of the isotherm at the origin. It is due to overloading
and is independent of column length and flow rate. It increases with decreasing column diameter and with decreasing
film thickness. Thermodynamic functions such as heat of
adsorption and entropy of analytes were determined for two
bonded stationary phases by Lu et al. (A12). The reaction
between these functions and surface properties and resolution
performance of the bonded stationary phases were discussed.
Purnell et al. (A13) discussed theory and practice of coupled
columns of any kind. An example is presented of its use in
the optimization of a sample analysis with serial columns
which further establishes the quantitative validity of the
theory and illustrates its practicality and simplicity in use.
Guiochon and Gutierrez (A14) derived an equation for the
prediction of the plate height on a serial combination of capillary columns in GC. The equation together with an
equation for the apparent capacity factor can be used to
optimize the system parameters in resolving a mixture.
Procedures are described (A15) for the calculation of programmed temperature GC retention times, elution temperatures, retention indices, and two kinds of equivalent temperatures from isothermal data. These procedures involve
the determination of upper integral limits using numerical
integration and root-trapping methodology. Computer programs were written for both single ramp/multiplateau temperature programs. Experimental verification of the theory
of serially coupled GC columns indicates it to be entirely valid
and free of all assumptions other than that of carrier gas
ideality (A16). Selectivity tuning in OTC GC is presented by
Sandra et al. (A17). Selectivity tunihg can be performed in
three different ways, namely by synthesizing a tuned stationary phase, by mixing the basic phases, or by coupling
OTCs of different selectivities. Pretorius and Lawson (A18)
derived equations to predict the extent to which the sample
size may be increased, without decreasing the column performance by stationary phase focusing at subambient temperatures. Berezkina et al. (A19) discussed dynamic and
impulse chromatographic methods for the e uilibrium study
of heterogeneous reactions in gas-condense phase systems.
Nygren and Olin (A20) derived equations for predicting the
Et
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ANALYTICAL CHEMISTRY, VOL.
60.NO. 12, JUNE
15, 1988
results of exponentially flow programmed separations in gas
chromatography. Zolotarev et al. (MI)derived equations for
calculatin parameters in a capillary column formed from two
coaxial cyknders. Ceulemans (A22)evaluated the correlation
between column efficiency, resolving power, and analysis time
based on the quasi-linear relation between peak width and
retention times. On the basis of the equations derived, a much
more rational choice of columns and operating conditions
becomes possible.
High oven temperature on-column injection at column
temperatures well above the boiling point of the solvent, is
highly attractive for rapid analyses at elevated temperatures
(A23). Movements of the solute within the column inlet are
described, from which technical requirements are derived.
Avoidance of peak dmbrtion is also discussed (A24).Roeraade
(A25) discussed the advantages of the at-column injection
technique which includes quantitative transfer of sample, no
dead volume, and direct transfer of sample to a narrow bore
column or a precolumn. The application of the cooled needle
technique to split and splitless samplin onto OTCs to simulated distillation analyses was describe by Schomburg and
Haeusing (A26). Boeren and Gerner described an automatic
sample introduction onto narrow bore columns with a splitter
as well as the splitless injection of both solids and gases (A27).
The speed of analysis in OTCs can be substantially increased
by reduction of the column inner diameter. However, special
demands are then posed upon instrumental design. The
sampling system is highly critical because it has to be capable
of delivering small injection bandwidths which must be compatible with the column inside diameter (A%). A simple back
flushing, peak-cutting method was developed for the determination of trace components present in the tail of a major
component peak by Guan et al. (A29).Alexander et al. (A30)
described a method for coupling glass and fused silica OTCs
by using PTFE shrinkable tubings. Kaiser et al. (A31) reviewed current status of high-resolution column technolo
for GC. Ettre (A32)reviewed the interrelations between t u E
diameter and film thickness, their influence on the efficiency
and resolution, and their influence on sample capacity in
OTCs. Large diameter OTCs in GC analysis provide the
packed column chromatographerwith a simple route to higher
resolution GC. The columns seem fully compatible with all
common modes of detection (A33). The theory that predicts
the retention time, retention temperature, and peak width for
any kind of multistep temperature programming and the
principle of optimization is described by Lu et al. (A34). The
optimization of GC temperature programs using simulated
retention times and peak widths is described by Dose (A35).
A time/resolution compromise term is included in the chromatographic response function, and the effects of changing
the weight of that term are investigated. Convergence to the
experimental optimum temperature program is demonstrated
in one case by searching the setting space about the determined optimum. Freeman and Jennings (A36) optimized GC
separations based on the use of Stationary phases specifically
designed to maximize solute alphas. Selectivity can be further
tuned by differential variations in the carrier gas velocity
through dissimilarly coated coupled columns or t@mperature
variations in columns of at least moderate polarity. Hyver
and Phillips ( A 3 9 evaluate chromatographic theories for
enhancing resolution, speed, and sensitivity in HRGC and
HRGC/MS. Optimum performance of HRGC columns as a
function of tube diameter and film thickness under various
operating conditions was studied (A38) and a computer program was written for calculation of H-u curves and minimum
analysis time. Saxton (A39) describes a simultaneous parameter compensation in the replication of programmed GC
retention measurements. Golay (A40)discusses the problem
of optimizing the capacity ratio of an OTC for a selected
presumably most critical component, and it is considered as
a function of the diffusion time in the stationary phase. The
essential column parameters are derived for given inlet
pressure and analysis time. A double advantagecan be derived
from the use of high inlet pressures. Lin et al. (A41) described
conditions to select the optimal operation conditions for GC.
Basic software is described to obtain the whole imitating
chromatogram at any given temperature and to predict the
peak's separation in relation to temperature. Optimization
of stationary phase selectivity for the GC separation of C
cyclic and aromatic hydrocarbons using squalane and liquij
d
GAS CHROMATOGRAPHY
Ray E. CWnml la a Research Sdsnlbt wlth
me Ontarb M i n W of Envlnnment. Labaatwy savlces Branch. tie graduated wlth hla
Ph.0. degree hom me University of Waterloo h 1981. Or. Clement has taylht under- ;
graduate courses on GC technlqws and insbYmentation and is coau3horlng a baak on "
computerized GCIMS. His principal ~emarch areas invoke the uses of GC and
~
of toxic organic substances In the environment. which includes the chlorinated dibenzo-pdioxlns and dlbenrafurans. or.
Clement cumen9 serves on the Edllorlal
Board of Chemosphere.
on SIMCA 3B algorithms was evaluated by Onuska et al.
(A45). The objective of utilizing SIMCA 3B was its evaluation
for a possible identification, classification, and categorization
of Aroclors in environmental samples (A46). Parameters
affecting the quantitative performance of cold on-column and
splitless injection systems were evaluated by SneU et al. (A47).
Analytical results were evaluated as based on the interlaboratory reproducibility of gas chromatographic data obtained
with capillary columns by Stoev (A48). The study was carried
out on a mixture of n-alkanes.
LIQUID PHASES
F r a h 1. Onuska is a Research Sclannst
at
Nalbnal Water Research Insthie in
Burlington. Omarb. tie recelv~dhi8 DIP.
Eng. diploma from Slovak Technical Unhrershy. Bratislava. hls M.S. degree from Czech
Technological Unkerslty. Prague. and his
Ph.0. t o m Purkyne Unkersily. Bmo. For
me last 13years he has headed B gas c h r ~
matcgraphy and OClMS laborata1 the
Analytical Mamods D~IsIoII.Canada centre
fa Inland Waters. HIS research imerests
are in envtanmental organic trace analytkai
chemishy. Including development of inshumentation and methodology with an emphasis on toxk aganic pciiutants in water. sed!WnI. fish. and wildlife. Onuska currently Serves on the Advisory Board of
ma Jownal Of H7gh Resolution Chmmsfography and Chromarography Cornmunlcsms.
Oaq A. E k m a n is an As60~lateProteo~ar
of Chemistry st New Mexico State UnkersC
l y in Las Cruces. NM. He received hls B.S.
degree in 1974 ham West Chester State
University and his Ph.0. degree in 1978 at
me unkersity 01 Colorado. He was a postdoctoral fellow al Unkersity 01 Waterloo,
Ontario, horn 1978 to 1980. His research
interests are In selaclwe chemical interaclkm in chomatography. separaUon of c o m
plex chemlcal mixtures. envlronmental
chemistry of hazardous organlc compounds.
and ion mabilw spectrometry. He has
taught instrumentation and q~antltatlve
analysis at me undergraduate level and
elechonks and mparaHonslmass specnome
HHb.rt H. Hill. Jr.. is a FTotessor of C h e m
lstry at Washington State Unkerslty where
he directs an ac1Ive remarch program in
ma devek.pmem of insbumematbn for trace
agank anabsb. His resewch interests include gas chromatwphy. supercMica1 num
chromatography. bn mobility spectrometry,
ambient presswe bnizatlon sources. and
mass spectrometry. HB r e ~ e i v dhis B.S
degree In 1970 from Rhcdes College in
Memphis. TN. his M.S. degree In 1973 trom
the University of Missouri. Columbia. MO.
and hls Ph.0. w
e
e in 1975 trom Dalhousle university. &Inax. ~ 0 v ascotla. cenada.
In 1975 he was a poa&ctorai teliow at the
University of Waterlw. Ontavb. and in 1983-1984 he was a visnlng prafes8oT at Kyoto Unkersity. Kyoto, Japan. He has been on the faculty at Washington state university since 1978.
I
'
crptal glass capillary mlumns in series is described by Krnpcik
et d (A42). The optimization criterion used was derived from
the Kovats retention indices of the solutes. The use of
multichannel chromatographic detectors that produce spectra
characteristic of the eluents permits the deconvolution of
partially overlapping peaks without any assumptions about
peak shape or prior knowledge of the spectra of the individual
compounds (A43). Crilly utilized numerical deconvolution
of gas chromatographic peaks using Jansson's method (A44).
The maximum peak amplitude of the instrument and peak
nonnegativity serve as constraints to improve the peak estimation. Superresolution is achieved without significantly
degrading the chromatogram signal-tc-noise ratio. Application
of chemometricz in homologuespecificanalysis of PCBs based
In general, advances with liquid phases in gas chromatography were aligned toward materials that exhibited specific
solute-solvent interactions for improved resolution over
general dispersion forces. Several different types of stationary
phases were investigated and included liquid crystals ( B I - B ) ,
modifiedsiloxanes (B9-B12),crown ethers (B13,B14), organic
salts (BZ5-B17), and other polymers (B18, B19). The emphasis with liquid crystals was on separation of positional or
geometric isomers which was influenced by ratios of lengthto-breath dimensions in solutes (B3-B6) and terminal or
lateral substituents in the liquid crystal phases ( 8 4 ) . Separation factors were dependent more on liquid crystal structure
than on nematic range (BO, thermooptical techniques were
combined with chromatographic methods for improved
characterization of liquid crystals ( B n ,and binary mixtures
of liquid crystals were evaluated by using thermochemical
parameters (B8). With polysiloxanes, methods for functional
group elucidation in existing columns were described (B9)and
a family of polar alkyloxyphenyl derivatives were evaluated
(BZhB12) for high-temperature separations of analytes based
on specific intermolecular interactions. Polarity was also
introduced into bonded capillary columns through crown
ethers that were chromatographically comparable to Carbowax-20M (813)and exhibited thermal stability (B14). Specificity was added to liquid phases with liquid melts of salts
including alkylated ammonium tetrafluorohorates (B15) or
thiocyanates (B16) and chromatographic aspects of such
substances were reviewed (B17). Dispersive forces were weak
in salt-solute interactions and dipole moments were better
indicators of retention. Other developments with liquid phases
were made by using more conventional polymers and included
assessment of polyethylene in two forms (low density branched
and high density linear) for separations of alkenes and aromatic hydrocarbons (B18)and simple addition to OV-101of
N-acyl capped valinamide for chiral amino acid separations
(B19).
The chemistry of liquid phases for GC was explored for the
effects of cross linking in bonded phases (BZO-BZZ),identification of structural rearrangements in stationary phases
(B23),degredation and oxidation of liquid phases (B24,B Z ) ,
synthesis of materials for use in 400 "C+ columns (B26),and
modification of phases with complexes or polar moieties (B27).
Cross-linking was probed for contribution to immobilization
of Carbowax-20M (BZO),retention by adsorption at the gasliquid interface (B21),and immobilization of chiral stationary
phases (822). Abnormally large retention volumes for polar
solutes with certain polyesters (823) were attributed to
structural rearrangements that were temperature induced.
Consequences of temperatures were also examined with
analysis of degredation products from immobilized silicone
phases (824). Cyclic compounds were found in both SE-52
and SE-54 while the cyanopropyl(pbeny1)siloxy unit in
OV-1701exerted a destabilizing effect on the liquid phase.
In a remarkable development, a column containing OV-17was
heated under oxygen carrier gas flow and a new phase was
produced which showed improved peak symmetry of many
polar compounds with no ill effect on nonpolar compounds
(825). Changes in the retention index and a reduction in
polarity via the McReynolds values were observed. A final
investigation related to temperature was the report of methyl
polysiloxanes in AI-clad flexible fused silica capillary columns
which were suitable for programming to 440 "C with separation of alkanes comprised of carbon numbers from 90 to 100
(B26).
Specific interactions were also central in the development
of liquid phases modified with lanthanide Bdiketonates for
complexation interaction (827) and in the reports on ligand
ANALYTICAL CHEMISTRY. VOL. 60, NO. 12. JUNE 15, 1988
281R
GAS CHROMATOGRAPHY
exchange GC (B28, B29) commonly associated with liquid
chromatography. In ligand exchange GC, a copper stearate
stationary phase was combined with an ammonia-containing
mobile phase for separation of dialkyl (B28) and alkyl aryl
(B29)disulfides. Temperature and mobile phase composition
were adjusted to effect separations. Thiol-bonded silicas were
used to retain copper ions that interacted specifically with
olefins and aromatic hydrocarbons through .rr complexes (B30).
Two developments in this subject were not easily inserted
into categories discussed and will be mentioned individually.
The organosilicon chemistry for preparation of capillary
columns was reviewed (B3I) and the International Union of
Pure and Applied Chemistry issued guidelines in six categories
for characterization of liquid phases by using uniform procedures (B32). This last reference should greatly facilitate
comparisons of new liquid phases in a systematic framework.
SOLID SUPPORTS AND ADSORPTION
Natural materials were emphasized in recent studies on
solid supports for GC separations and greatly overshadowed
the use of synthetic organic polymers. In accord with patterns
from the last decade and with developments in liquid phases,
modifications of materials for improved specificity were emphasized and were based on mostly empirical models of GSC
interactions. Particularly noteworthy is the huge interest from
European investigators, all of which were not included here.
Studies on adsorptive and chromatographic properties of
zeolites were directed toward effects from cations (CI-C3) and
water in the carrier gas ((24). Small hydrocarbons were the
central concern in most of these reports and separations were
improved with addition of water vapor to the carrier gas.
Zeolites modified with alkali or alkaline-earth metal deposits
exhibited trends in retention for metal families or groups
which differed between saturated and unsaturated hydrocarbons ( C l ) . Cation-hydrocarbon interactions were recognized as dominant absorptive mechanisms in N-A-type zeolites
(C2). The adsor tion of a binary mixture of carbon dioxide
and water on C d zeolites was successfully modeled to existing
equations of adsorption (C6). Methods were described to
chromatographically determine OH and adsorbed water on
Zeolite surfaces ((75).
Chemical modification of other conventional adsorbents was
also a major thrust for nonorganic synthetic materials and
included modified silica (C7-C1 I ) , altered carbon black
(C12-C14), titanate-coupled aluminas (C15),plasma-modified
silochrome and carbon black (C16),and volatile modifiers with
supporting theory (CI7). A common theme for all these investigations was user-directed selectivity in adsorption or
separation using specific analyte-sorbent interactions introduced through the modifying process or altered material.
Gas-solid chromatography was used to explore the properties of two other natural materials not usually associated
with GSC such as lactose (C18),cyclodextrin (C19),cellulose
(C20), asbestos (C21), and salt-modified adsorbents (C22).
Cyclodextrin was used as a stereospecific material for resolution of substituted aromatic hydrocarbons.
Synthetic organic polymers were the subject of a few studies
including thermodynamics of retention for alkanes alcohols
on Poropaks (C23),modificationsof styreneDVEi ( 24-C27),
and chromatographic effects from bead sizes (C28). These
studies were aimed a t further elucidating the properties of
porous polymers such as effects of inert diluents, number of
methylene groups in homologous series of adsorbates, and the
consequences from size distributions among various batches
of porous polymers. Other organic compounds used as adsorbents were tributylamine salts (C29),molten salts (C30),
and metal-vinylpyridine complexes (C31).
A very few physicochemical studies were made as evident
from only three reports on the measurement of effective
diffusion coefficients in porous packing (C32),determination
of the surface acidity of solid catalysts (C33),and sorptiondiffusion in molecular sieves (C34). Interesting applications
of GSC to quantum symmetry restrictions in homonuclear
diatomic molecules (C35)and target factor analysis (C36) were
noteworthy. Otherwise, theoretical treatments in GSC were
weakly represented and eclipsed easily in numbers alone by
applied GSC not cited here.
Two articles of general interest were a historical account
of Schuftan’s work in GSC (C37) and a review of adsorbents
L
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ANALYTICAL CHEMISTRY, VOL. 60, NO. 12. JUNE 15, 1988
(C38). An interesting combination of GSC with GLC can be
found in two reports of capillary columns packed with barium
sulfate (C39, C40) for improved resolution of positional/
substitutional isomers of olefins and aromatic hydrocarbons.
SORPTION PROCESSES AND SOLVENTS
In comparison to the last review in 1986, a surprising
amount of activity has occurred in this subject and included
some significant advances in describing the molecular basis
for chromatographic processes. However, the breadth of investigations was narrow and nearly 85% of all of references
abstracted in this category can be placed in equal numbers
into two divisions, namely retention indices predictions and
thermodynamic measurements in GLC. Particularly noteworthy developments have been occurring principally in
laboratories from Europe and Asia. Discussion will be organized into the three subjects of retention indices, thermodynamic aspects in GC, and general or isolated subjects.
One issue concerning retention indices @I) is the prediction
of RI values for temperature programmed conditions using
data from isothermal chromatography (01-08). Advances
have been centered on the development of appropriate
coefficients €or use in linear equations. Presently, precision
is only slightly better than 0.5 unit for predicted programmed
RI. Predictive capabilities for solution processes with a slightly
different emphasis were addressed through the use of mathematical models for calculation of RI units under completely
new temperature or column conditions (09-021). This was
commonly approached by using a single family of compounds
for preparation of equations with physicochemical parameters
or with solute-solvent energies of interactions. Compounds
investigated since 1986 included aliphatic and aromatic hydrocarbons (09-012,015, 0 2 0 , 0 2 0 , alcohols (022), carboxylic acids or esters (013, 0 1 7 ) , quinoline bases (014),
ketones (D16),dialkyldormamidines(DI9),amines (020),and
nitroaromatic hydrocarbons (018). These investigations were
not restricted only to relatively uncomplicated methylsiloxanes
but also included a wide selection of medium to highly polar
phases. Examples of each approach were models from parameters such a boiling point, refractive index, or others ( 0 1 1 ,
0 1 2 , 0 1 6 , 0 2 3 , 0 2 4 )and models from molecular moieties or
interaction energies ( D 6 , 0 1 2 , 0 1 4 , 0 1 7 , 0 2 5 ) .Finally, the
effects from concurrentmechanisms of retention were explored
(026) and limitations on attempts to model and predict retention were critically reviewed (027).
An equal number of studies were devoted to the determination of terms of interest in physical chemistry using GLC
and included activity coefficients (028-031 ), interaction/
solubility parameters (032-035), solute-solute interactions
(036),thermodynamics in binary liquid crystals (037,0 3 8 ) ,
free energies (D39),and partition coefficients (040). The goal
in each of these investigations was to explore solute-solvent
processes by using the avantages of speed and convenience
of GC. Other equilibria such as formation of complexes (041)
or solubility in complexing solvents (042)were also explored
by using GC. Perhaps the most remarkable development
recently has been the adaptation of advanced multivariant
data analysis to address longstanding difficulties in chromatography, namely systematic interpretation of large amounts
of retention information (043-047). These techniques may
become powerful tools in recognizing various molecular contributions to retention mechanisms (044) and should be
considered seriously in future investigations. Other pertinent
articles were found in the determinationof nonadditivit (048)
and the role of kinetic coefficients in retention (04931a description of thermodynamic studies using volatile stationary
phases (050),a mathematical determination of dead time (i.e.,
void volumes (D51)),a discussion of the choice of concentration scales ( 0 5 2 ) ,a proposed extension of the Kovats RI
system (053),a new liquid phase classification scheme (054),
and a brief review of thermodynamic measurements in GC
(055).
In the category of general subjects, the influence of column
effects as related to stationary phases was also considered for
chromatographic im ortance from several perspectives.
Studies included the [ehavior of molecules a t interfaces or
thin films (i.e., mixed retention mechanisms (056-060)),
overload phenomena (D61),liquid phase swelling (062),and
thermal stability of liquid phases (063). A general critical
GAS CHROMATOGRAPHY
review on liquid phase selection was given by Yancey (064).
Liquid organic salts were examined from consideration of the
anion effects on solute retention ( 0 6 5 ) and retention mechanisms ( 0 6 6 ) .
OPEN TUBULAR COLUMN GAS
CHROMATOGRAPHY
The capillary rise method was used to obtain contact angle
measurements on untreated fused silica and fused silica
treated with a variety of deactivating reagents. The contact
angle data were used in the construction of Zisman plots which
allowed characterization of the wettability of the surfaces by
their critical surface energies. The wettability of raw fused
silica was found to be widely variable which adversely affects
attempts to fully deactivate the surface. Hydrothermal
treatment of the fused silica with HNOBwas found to be
adequate for cleaning and hydroxylating the silica surface so
as to allow complete deactivation. Simple silylating reagents,
cyclic siloxanes, and polysiloxanes covering a wide range of
polarity were used and evaluated as deactivatingreagents (El).
Berlizov et al. (E2) studied properties of Pyrex glass and
quartz capillary columns before and after deactivation with
OV-101. Heeg (E3)observed various capillary materials under
the electron microscope and a comparison was made with
those capillaries leached with inorganic acids. Berezkin et al.
(E4)investigated the role of adsorption at the stationary phase
interface in capillary columns prepared with cross-linked and
non-cross-linked phases. It seems that deactivation of fused
silica tubing is still causing significant problems especially with
more polar stationary phases. Wolley et al. (E5) described
reaction conditions for surface deactivation of fused silica
columns with polymethylhydrosiloxanes, and phenylhydrosiloxanes (E@. Van de Ven et al. (E6,E7) studied deactivation
processes with silazanes. Ogden (E9) used tetrakis(3-cyanoethy1)tetramethylcyclotetracyclosiloxanefor GC and supercritical fluid chromatography columns. Markides et al. (E10)
described a method for surface deactivation of fused silica
capillary columns with a cyanopropylhydrosiloxane reagent
at 250 "C. A procedure was developed to remove acidic impurities that are present in polar stationary phases. Wolley
et al. ( E l l )deactivated small diameter fused silica columns
with a mixture of polymethylhydrosiloxanes and several low
molecular weight organosilicon hydrides. Rohwer et al. (E12)
deactivated nickel tubing by chemical vapor deposition of silica
from silane gas and subsequent treatment with cyclooctamethyltetrasiloxane. The technique of spontaneous coating
of capillary columns employing liquefied butane and ethylene
chloride as solvents of the stationary phase was described by
Janak et al. (E13,E15). Grob and Grob (E14)provided hints
for statically coating capillary columns. The hints include
ressurizing before pumping as a repair technique for
greakthrough by using a compressed gas at 4-5 bar for 15 min
to every freshly filled column, the addition of methylene
chloride to pentane solvent to reduce pumping time, and the
use of vacuum reservoirs as vacuum source instead of the water
pump.
Wickramanayake and Aue (E16)described preparation of
a bonded polyoxyethylene phase. There is circumstantial
evidence the nonextractable layer is held by multiple hydrogen
bonding. Horka et al. (E17) described a procedure for the
preparation of an immobilized stationary phase based on
Carbowax 20M for capillary column GC. The stationary phase
cross-linking was carried out with Desmodur N 7 5 , pluriisocyanates. The properties of the prepared capillary columns
are compared. A simplified method for Carbowax 20M and
40% dicumyl peroxide was published by Bystricky (E18).
The efficiency of fused silica OTCs coated with thick films
of polyphenylmethylsiloxane was compared to thin apolar and
medium polarity coatings. Experimental data demonstrate
a significant loss in chromatographic efficiency of thick films
of medium and polar siloxane stationary phases. The low
diffusion.coefficients in the liquid phase is responsible for this
behavior. The influence of the temperature and the nature
of the efficiency was also studied (E19).
Blum (E20-E22) provided detailed procedures for the
preparation of inert and high-temperature apolar, moderately
polar, and polar glass capillary columns using OH-terminated
polysiloxane stationary phases. Intensively leached silica
surfaces with OH-terminated phases provide a new way of
producing capillary columns with substantially increased inertness and thermostability. All processes involved in their
preparation are discussed, and detailed working directions are
given for the following phases: OV-1701-OH, OV-31-OH,
OV-61-OH, OV-17-OH, OV-240-OH, and PS-347.5 and PS086. There is no doubt so far thar the principle of terminal
silanol groups is applicable to all silcone phases and may
replace the traditional end-capped stationary phases in the
future. Duquet et al. (E231 synthesized a cyanopropylsilicone
stationary phase for fused silica OTCs. Wide bore columns
coated with this phase were tested with respect to efficiency,
activity, and thermal stability. The selectivity of the phase
for fatty acid methyl esters is very good. A simple method
is described by Eddib et al. (E24) for preparing thermally
stable and highly efficient capillary columns coated with highly
polar cyanosilicone phases over previously deposited silica
layer. Aerts et al. (E25) described preparation of a narrowbore (50 pm) and wide-bore (320 pm) OTCs for immobilized
cyanopropyl-substituted silicones containing 60 and 88 %
cyanopropyl substitution. The polarity of polar columns
appeared to be greatly dependent on column temperature and
is completely different for wide and narrow bore columns.
Immobilization of stationary phase f i i s using y radiation was
studied by Borek et al. (E26). Columns were irradiated with
2-10 Mrad dose to study the immobilization of stationary
phases. An immobilization of 83 to 100% was obtained with
SE-30 and SE-54 but less than 14% for Carbowax and Silar
1OC. Chuang et al. (E27) achieved immobilization of OV-1701
vinyl and OV-225 vinyl using ozone as an initiator. Farbrot
et al. (E28)polymerized stationary phases in 12-50 pm open
tubular columns used in LC and GC. Melda et al. (E29)
discussed thick film capillaries and their applications for
process gas chromatography in comparison with packed
columns.
SUPERCRITICAL FLUID CHROMATOGRAPHY
The present state of supercritical fluid chromatography
(SFC) has been reviewed by many authors (FI-F7).The
principles, instrumentation, and applications of SFC are
discussed.
Schwartz et al. (F8)compared separation efficiency and
speed of packed and capillary columns for SFC by using plate
height equations and van Deemter plots. Three hypothetical
molecules that require progressively higher fluid density for
their migrations were selected. When solvent viscosities and
solute molecular weights are large, packed columns appear
to have a distinct advantage over capillary columns with regard
to the number of plates generated per unit time. A similar
subject was discussed by Caude et al. (F9).
The preparation of immobilized polysiloxane coated on
packings or capillaries was discussed with regard to efficiency
(FIO),speed, pressure drop (F11),
deactivation, polarity and
thermal stability (F12),and kinetic column effects and
chromatographic performance (F13).Unified molecular theory
of chromatography and its application to supercritical fluid
mobile phases have been described by Martire et al. (F14).
Hydrodynamic description of SF flow through the porous
packing of analytical high-performance columns is founded
on Darcy's law, the Peng-Robinson equation of state, and
viscosity correlation. This model fits results with a very good
accuracy for both pressure drop of several eluents such as COz,
NzO, CF3H,CBrF3,and SFs through various types of columns
and eluent residence time measurements. These results show
that it is possible to describe supercritical fluid properties with
relatively simple correlations. Fields and Lee studied effects
of density and temperature on efficiency in capillary SFC
(F16).Yonker and Smith (FI7)investigated effects of density
on enthalpy and entropy of transfer for SFC. The results
demonstrate the independence of enthalpy and entropy of
transfer with supercritical fluid density during chromatographic separations. The simultaneouscalculation of pressure,
density, and temperature profiles for packed columns used
in SFC is described (F18).The results show that pressure
profiles over packed columns are approximately linear. The
density decreases along the column length and so does the
temperature of the eluent. Both the variations in density and
in temperature are enhanced by using smaller particles or
higher flow rates. The pressure- and the temperature-dependent behavior of the chromatographic parameters for
ANALYTICAL CHEMISTRY, VOL. 60, NO. 12, JUNE 15, 1988
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GAS CHROMATOGRAPHY
binary eluent mixture containingpentane and 1,li-dioxane was
studied (F19). Yonker'et al. (F20) studied effects of pressure
on retention in SFC and an effect of solute concentration on
retention. The optimum pressure conditions can be obtained
for maximum resolution of two solutes during pressure programmin or isobaric separations (F21). Christensen (F22)
describe8 on-line multidimensional chromatographic separation, which makes use of the unusual properties of supercritical mobile phase. Leyendecker et al. (F23, F24) studied
properties of various low boiling eluents. Kuei et al. (F25)
assembled instrumentation that allows the use of supercritical
ammonia as mobile phase. In addition, the stabilities of
various polysiloxane stationary phases were examined. The
effects of modifiers in supercritical fluid chromatographywere
examined (F26-F28). With carbon dioxide as the primary
mobile phase, the modifiers investigated included methanol,
2-methoxyethanol, 1-propanol, THF, dimethyl sulfoxide,
acetonitrile, SF6,and Freon 11. Mourier et al. (F29) studied
the effect of the physical state of the supercritical fluid on
solute retention. French and Novotny (F30) evaluated xenon
as a unique mobile phase which is due to its optical transparency and is highly suitable for SFC/Fourier transform
IR spectrometry.
Various studies of retention processes in SFC with binary
(F32) and multiple gradienta by pro ramming eluent composition and temperature (F31) an pressure (F33) were
studied. They appear promising for extendin the range of
amenable separations. Similarly, retention an resolution in
density-programmed SFC were studied by Linnemann et al.
(F34). With pentane and 1,Cdioxane as a binary eluent
system and silica as the stationary phase, three-dimensional
network plots of capacity ratios, selectivities, effective plate
numbers, and resolutions for PAHs vs column temperature
and eluent composition at constant pressure were obtained
(F35). The dependence of reduced plate height on reduced
velocity in carbon dioxide SFC with packed columns was
studied by using the Knox model and supplementary coefficients with a parabolic dependence on velocity were added
(F36).
A sample introduction system for capillary SFC, which
allows the dissolution of the sample in the supercritical mobile
phase before being introduced into the column was described
by Jackson et al. (F37). The potential of such an injection
system was demonstrated but further developments are
needed to make the technique of practical utility.
Performance of capillary restrictors in SFC was examined
(F38).The transport of low volatility analytes is facilitated
by heating the fluid prior to the restrictor or, less effectively,
by heating in the restrictor. The successful transport and
detection of nonvolatile compounds by FID with SFC were
demonstrated. An integral restrictor for capillary SFC was
designed by Guthrie et al. (F39). The device is reproducible
and mechanically stable and can be easily altered to produce
a specific mobile phase flow rate.
The properties of a double-chamber pneumatically driven
piston pump (F40),syringe pumps, and reciprocating piston
pumps in SFC were compared (F41). A computer-controlled
pumping system for SFC was designed based on a pneumatic
amplifier pump by Pariente et al. (F42).
A very attractive technique emerging from utilization of a
suitable supercritical fluid separation is supercritical fluid
extraction. Nagahama reviewed the principle, applications,
and future trends of this novel technique (F43). Saito et al.
(F44) reviewed supercritical fluid extraction (S46)and SFC
and their directly coupled systems. Gmuer et al. (F45) designed a prototype for direct couplin of SFE and capillary
SFC. Smith et al. (F46) discussed S#C, SFC/MS, and microscale SFE by supercritical ammonia combined with chromatographic methods. Campbell et al. (F47) studied semipreparative SFC which permits high-quality separation of
coal tar with easy solvent removal. Saito and Hondo (F48)
reviewed on the historical background and applications SFE
and SFC and their applications in food processing. Tanaka
(F49)reviewed the use of SFE in the pharmaceutical industry.
An elegant method for the application of SFC to environmental samples using SFE-GC/MS was published by Hawthorne et al. (8'50, F51). An apparatus and procedures for
direct coupling of SFE to capillary SFC was described by
Gmuer (F52). The method can be used for monitoring cheese
ripening, rancidity development in dairy products, and de-
d
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ANALYTICAL CHEMISTRY, VOL. 60, NO. 12, JUNE 15, 1988
tecting aroma defects in butter.
INSTRUMENTATION AND DETECTORS
Detectors and injectors for high-resolution capillary gas
chromatography were the focus of instrumental research and
development over the past two years. Of specific interest was
the quantitative introduction of mid to high molecular weight
components into high-resolution gas chromatographic columns. Also the explosion of supercritical fluid chromatography led to rapid developments in SFC detectors and instrumentation.
Sample Introductlon
As the efficiency of chromatographic columns have continued to improve, the importance of injecting narrow bands
onto the column while maintaining the quantitative integrity
of the sample has increased. Thus the improvement of oncolumn injection methods has received considerable attention.
Two designs for inexpensive on-column injedon were reported
( G l , G2). Althou h efforta were made to increase injection
volume, Grob an Neukom (G3) found that phase soaking
effects of large volume injections (e.g. 70 pL) reduced peak
areas from that expected in comparison with submicroliter
injections while Termonia et al. (G4) reported good quantitative data for large on-column injections and Lawson et al.
(G5)reported on an inlet which could handle up to 20-pL
injections with a 1% relative standard deviation. Along with
injection volumes, temperature effects were also investigated.
A multipurpose cold injector was reported which could not
only be used for on-column injections but could also be
modified for split s litless or solvent vented injections (G6).
Grob and Laeubi ?G7), usin two independent on-column
injectors, described technic3 requirements for on-column
injections into columns maintained at high temperatures.
To accurately control injection temperatures, Bruno and
Shepherd (G8) developed a miniature mercury contact switch
that could be placed inside the injector or other components
of a chromatograph. Another temperature control device to
aid injection was reported by Pretorius et al. (G9).With
operation on the principle of Joule-Thomson cooling, it can
be used for thermal focusing of volatiles in a capillary column.
Cryofocusing is, of course, a common aid in the injection of
volatile compounds. Kolb et al. (GIO)investigated this method
for sample enrichment during equilibrium headspace sampling.
Although direct injection techniques were employed using
sampling of volatiles from fluids was
a retention gap (GII),
commonly accom lished by stripping and trapping methods.
Both repetitive (812) and automated (G13)studies were reported. Novak and Cermak (G14) reported a method for
transferring substances from trapping columns into a gas
chromatogra h without affecting the conditions for injecting
sample stanlards through the common septum port. Other
novel transfer techniques have been reported as well.
Goldsmith (G15) reported the use of microwave desorption
and Pawliszyn and Liu (G16)described a sample introduction
method using laser desorption. Of particular interest was the
introduction of volatile samples into very small diameter
columns. Phillips et al. developed a method for thermal
desorption modulation (G17)while Van Es et al. (G18)
evaluated input bandwidths as a function of column diameter.
The most intense activity in research and development of
sample introduction methods over the past two years was in
the area of high molecular weight and polar compounds.
Standard techni ues such as pyrolysis continued to be investigated (G19,820)but more emphasis was placed on the
introduction of high molecular weight compounds without
thermal degradation. Bayona et al. (G21) discussed the advantages and disadvantages of standard vaporizing injectors
for high molecular weight introduction and Lawrence (G22)
reported a method for transferring high-boiling compounds
from sample adsorptiontubes. Considerable interest, however,
was shown for programmed-temperature injection (PTI)
techniques. With initial investigations primarily focused on
the determination of triglycerides (G23, G24),the use of PTI
proved promising. Reglero et al. (G25)have reported on the
optimization of the technique.
One driving force behind investigations into PTI was the
difficulties encountered when injection ports are maintained
d
GAS CHROMATOGRAPHY
continuously a t elevated temperatures. Complications from
septum decomposition are especially troublesome. Although
Skornyakov and Poshemanskii (G26)reported the development of a septumless injection device, supercritical fluid injections were also investigated to minimize high-temperature
problems (G27,G28). Typically, a supercritical fluid such as
C 0 2 was used to extract the sample from a solid matrix and
quantitatively transfer the extract through a decompression
chamber directly to the inlet of a gas chromatograph. Injection
via supercritical fluids was also accomplished after preliminary
separation of the sample by supercritical fluid chromatography. Levy et al. (G29)reported the development of this new
multidimensional separation technique with heartcut examples. Of course, if supercritical fluid chromatography is to
be used as an injection method for gas chromatography, injection methodologies for the supercritical fluid chromatography must also be considered (G30).
Liquid chromatography was also investigated as a method
for introducing compounds into a gas chromatograph. Of
primary concern in this interface was solvent elimination and
evaporation. Grob et al. (G31-G33)developed a method for
concurrent solvent evaporatibnin which they use the retention
gap approach. Raglione and Hartwick (G34)used a bundled
capillary stream splitter for solvent volume reduction. In a
related injection method, Rogelqvist et al. (G35)directly
coupled a liquid-liquid extractor to a gas chromatograph by
using segmented flow injection.
Two reviews were published that provided an excellent
overview of modern inlets for capillary gas chromatography
(G36,G37).
Detectors
As always, a number of excellent reviews on gas chromahas written
tographic detectors were published. Dressler (HI)
a comprehensive book covering selective detectors and Patterson (H2)compared the various methods of ionizing GC
effluents. Brinkman and Maris (H3)reviewed GC detectors
that were used with liquid chromatography and other general
reviews were also published (H4,H5).
Althou h investigations were reported that used catalytic
,
(H7,
H8),and thermal concracking b6)electrochemistry
the majority of research on GC detectors was
ductivity (H9),
focused in three areas: ionization, light absorption, and light
emission.
Ionlzatlon Detectors
For routine analytical quantification of components separated by gas chromatography, ambient pressure ionization
detectors remain the primary detection method of choice for
most analyses. This category of detectors includes the flame
ionization detector (FID), the electron capture detector (ECD),
the photoionization detector (PID), the thermionic ionization
detector (TID), and He ionization detector (HeID), and the
ion mobility detector (IMD) plus several miscellaneous ionization methods.
The FID continues to receive considerable attention. Recent research on the detector has been focused on efforts to
improve its sensitivity. Cool and Goldsmith (11)have reported
ionization enhancement of the FID with laser excitation of
CH. Using stilbene 420 in a dye laser that was pumped with
an argon-ion laser, they were able to achieve a 6% enhancement of the ionization reponse of methane in hydrogen. In
another study, Axner et al. (12)investigated laser-enhanced
ionization for 23 different elements in aqueous solutions with
ionization in an acetylene/air flame. Other methods to enhance performance of the FID have also been investigated.
Gonnord et al. (13)compared various electronic methods to
improve signal-to-noise ratio and Colson (14)has suggested
methods to improve the high-end linearity of the detector.
Flame ionization for the selective detection of Si-containing
compounds was also reported (15,16).
Mechanistic investigations of the ECD continue to produce
surprising and useful analytical results. Arguments for the
space-charge mechanism of electron-capture response were
presented in several papers by Aue and co-workers. Using
ac polarization of two commerical detectors and two lab-built
detectors as a probe for the mechanism, they achieved two
response maxima as they scanned the polarization frequency
from 10 to lo6 Hz (17). The low-frequency maximum was
attributed to cation-electron recombination within the plasma
while the high-frequency maximum was attributed to a migrating negative space charge. Analytically, ac electron-capture detection behaved similarly to unipolar detectors but it
was suggested that ac operation may have benefits for the
detection of weak electron-capturingmolecules. Confirmation
of the space-charge-based mechanism was demonstrated by
the development of an electron-capture detector which provided a current increase in response to electron-capturing
molecules (18). Supporting information for the heterogeneity
of charge distribution in the electron capture detector was
provided by a study of 63Ni0 range and backscattering in
confined geometries (19-111). In these studies it was found
that the majority of gas-phase ionization occurs within 4 mm
of the foil. No evidence was found for the very large range
estimates reported in the literature. In other ac potential
experiments, Baumbach et al. (112) found that superimposing
a high-frequencyac potential over the dc potential of an ECD
can provide orders of magnitude response specificity for some
compounds. The response of low electron affinity compounds
was also investigated by Valkenburg, Knighton, and Grimsrud
(113). Improved response for aromatic hydrocarbons using
positive ion stabilization and alkyl chloride sensitization was
reported and a kinetic model developed to explain this response enhancement. Chen et al. (114) reported on the importance of kinetics and thermodynamics, reviewing the kinetic model for the electron-captureresponse. Simmonds (115)
investigated photoemission from thin metallic films as a source
for thermal electrons. Wise et al. (116) reported the development of a multimode ionization cell that provides turnable
selectivity. By varying the internal pressure of an electroncapture-type cell from ambient to less than 1Torr, they could
operate the detector as a conventional electron capture detector, a low-pressure Ar ionization detector, and a crosssection ionization electron emission detector. A new derivatizing reagent for the ECD, pentafluorobenzyl p-toluenesulfonate, was reported which enables the determination of
bromide, iodide, thiocyanate, and nitrite by GC/ECD (117).
Other derivatizing reagents used with ECD were reviewed for
trace analysis (118). ECD detection was applied for the determination of total and free thyroxin in serum (119),mitotane
in plasma (120),and propafenone in biological fluids (121).
Investigations of the PID included high sensitivity studies
and optimization of the detector for gas capillary chromatography. Driscoll (122)reported the operation and performance characteristics of a PID with a cell volume less than
50 p L for use with capillary chromatography. The use of the
PID for the trace determination of volatile polar compounds
was investigated by Sung et al. (123)and Norlander and
Carlsson reported the detection of 70 fg of methadone (124).
Arnold et al. (125)also reported the use of a photoionization
detector with high sensitivity. Its uses for the detection of
purgeable halocarbons (126)and in recycle GC systems (127)
were investigated.
The TID, also known as the NPD, is thought to respond
to nitrogen- and phosphorus-containingcompounds by surface
ionization on heated alkali-impregnated sources. In a study
of the nitrogen mode of the TID using 36 compounds, Jones
and Grimsrud (128)report that thermal decompositionof the
analyte on the hot emitter surface followed by electron transfer
from the surface to one of the decomposition products was
the mechanistic model which best fit all the results of their
experiments. Patterson (129)reports that by the systematic
variations of each of three key parameters (the work function
of the thermionic emission surface, the temperature of the
thermionic surface, and the gas phase environment), thermionic detection can be expanded to a variety of operational
modes. Fujii and co-workers (130-133)have investigated the
ionization response of surfaces with a high rather than a low
work function for the detection of compounds eluting from
a GC. While much of the initial investigations of high work
function surfaces such as Pt and Re have been conducted with
trimethylamine, response for non-nitrogen-containing compounds such as the polycyclic aromatic hydrocarbons have
also been reported. Applications of the TID have included
the determination of reducing disaccharides(134),chlorinated
phenolic compounds (135),nitrogen-containing hazardous
pollutants (136),nitrogen-containing drugs ,(137),opium alkaloids (I38),and the classification of Bacillus stearotherANALYTICAL CHEMISTRY, VOL. 60, NO. 12, JUNE 15, 1988
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GAS CHROMATOGRAPHY
mophilus after pyrolysis GC (139). K1 s et al. (140)have
compared the usefulness of thermionic Jetectors for toxicological analysis.
The HeID operates on the principle of Penning ionization
and has been useful for the determination of volatile inorganic
ases which do not response well in the FID, although it can
e! used to detect organic compounds as well. A major development in the HeID during the past two years has been
the introduction of a pulsed-modulated detector. By anal0
to the three modes of operation of an ECD, h e y and T&
(141)investigated an HeID in fixed-frequency, constantcurrent, and direct-current modes of operation. While they
found the eatest sensitivity through direct current operation,
the pulsefmode offered greater stability and the constantcurrent mode increased the detector's dynamic range. Beres
et al. (142)constructed a Penning ionization detector from
Teflon and glass which was extremely inert and had a detector
cell volume of less than 5 pL. Useful after capillary gas
chromatography, the detector can be operated with both Ar
and He. General theory of operation of the HeID was reviewed
by Merten et al. (143)and by Rotin et al. (144).
The IMD is an atmospheric pressure time-of-flight ion
separation device developed as a capillary GC detector by Hill
and co-workers. Its multimode capabilities permit FID-like,
ECD-like, and molecular selective operation. Using a Fourier
transform method, they were able to obtain ion mobility
spectra from compounds eluting from a capillary column (145).
Mobility data collected in this manner can be used to predict
ion separation (146)and detector selectivity from literature
data which have been compiled into a single table (147).
Another detector investigated was based on quenching
ionization in a microwave plasma (142). For most or anic
species detection limits were in the range of IO4 to 10-B g/s
with a linear dynamic range of 4-6 orders of magnitude.
Absorptlon Detectors
Atomic absorption spectrometers were interfaced to gas
chromatographs to provide specific detection of volatile
metal-containing compounds. A general review of the technique was presented by Ebdon et al. ( J I ) but the primary
focus for research was on the determination of organolead
compounds. Forsyth (J2)designed a low-volume quartz
T-tube furnace for the atomization and AA detection of alkylleads separated by capillary gas chromatography. Key
design features of this furnace were extension of the heating
elements to the edge of the detector casing, the addition of
an in situ hydride generator, and the transference of the
analytes aa hydrides from the GC to the furnace. Propylation
of ionic alkyllead species with PrMgCl was found to offer
better recoveries than butylation (J3)and an investigation
of factors influencing sensitivity and accuracy for the determination of alkylselenides and alkylleads was conducted by
using cryogenic trap techniques (J4).
Next to GC/MS (covered elsewhere in this review), GC IR
provided the most detailed information for compound i entification. With Fourier-transform operation "on-the-fly" IR
spectra could be obtained and new algorithms were developed
for interpretation and selective detection. Several reviews on
GC/FT-IFt provided current information on this rapidly advancing method of identifying GC peaks (J548).FT-IR was
successfully employed for the identification of compounds in
JIO) and perfumes (JI1).
complex samples of essential oils (59,
An advantage of FT-IR over MS identification methods was
demonstrated by the differentiation of various isomers encountered in the determination of flavors (J12)and dioxins
(J13). Because of the nondestructive nature of FT-IR,
identification power after GC was enhanced and investigated
by direct coupled GC/FT-IR/MS systems (514417).Sensitivity of the technique was reported to be improved down
to the low nanogram and picogram range (J18).Sensitivity
improvements were largely due to continued development of
the optical configuration. Two approaches were reported: the
light-pipe and matrix isolation. Schneider and Demirgian
(J19)compared these two approaches. Ghijsen et al. (J20)
studied the effects of increasing the diameter of the light pipe
while Henry et al. (521)investigated methods to discriminate
against emission from the end of a hot light ipe. Rossiter
et al. (J22)reported that gold light pipes provifed exceptional
inertness and excellent high-temperature performance. Fuoco
d
286R
ANALYTICAL CHEMISTRY, VOL. 60, NO. 12, JUNE 15, 1988
et al. (J23)investigated the matrix isolation method by
t window cooled
trapping the GC eluate on the surface of an E
to a temperature of -45 "C. Fehl and Marcott (524)evaded
the problem of FT-IR sensitivity by applying a preconcentration step utilizing an injector/trap procedure. The tremendous quantity of data generated by FT-IR has prompted
the development of a variety of orithms for data reduction.
Anderegg and Pyo (J25)reporte a library search routine to
retrieve spectra of compounds of interest. Bowater et al. (J26)
developed a new algorithm for the generation of chromatograms from FT-IR data based on maximum absorbance. This
method was found to be more sensitive than the integrated
absorbance method and offered an alternative to the GramSchmidt method. Wang and Isenhour (J27)introduced the
use of a time-warping algorithm which eliminated the time
axis of a chromatogram so that chromatograms can be adjusted to match peaks.
Other absorption methods that were investigated included
optoaccoustic detection (J28)and photothermal detection
(J29,530). By use of a Helmholtz resonator as the optoacoustic detection cell, detection limits as low as 18 fmol were
reported for SF6. With photothermal methods, detection
limits of 0.7 ng for Freon and 1pg/s for SFs were reported.
9
Emlsslon Detectors
The category of gas chromatographicdetedors that operate
on the principle of light emission encompassesa wide variety
of design, modes of operation, and analyte response. In
general, the diversity of this category can be attributed to the
means by which the analyte, or its products, is excited. Because of the specificity of excitation energy and emission
energy, these detectors generally provide selective or specific
responses. Detectors in this category include the flame
photometric detector (FPD), chemiluminescence detectors,
plasma emission detectors, laser-based fluorescence detectors,
and radioactive detectors.
The FPD was characterized in the sulfur mode for compounds in petroleum (K1) and in the phosphorus mode for
organophosphorus pesticides (K2).Lee and Siebert (K3)
reported a new procedure for calibration. A number of improvements to the FPD were reported as well. Barinaga and
Farwell (K4)constructed a system that reduced the dead
volume in a commercial FPD by 8- to 20-fold and Wakayama
et al. (K5)developed a background correction method in which
they quenched the P response with a modulated magnetic
field. Chlorine and bromine com ounds were selectively
detected in the FPD by doping with 8 u (K6). Detection limits
of 0.5 ng/s for 1,4-dichlorobutaneand 0.07 ng/s for bromoform
were reported. Infrared emissions from flames as the basis
for chromatographic detection of organic compounds were
investigated by Hudson and Busch (K7). Using an optical
filter to isolate the asymmetric stretch of carbon dioxide at
4.3 pm,they calculated a detection limit of about 300 pg for
ethanol.
Plasma excitation methods include inductively coupled and
microwave induced systems. The inductively coupled method
was investigated by Duebelbeis et al. (K8)for the detection
of volatile organometallics but microwave induced plasmas
were investigated more extensively. Goode and Kimbrough
(K9)studied the signal-to-noise ratio of the microwave-induced
plasma detector (MIPD) and determined that the dominant
noise at the limit of detection was probably due to column
bleed. Although the MIPD has potential as a versatile element-specific detector in gas chromatography (KIO),there was
fluorine
special interest in its operation as an oxygen (Kll),
(K12),
and deuterium (K13)selective detector. Panaro et al.
(K14)took advantage of a direct current plasma to monitor
methylmercury in fish samples. Detection limits were lower
than those obtained with ECD but the cleanup procedure was
more extensive.
Laser based emission detectors offer both atomic and molecular fluorescence detection. D'Ulivo et d. (KI5) interfaced
a multichannel nondispersive atomic fluorescence spectrometer to a capillary chromatograph by using a minature flame
for atomization. The system was evaluated for alkylselenides,
alkylleads, and alkyltins and detection limits of 10 pg of Se,
30 pg of Pb, and 50 pg of Sn were reported. Atomic
fluorescence detection of a variety of bis(trifluoroethy1)dithiocarbamate complexes was also reported after GC sepa-
GAS CHROMATOGRAPHY
ration (K16).Molecular fluorescence was typically accomplished at subambient pressures after supersonic jet expansion.
Most of the development efforts have been focused on the jet.
Imasaka et al. (K17)used a high-temperature pulsed nozzle,
Pipich and co-workers (K18, K19) employed a pulsed jet
expansion system in which they achieved detection limits from
2 to 6 ng for monomethylanthracenes, and Stiller and Johnston (K20) were able to achieve a 50-pg detection limit for
naphthalene by using a jet nozzle based upon sheath flow gas
dynamic focusing.
Excitation from chemical reactions form a subgroup of GC
detectors known as chemiluminescence detectors. In general,
the excitation energy is supplied by reactions with ozone. A
review of the development of chemiluminescence as a detection method for GC has been published (K21). Chemiluminescence of products after catalytic reduction pyrolysis
products (thermal energy analyser) was employed for the
detection of nitrosamines (K22-K24) and polycyclic aromatic
hydrocarbons (K25). The chemistry occurring in redox
chemiluminescence detectors was investigated by Pourreza
et al. (K26).
Other emission detectors that have been reported include
molecular fluorescence of native fluorescent compounds as
they passed through a heated flow cell (K27) and a radioactive
detector using scintillation counting (K28).
SFC Detectors
The unique gaslike and liquidlike properties of supercritical
fluids continued to encourage investigations in which gas and
liquid chromatographic detectors were interfaced to supercritical fluid chromatographs. Novotny (L1)reviewed detection strategies that can be used with SFC while Later et
al. (152)discussed spectroscopic detection methods for capillary
SFC.
While the FID remained the GC-type detection method
most commonly used in SFC, other detectors traditionally
employed with gas chromatographs were investigated after
SFC. West and Lee’s (L3)evaluation of a thermionic detector
for nitrated polycyclic aromatic compounds found that the
nitro-selective mode of operation produced a 20-pg detection
limit for p-nitrophenol although linearity was confined to a
narrow range. Two other modes of operation were found to
be either unstable during density programming or too low in
sensitivity. Nevertheless, with the nitro-selective mode of
operation, they successfully detected a variety of nitro-containing compounds that could not be separated by gas chromatography. Sulfur- and phosphorus-selective detection
modes of a dual-flame photometric detector were found to be
less sensitive after SFC than after GC (154). Another unsuccessful attempt to adapt a GC-type detector to SFC was
the construction of a high-pressure photoionization detector.
When C02was used as the mobile phase, the quenching effect
of the gas reduced the sensitivity of the detector to an unacceptably low level (L5). Perhaps the most successful of the
GC-type detectors to be investigated in the past two years was
the ion mobility detector (IMD). Rokushika et al. (L6)constructed a capillary SFC system in which an IMD was placed
after an on-column UV detector. With COP as both the
chromatographic mobile phase and the ion mobility drift gas,
this investigation demonstrated the advantage of IMD for the
detection of compounds that do not contain chromophoric
groups. Eatherton et al. ( L n ,using a unidirectional flow ion
mobility detector, were able to efficiently eliminate the COP
mobile phase from the detector so that the ion mobility
spectrometer could be operated in the conventional manner
with N2 as the ion mobility drift gas. Using the Fourier
transform capabilities of this instrument, they were able to
capture complete ion mobility spectra of individual oligomers
separated by SFC and, using the selective monitoring mode,
they were able to detect specific oligomers in polymeric material.
The UV absorption detector has been the LC-type detection
method most widely used in SFC. Jinno et al. (L8, L9)employed a mutlichannel ultraviolet detector with computerenhanced spectroscopic separation to identify EPA priority
pollutants and a variety of PAHs after SFC separation. Light
scattering after nebulization of COPsupercritical fluid was
found to be more sensitive as an SFC detector than as a HPLC
detector (L10).Separation and detection of triglycerides,
poly(ethy1eneglycol), poly(oxyethylenes),polysaccharides, and
phospholipids were demonstrated with this technique (L11).
Light scattering from an Ar ion laser beam was also used to
probe the presence of aerosol after supersonic jet expansion
of supercritical COP,N20, SF6,n-pentane, and benzene (LI2).
The most active area of SFC detector research during the
past two years has been in the development and investigation
of identification methods, primarily infrared spectrometry and
mass spectrometry. For infrared spectrometry, two types of
interfacing approaches have been investigated: direct flow
cell and solvent elimination. The direct flow cell method has
the advantage of in-line, real-time detection but offers some
limitations as well. One problem with a direct flow cell is that
the COP transparency varies in the Fermi resonance band
region as a function of pressure (L13)and the addition of polar
modifiers degrades the overall quality of the spectra (1514).
Solvation effects of supercritical COPwere also monitored as
a function of density (L15). Nevertheless, COPoffers large
transparency regions where many functional groups can be
detected (L16). For example, free fatty acids were detected
by FT-IR after SFC from butter, soap, soybean oil, and coconut oil samples (L17). The extent of dimerization and the
degree of unsaturation of each component could be determined
by FT-IR spectra obtained for individual chromatographic
peaks. In addition to COP and modified COP, Freon was
investigated as a mobile phase for SFC/FT-IR (L18).Although the instrumentation required was somewhat more
complex, enhanced sensitivity, more extensive spectra, and
a greater selection of mobile phases were possible when FT-IR
was interfaced to SFC via the solvent elimination method.
With components aspirated from a capillary SFC column
directly onto a ZnSe window through a restrictor, FT-IR
spectra were obtained without interference from the mobile
phase (L19).Complete identification spectra were obtained
at the 50-ng level (L20). In a similar approach, diffuse reflectance FT-IR spectra were obtained after capillary SFC
(1521). A comprehensive review discussing both direct flow
cell and solvent elimination methods for infrared detection
was reported by Jinno (L22).
Mass spectrometry coupled with supercritical fluid chromatography received considerable attention over the last two
years for the identification of high molecular weight and
thermally labile compounds. The fundamentals and practice
of supercritical fluid chromatography/mass spectrometry were
reviewed in which supercritical fluid properties, various
methods of SFC/MS interfacing, and a variety of SFC/MS
applications were discussed (L.23425). The majority of investigations of SFC MS involved chemical ionization mass
spectrometry (CI- S) after capillary SFC. By use of a capillary restrictor, CI-MS data were reported for polynuclear
aromatic hydrocarbons and various lipids (1526).Lee and
Henion used a benchtop mass spectrometer with CH,-CI for
the detection of decafluorotriphenylphosphine but found
tailing at the low nanogram levels for caffeine and fatty acids
(L27). They attributed this tailing to the capillary restrictor
interface and suggested that improvements in the interface
were needed. For additional selectivity and complementary
structural data, other CI reagents were investigated including
ammonia for the determination of carbamate and acid pesticides (L28, L29). Improved methods for interfacing microbore and capillary SFC using a high flow rate interface were
described by Smith and Udseth (L30). In this design, a
mechanical pumped expansion region was employed behind
the chemical ionization repeller electrode to allow higher gas
flow rates. Matsumoto et al. (L31) reported the use of a
self-spouting, vacuum nebulizing assisted interface for the
determination of styrene oligomers, triglycerides, and poly(ethylene glycol) derivatives. Direct introduction of C02 into
Fourier transform mass spectrometers provided higher resolution than quadrupole systems (L32,L33). Electron-impact
ionization was also reported in which chemical ionization
contributions and clusters from the solvent were not observed
(L34).
d
GAS CHROMATOGRAPHYhlASS
SPECTROMETRY
Few fundamental developments in the area of GC/MS were
reported during the previous two years. A review discussed
the limitations and guidelines for the qualitative and quanANALYTICAL CHEMISTRY, VOL. 60,
NO. 12, JUNE 15, 1988 287R
GAS CHROMATOGRAPHY
titative analysis of mixtures by GC/MS ( M l )while a recent
book described the basic principles of GC MS (M2). One area
of tremendous potential is that of multi imensional GC/MS
(M3, M4). Hagman demonstrated the advantages of this
technique for the determination of volatile organic compounds
in polymers by dynamic headspace multidimensional GC/MS
(M5). Capillary-to-capillary column heartcutting provides
superior separation of seleded components resulting in purer
mass spectra and improved identification by computer library
searching (M6).
Developments in GC/MS data evaluation were reported.
Smoothing of GC/MS selected ion monitoring data was found
to achieve only a minor improvement in precision while introducing bias in the peak height ratio calculation (M7). It
was found by Pettit that at least five selected ion monitoring
scans need to be taken over the top half of the peak to achieve
an error less than 3% in the estimate of a GC peak height
(M8). A method was described to estimate GC/MS response
It was shown
factors when standards are not available (M9).
that the relative standard deviation method for determining
the working range of a GC/MS may have greater probabilities
of large errors than previously suspected, and a new method
based on the x2 distribution was proposed (MIO). Scott
presented a new method of classifying and identifying air
pollutants based on pattern recognition of mass spectral data
(M11).
Work continues to be performed on the combination of
GC/MS with the FT-IR technique. Wilkins described the
automated correlation of FT-IR and GC/MS reconstructed
ion chromatograms (M12). A mass analyzer was interfaced
to the light pipe of an FT-IR in a serially interfaced GC/
FT-IR/MS system (M13). Negative chemical ionization and
accurate mass measurement were found to im rove the reliability of both IR and MS search results in a Gt/FT-IR/MS
Laude described the use of a pulsed valve that
system (M14).
provides momentary gas pressure in GC/FT-MS chemical
ionization operation (M15). Use of this valve overcomes
problems in source pressures that restrict the mass resolution
and accuracy obtainable. Laser ionization GC/MS of nitroand nitroso-containing compounds was found to produce
substantial quantities of NO+, in contrast with electron impact
GC/MS (M16). Lasers were also used for a multidimensional
instrument applied to the characterization of environmental
samples for polycyclic aromatic hydrocarbons in another investigation ( M I 7). The laser-analyte products (cations,
electrons, and photons) were simultaneously monitored. The
time-of-flight mass spectrometer used allowed an entire
photoionization mass spectrum to be obtained for each laser
pulse. Time-of-flight mass spectrometers are ideal for use in
GC/MS applications because they can produce up to 10000
mass spectra/s, although some improvements to the data
system to allow processing of such large number of spectra
are needed (M18).
(4
METHODOLOGY
Pyrolysis
Recent developments in improving the reproducibility in
solids analysis by pyrolysis GC have been reviewed (N1).
Reviews of pyrolysis GC for characterizingpolymers have also
appeared (N2,N3). The combined use of pyrolysis GC with
other techniques such as infrared spectroscopy (N4),FT-IR
(N5),and m889 spectrometry (N6)is increasing in importance.
Such techniques have been used to fingerprint complex biomachine copier toners (N4),and other
logical materials (N6),
macromolecules such as epoxy and phenolic resins (N5). The
techniques of pyrolysis MS, pyrolysis GC, and infrared
spectroscopy to analyze paint resins were found to be complementary, and the use of a combination of these techniques
was recommended (N7). Prepyrolysis was used to simplify
the identification of many polymers in paper by pyrolysis GC
(N8). Sufficient polymers were present in the paper tested
that survived prepyrolysis to be identified by pyrolysis GC
at a higher temperature. Pyrolysis GC/MS was successful
in differentiating reproducibly between eight strains of group
A streptococci and six strains of group B streptococci by the
presence of a single chemical marker appearing only in the
pyrograms of group B or anisms (N9). The potential exists
for further correlations getween the chemical structure of
microorganisms and pyrolysis products.
288R
ANALYTICAL CHEMISTRY, VOL. 60, NO. 12, JUNE 15, 1988
Multicolumn Chromatography
Multidimensional GC is becoming less a topic of research
and more a method of routine analysis. It is surprising that
few commercial systems are yet available. Definitions and
characteristics of multidimensional GC have been described
by Schomburg (01).A new type of packed column was used
in a two-dimensional system without need of cold-trapping
(02). Combined SFC[multidimensional GC was found to be
very useful for selective heartcutting (03, 04).
Many new studies were reported concerning the development and use of serially coupled columns. The theory and
practice of coupled columns were described by Purnell(O5),
who also presented experimental verification of the theory
(06). Their general theory of serially coupled GC columns
was shown to be valid and free of assumptions other than that
of carrier gas ideality. Jianying developed a multidimensional
window diagram method to select optimum column temperature and gas flow velocities in the series-coupled systems (07).
Fundamental relationships in multicolumn GC used for tuning
selectivity were discussed (08). Methods of preparing hybrid
fused-silica columns were described (09). An equation to
predict plate height on serially coupled WCOT columns has
been developed and was found to have good agreement with
experimental data (010). Methods for optimizing separations
in serially coupled columns (011)and for columns composed
of mixed stationary phases (012) have been presented.
Dramatic selectivity changes in serially coupled columns of
differing polarity were shown to occur with even slight carrier
gas flow changes in one part of the column series (013). Serial
micropacked fused-silica capillary columns were studied by
Malik (014). He explained theoretically the advantages of
locating the segment containing the finer sorbent fraction near
the column outlet on the basis of better efficiency and mass
transfer coefficient.
A review of multidimensional LC LC and LC GC separations has been presented (015). he state-of-t e-art and
future outlook of HPLC GC have been reviewed by Grob
(016). Introduction of IdPLC fractions directly to capillary
GC columns is performed either by the retention gap technique or by fully concurrent solvent evaporation (017, 018).
A loop-type interface for concurrent solvent evaporation has
been described (017). Experimental background for facilitating column temperature selection with concurrent HPLC
eluent evaporation in coupled HPLC/HRGC systems was
discussed (019)and the minimum column temperatures required for eluent transfer were experimentallydetermined for
solvents used as HPLC eluents (020). The use of HPLC/
HRGC was demonstrated for residue analysis (021)and as
a replacement for GC/MS in the determination of diethylstibestrol in bovine urine (022).
4
h
Headspace Gas Chromatography
Reviews on the use of headspace GC (HGC) in the flavor
and fragrance industry ( P I )and for systems not in thermodynamic equilibrium (P2)have been presented. Techniques
for cryofocusing and cryogenic trapping have also been reviewed (P3). A collaborative study for ethanol in canned
salmon showed that repeatability and reproducibility of HGC
can be better than 5 % (P4). Most new work in HGC was to
study cryogenic focusing ( P 5 4 9 ) . By simple cooling of the
GC oven, headspace vapors were cryofocused at the head of
a fused silica WCOT column coupled to a packed column
injection port (P5). A multiple headspace injection technique
was used to increase analytical sensitivity. The theoretical
background and instrumentation of cryogenic trapping for
HGC have been presented (P6).Profiling mid-to-highboiling
compounds in the headspace of foods was performed by
off-line sorbent trapping followed by automated thermal
desorption and splitless injection into a cryogenically cooled
WCOT column (P7). Principles of purge-and-trap (P&T) onto
Tenax T A followed by thermal desorption onto a WCOT
column retention gap with cryofocusing were discussed as
applied to favor and fragrance chemistry (P8). The effects
of sampling and desorption arameters on recovery for this
system were reported (P9). Effects of trapping temperature
and WCOT column film thickness in P&T GC were studied
(PIO).Quantitative recoveries and good chromatography can
be obtained by careful control of conditions. GC analysis of
GAS CHROMATOGRAPHY
trapped headspace volatiles has also been performed by microwave desorption from graphite (P11)and by on-column
injection of solvent used to recover volatiles from activated
carbon traps (P12).
mixtures was presented (R17).By measuring retention on
SE30 and OV351 columns, Kuchar was able to simulate the
octanol-water system for evaluating the lipophilicity of selected esters of aromatic and aliphatic acids (R18).
Chemometrlcs
A theoretical model of peak overlapping was presented
where sample components are randomly distributed along the
retention axis (81).It allows for a prediction of the probability
distribution of the number of sample components when the
number of resolved peaks is known. Deconvolution of overlapping GC peaks was studied by using Jansson’s method (Q2,
83) and by extension of the Fourier spectrum (Q4). Partially
overlapping chromatographic peaks can be deconvoluted
without any assumptions about chromatographic peak shape
or prior knowledge of the spectra of the individual compounds
by using multichannel detectors that produce spectra characteristic of the eluents (85).SIMCA pattern recognition was
applied to the grouping of bacteria (86) and the homologue-specific analysis of PCBs (87). The effects of sludge
treatment on soil samples were determined by pattern reco ition without prior knowledge of chromatogram peak
i g n t i t y or compound class type (Q8). For the principal
component modeling of crude oil fractions using GC profiles,
prior normalization to percentages was unnecessary when
logarithmic data were used (89).
A method for the generation of GC/FT-IR chromatograms
using maximum absorbances was reported (810). Because
it can create both universal and selective reconstructions with
ood sensitivity, this method is an alternative to the Gramchmidt method and should replace the integrated absorbance
method. Howery predicted retention indices for 42 solutes
and 24 stationary phases to better than 1% by using target
factor and multiple regression analysis (QII). New numerical
methods were also reported for the scaling of analytical data
(Q12)and for selecting exponential flow programs in WCOT
GC (Q13). An improved numerical integration method for
modeling GC line shapes (Q14)and a fast multiparametric
least-squares adjustment of GC data by using Wentworth’s
method (Q15)were also presented.
8
MISCELLANEOUS
Several recent reviews are of interest. Grob published a
book describing on-column injection techniques (RI)and
reviewed the use of retention gaps (R2).Recent developments
in inverse GC applied to polymer blends (R3) and for the
determination of the polarity of nonionic surfactants (R4)have
also been reviewed. Berezkin reviewed the main applications
of temperature gradients as used in GC (R5).Miller used
recycle GC to obtain improved separations for nonpolar analytes (R6).Adsorptive polarity is additive, and therefore a
serious limitation for the use of recycle GC for polar analytes.
An improved method for determining dead times in inverse
GC (R7)and the use of reversed-flow GC to determine mass
transfer and partition coefficients across gas-liquid boundaries
(R8)were discussed. Schurig presented a method for separation of isomers of underivatized aliphatic alcohols and ketones by complexation GC on optically active metal chelates
(R9).Thermodynamic and kinetic parameters relating to the
sorption-diffusion of aromatic hydrocarbonsin zeolites at high
temperature (613-713 K) were evaluated by the GC pulse
method (RIO). Ha and co-workers studied the operational
characteristics of a moving-feed injection system for the GC
separation of diethyl ether and dichloromethane (R11).
Bartu presented heuristic methods to minimize retention
times of the most difficult to separate component pairs in
mixtures (R12).Thermal desorption modulation was discussed
as a replacement for conventional sample injection in very
small diameter WCOT GC columns (R13). Multiple pulses
of a short section of column whose temperature can be rapidly
and precisely controlled result in a multiplexed detector output
signal from which chromatogramscan be computed. Methods
were presented for precise detection of void zones in packed
GC columns (R14)and for the determination of intraparticle
difusivities of large-pore particles in packed columns (R15).
A new means of quick and safe optimization to achieve
maximum efficiency, termed “peak number IO”,was developed
by Kaiser (R16).A mathematical procedure to predict the
optimum composition of mixed stationary phases for complex
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(E29) Melda, K. J.; Leaseburge, E. J. Anal. Instrum. 1988, 22, 1-6.
.
.
.
.
SUPERCRITICAL FLUID CHROMATOGRAPHY
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1F21 Schoenmakers. P. J.: Verhoeven. F. C. C. J. G. Trends Anal. Chem.
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___
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INSTRUMENTATION AND DETECTORS
Sample Introductlon
(Gl) Vouros, P. J . Chromatogr. 1987, 407, 305-9.
(G2) Hartman, T. 0.; Rosen, R. T.; Ho, C. T.; Rosen, J. D. LC-GC 1987, 5(9).
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GAS CHROMATOGRAPHY
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Detectors
(HI) Dressler, M. Selective Gas Chromatographic Detectors ; Elsevier: Amsterdam, 1986.
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Schlegelmilch, F. Prog. Essent. 011Res ., Proc. I n t . Symp Essent. Oils ,
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.
Ionlzatlon Detectors
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(12) Axner, 0.;
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Absorpllon Detectors
(Jl) Ebdon, L.; Hili, S.; Ward, R. W. Analyst (London) 1986, 771(10),
113-38.
(J2) Forsyth, D. S. Anal. Chem. 1987, 59(13), 1742-44.
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GAS CHROMATOGRAPHY
Emlrrlon Detectors
(Kl) Bradley, C.; Schiller, D. J. Anel. Chem. 1988, 58, 3017-21.
(K2) Trotter, W. J. Int. J. Envlmn. Anal. Chem. 1987, 30(4), 299-308.
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.
.
SFC DETECTORS
GAS CHROMATOGRAPHYIMASS SPECTROMETRY
(Ml) Millington, D. S.; Norwood, D. L. Org. Carcinog-Drinking Wafer; Ram,
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Sci. 1988, 24(1), 26-33.
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(M8) Pettit, Brian R. Biomed. Envlron. Mass Specfrom. 1986, 13(9), 473-5.
(M9) Sauter, A. D.; Downs, J. J.; Buchner, J. D.; Ringo, N. T.; Shaw, D. L.;
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(M18) Allison, J.; Holland, J. F.; Enke, C. G.; Watson, J. T. Anal. Insfrum.
1987, 76(1), 207-224.
METHOWLWY
(Ll) Novotny, M. J. High Resoluf. Chromafogr. Chromafogr. Commun.
1988, 9(3), 137-44.
(L2) Later, D. W.; Bornhop, D. J.; Lee, E. D.; Henion, J. D.; Wleboldt, R. C.
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(L3) West, W. R.; Lee, M. L. J. High Resolut. Chromatogr. Chromafogr.
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8.
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\-
.
(L27) Lee, E. D.; Henion, J. D. J. High Resolut. Chromatogr. Chromatogr.
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~
Pyrolysis
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Multlcolumn Chromatography
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~
MISCELLANEOUS
(R 1) Grob, Konrad On-Column Injection in Capillary Gas Chromatography:
Basic Technique, Retention Gaps, Solvent Effects; Verlag: Heidelberg,
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Mass Spectrometry
A. L. Burlingame*
Department of Pharmaceutical Chemistry, T h e Mass Spectrometry Facility and T h e Liver Center, University of
California, S a n Francisco, California 94143-0446
D. Maltby
Department of Pharmaceutical Chemistry and T h e Mass Spectrometry Facility, University of California, S a n
Francisco, California 94143-0446
D. H. Russell
Department of Chemistry, Texas A&M University, College Station, Texas 77843
P. T. Holland
MAFTech, Ruakura Agricultural Centre, Hamilton, New Zealand