Gas Chromatography - ACS Publications

Anal. Chem. 1992, 64, 170R-180R
(410) Favatl, F.; King, J. W.; Mazzantl, M. J . Am. OM Chem. Soc. 1991, 68,
422-427.
(411) mnkston, J. D.; Deianey, T. E.; Bowling, D. J.; Chester, T. L. J . Hb@
Resol&. Chrometogr. 1991, 14. 401-406.
(412) m a k e s , M.; Vasconwlos, A. M. p.; ames
de ~ ~ ~E. J,~ s,;e
Chaves das Neves, H. J.; Nunes da Ponte, M. J. Am. 011 Chem. SOC.
1991, 68, 474-480.
(413) Rossi, M.; Schiraldi, A.; Spedicato, E. Dev. food Scl. 1890, 2 4 ,
855-863.
(414) Ong, C. P.; Ong, H. M.; Li, S. F. Y.; Lee, H. K. J . Mlcmolumn Sep.
1990, 2, 69-73.
(415) Pellerin, p. pedum. fbvw. 1881, 16, 37-39.
(416) Nykanen, 1.; NYkanen, L.; Alklo, M. J . €sent. 011 Res. 1991, 3,
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(417) Miles, W. S.; Qulmby, B. D. Am. Lab. (faIdbM, Conn.) 1890, 22,
28F, 28H, 28J, 28L.
(418) Ondarza, M.; Sanchez, A. Chromatographie 1990, 30, 16-19.
Gas Chromatography
Gary A. Eiceman*
Department of Chemistry, New Mexico State University, Las Cruces, New Mexico 88003
R. E.Clement
Ontario Ministry of the Environment, Laboratory Services Branch, 125 Resources Road, P.O. Box 213,
Rexdale, Ontario, Canada M9W 5L1
Herbert H. Hill, Jr.
Department of Chemistry, Washington State University, Pullman, Washington 99164
loyed for predictingretention indexes for trans-diazenes (A6).
Ecubic
everal approaches to modeling retention were compared to
s lines (A7)for variance in predicted retention indices.
INTRODUCTION
This review of the fundamental developments in gas
chromatography (GC) covers 1990 and 1991. Since the
principal means of literature review was the biweekly Chemical Abstracts Service CA Selects for GC, publications appearing in late 1989 are also included, while significantpapers
published in late 1991 may not be. The related technique of
gas chromatography-mass spectrometry (GC-MS) is also
covered in this review.
General trends noted in recent prior reviews continued
during the last 2 years and advances occurred in each ate ory
addressed in this review. Noteworthy is the continuef attention given the principles of and rationales for the characterization of liquid phases and for the prediction of retention
behavior. Mechanisms responsible for the operation of traditional ionization detectors are not well described and were
addressed in the midst of rich utilization of optical detectors.
Interest in the combination of chromatographic columns in
serial manner to mimic mixed liquid phases or through valves
to isolate fractions for multidimensional chromatography has
own and might merit a separate category in future reviews.
ubtopics were added to the format for this year.
F
COLUMN THEORY AND TECHNIQUES
Developments in column theory and the techniques used
in describing column performance seemed to converge on a
few major themes. These included aspects on column retention, temperature programming, efficiency, and serially
coupled columns. The objectives that underlie these reports
were based on the prediction or optimization of resolution or
retention generally through semiempirical means. The prediction of retention or retention indices was the dominant
subject in this section by a substantial margin.
Retention. Retention of solutes in columns was addressed
using nearly a dozen approaches. A model succeeded for
calculating activity coefficients to predict retention with
nonpolar phases ( A l ) ,and the Wilson equation allowed the
prediction of activity coefficients in mixed phases (A2).
Molecular connectivity was develo ed for polychlorinated
dibenzofurans and accounted for t1e number of chlorines,
positions, and skeletal structure (A3). An approach employing
the quantitative structureretention relationshi (QSRR)was
evaluated for anabolic steroids (A4) and for Augs of abuse
(A5). Topological indexes and physical parameters were em170 R
T
The rok of alkyl groups in retention of heterocycles was explored and comparisons made to predictions using nonlinear
additivity concepts (AB). Monte-Carlo simulations of retention
times were accurate within 1-2% for nonpolar compounds and
nonpolar liquid phases (A9). Prediction of retention times
with serially linked columns was advanced through capacity
factor methods (A101 and through a two internal standard
method (A11 ) . Information indices for predicting retention
indices were explored for chlorinated hydroxybenzaldehydes
(A12).
Prediction of retention characteristics,other than retention
time or index, was the subject of several works and included
the simulation of a chromatogram (A13)and an assessment
of the number of constitutenta from peak shape distortion
(A14).
In some works, the emphasis on retention index merited
discussion separate from general retention behavior. Retention indexes for alkylbenzenes were predicted using equations
for mass and substituent structure (A15), Gibbs solvation
(A16),and linear free ener relations (A17). Two
;:;!?theoretical
models were deverped to relate molecular
structure and retention indices for alkylbiphenyls ( A B ) .
Especially interesting were examinations of the underlying
premises of retention indices (A19),the precision of determinations with polar columns (A20),
and the neighboring peak
effect (A21). Ambi 'ties in the McReynolds constants were
n
zalternative phase classificationbased
discussed (A22)a
upon multivariate analysis was illustrated (A23)and expanded
(a).
Other proposals to reevaluate the McReynolds liquid
phase set into clusters (A25) or to develop new equations (A26)
were reported. Rijks et al. (A27) created a database for retention indices for temperature-programmed GC and addressed experimental influences specific to a given column.
Retention was the theme of another claas of studies in which
specific influences that overn or confuse apparent retention
measurements were adfressed. The most pronounced effect
was adsorptions resulting in mixed mechanisms of retention;
this was explored for capillary columns (A28, A29) and for
packed columns with silica gel supporta (A30). Carr addressed
the assumption of negligible film thickness in ca illary
chromatography through two theoretical solutions (A317. The
effect of adsorption at the gas-liquid interface was found
dependent on film thickness when solutes and phases of
0003-2700/92/0364-17~R~10.00~00 1992 American Chemical Soclety
GAS CHROMATOGRAPHY
Gary A. Elceman is a Professor of Chemistry at New Mexico State University In Las
Cruces, NM. He received his Ph.D. degree
In 1978 at the University of Cobrado and
was a postdoctoral fellow at the University
of Waterloo, Ontarb. from 1978 to 1980.
I n 1987-1988 he was a Senior Research
Fellow at the US Army Chemical Research,
Development and Engineering Center at Aberdeen Proving Gd., MD. He has been on
the facuity at New Mexico State University
since 1980. His research interests include
the
development
of
selective
chromatographic phases, use of GC/MS for
environmental research, and the development of ion mobility spectrometry as a chemical sensor, process monitor.
and chromatographic detector. He also has interests in atmospheric pressure ion-molecule chemistry exemplified by the electron capture detector.
He regularly teaches separations chemistry and electronics at the graduate
level and quantitative analysis at the undergraduate level.
Ray E. ckment is a Research Sdentist with
the Ontario Ministry of the Environment,
Laboratory Services Branch, and Associate
Executive Director of the Canadian Institute
for Research in Atmospheric Chemistry (CIRAC). He graduated with his Ph.D. from the
University of Waterloo in 1981. Dr. Clement
has taught undergraduate courses on GC
techniques and instrumentation, and has
coauthored the book Basic Gas chromarugraphylMass Spectrometry: Principles and
Techniques. His principal research areas
involve the uses of GC and GClMS for the
analysis of ultratrace levels of toxic organics
in the environment, specifically for the c h b
rinated dlbenmpdbxins and dlbenzofurans. He has authored some 80 publications in this area and currently serves on the editorial board of Chemosphere. As a member of CIRAC, Dr. Clement is also interested in atmospheric research including gbbal warming and the long-range transport of toxic organics.
Herbed H. Hm, Jr., is a Professor of Chemistry at Washington State University where
he directs an active research program in
the development of instrumentation for trace
organic analysis. His research interests include gas chromatogaphy, supercritical fluid
chromatography, ion mobility spectrometry,
ambient pressure ionization sources, and
mass spectrometry. He received his B.S.
degree in 1970 from Rhodes College in
Memphis, TN, his M.S. degree in 1973 from
the University of Missouri, Columbia, MO
and his Ph.D. degree in 1975 from Dalhousie University, Halifax, Nova Scotia. Canada.
I n 1975 he was a postdoctoral felbw at the
University of Waterloo, Ontario, and in 1983-1984 he was a visiting professor at Kyoto University, Kyoto, Japan. He has been on the faculty at Washington State University since 1976.
different polarity were used (A32). Cross-links in phases
seemed to improve column behavior toward interface adsorption (A33).Retention by adsorption figured prominently
in the chromatographic properties of poly(ethy1ene glycol)
20M for which methanol showed interactions with residual
silanol groups and n-octane experienced interface adsorption
(A34).Finally, experimental parameters that affect resolution
or separation in GC were optimized using simplex procedures
(A35,A36).
TemperatureProgramming. Concerns in the subject of
temperature programming were represented by reports on
determinations,predictions, and analysis, and these have been
representative of concerns during the last decade at least. A
cubic spline method yielded favorable results with retention
index calculations for different heating rates (A37).Reproducibility or retention indices were examined for columns with
different phase ratios and void volumes (A38).Predictions
of retention indices for programmed temperature conditions
from previously developed theoretical models were compared
to empirical results (A39)and showed satisfactory agreement.
A comparison of several methods for assigning temperatureprogrammed retention indices under various heating rates was
presented, and cubic spline polynomials were preferred (AN).
Analysis of peak moments from temperature-programmed GC
suggested that conventional definitions for plate height and
peak variance may be incorrect, and new definitions were
proposed (A41).The sensitivity of retention indices for 49
polycyclic aromatic hydrocarbons to liquid-phase polarity was
assessed in terms of structure, and this was enhanced for the
branched or hydrogenated structures (A42).
Efficiency and Foundations. Attention in this section
was devoted principally to core concepb of chromatographic
theory and column parameters. The effect of temperature
on resolution in chiral systems was examined (A43)as was
temperature dependences of dead time for methane retention
(A44).The understanding of contact between molecules and
a liquid or stationary phase was given new insights by the
observation that hydrogen-deuterium exchanges occur for
deuterated ketone on fused-silica capillary columns (A45).
Concepts or turbulent flow in capillary columns has also been
reexamined, refined, and verified (A46).Others have explored
improved measurements of obstructive factors and porosity
(A47),effective diffusivities (A48),and binary diffusion
coefficients (A49).
Serially Coupled Columns. One development in column
basics with demonstrated advantages in separations and fast
growth in the literature has been serially coupled columns.
The foundations for mixed liquid phases derive from work
in the late 1970s by Laub and Purnell and can be easily
adapted to capillary columns by joining various lengths of
columns with different polarities to yield optimum phase
composition for a given sample. This topic should be regarded
as different from multiple-dimensional chromatography in
which portions of effluent are isolated and subjected to full
chromatographic analysis. An example of the original concept
of mixed phases as applied to serially connected columns was
shown by Fougnion (A50).An update by Purnell revised the
practical aspects of his theoretical model (A51).Computers
were used for serially coupled columns with a spreadsheet to
optimize length and temperature (A52)and to optimize temperature and pressure drop (A53).Descrepancies were found
in the Kovats retention index concept for series-coupled
columns (A54).
LIQUID PHASES
The themes in this section were on production and evaluation with goals much as in years past, namely, elevated
temperature stability, enhanced selectivity, and compatibility
with polar compounds. Large numbers of reports occurred
in the facets of production and the disclosure of new preparations. Included below are those which feature basic studies
or fundamental principles. This goal was relaxed slightly to
include aspects of liquid phase-substrate chemistry. A remarkable change from prior years was the absence of model
development for chiral phases and liquid crystals.
Synthetic Organic Phases. Two variations of polysiloxane stationary phases were noted and included a cyanophenyl-containing derivative (BI) and a nitro- and cyanophenyl moiety on a diethylene oxide side group (B2).These
phases exhibited both polar and polarizable character. In
addition, Lee et al. showed that the ethylene spaces were
necessary for the nitro- and cyanophenyl derivative phases
and that efficiencies were poor without the spacers (B3).
Liquid phases based on imides (B4)and carbonates (Bs)were
described and yielded high thermal stability and polarities
suited for specialized separations such as acrylic acid on the
polycarbonate phases. Two benzo-crown ether phases were
prepared, and selectivity was ascribed to size and shape of
solutes for a given crown ether ring (B6). Hydrogen bonding
also contributed to retention with crown ethers immobilized
on polysiloxanes (B7). The preparation of unconventional
packings with conventional liquid phases suggested some new
directions to liquid-phase investigations. Dimethacrylate
layers were formed on Chromosorb G (B8)to yield, surprisingly, retention by gas-liquid partition. Colloidal sorbents
of dioctylsebacate with carbon black (B9)were described as
effective for acylates and related compounds.
C h i d and Natural Phases. The principal subject in this
section was cyclodextrin and cyclodextrin derivatives as chiral
stationary phases (BIO-BI3). Methylated cyclodextrim have
been diluted in polar siloxanes to illustrate the role of inclusion
ANALYTICAL CHEMISTRY, VOL. 64, NO. 12, JUNE 15, 1992
171R
GAS CHROMATOGRAPHY
(BIO)and determine effects of dilution on resolution (BII).
Kenig has e lored derivatized cyclodextrinefor mechanisms
of selectivitv%12)
- .
. and for use with various functional ~ O U D S
(B13).
Metal-Based Phases. Some activity occurred in complexation gas chromatography, and a few articles were identified as relevant for discussion. Thermal stability of silver-based liquid phases was imparted through silver compounds of fluorinated acetates (B14). Another study devoted
to thermal stability involved palladium complexes (B15).
Studies devoted to exploring mechanisms of retention for
metal-based liquid phases were found for nickel complexes
in chiral separations (B16) and lanthanide B-diketonates in
chromatography of oxygen-containing organic compounds
(B17).
Production. The design and roduction of the liquid phase
are practically concomitant with tonding of phases to supports
for improved mechanical properties, and most articles are
highly empirical. A few articles involve detailed analysis of
findin s or examination of chemistries and can be included
here. blomberg reviewed current immobilization methods and
while others sought new approaches to imchemistry (B18),
mobilization such as plasma pretreatment of surfaces (B19),
a cross-linking w e n t (BaO),and repeated croes-linking (B21).
Immobilization of phases for packed columns in GC was reported and showed uniform coverage of solid support (B22).
I
_
SOLID SUPPORTS AND ADSORPTION
The emphasis during the last 2 years for the subject of this
section has been constant, and the adsorbants which received
greatest interest, as before, are natural materials. The theme
of such studies generally is the characterization of surface
chemistry or composition by assessing retention behavior of
particular compounds chosen to probe specific interactions.
Noteable in this review was the appearance of nearly a dozen
articles on the basics of adsorption processes or on ex erimental techniques. Derivatization of solids for specidzed
properties was evident but leas pronounced than for preceding
reviews. The largest category of works was in the interpretation of surface chemistry from adsorption measurements.
Adsorption Studies. Reports were found on adsorption
studies with roughly 10 classes of solids, and carbon was the
most examined material. A review on graphitized carbon black
emphasized the properties and uses during the last 20 years
( C l ) . Pankow (C2) developed equations to predict retention
of volatile compounds on graphitized carbon through correlations to vapor pressure and boiling point. Others (C3, C4)
also studied the adsorption behavior of graphitized carbon.
Particularly noteworthy were two studies on the heats of
adsorption with microporous carbon black (C5, C6). Carbon
fibers (C7, C8) were characterized for acid-base roperties
which were governed by pretreatment or staiilization.
Modification of carbon was reported to increase energetic
heterogeneity for adsorptions (C9).
The emphasis on glasses and silica was on derivatization
including the effeda on adsorption of alkenes on silica (ClO),
the role of surface sodium in adsorption (CZl),and the surface
free energies of glass fibers (C12). Composite oxides (C13)
and minerals (C14, C15)were also characterized for acidic
adsorption sites and effects of thermal treatments on surface
properties. The role of grou I and I1 metals in surfaces of
aluminas was examined in tge context of other adsorption
mechanisms (C16). Last in this general category of oxides are
zeolites or molecular sieves which were the subject of second
virial analysis (C17) and were modified with iron (C18) and
silver (C19) for specialized applications.
Two other natural materials for GC experiments were clays
and cellulose. Variations of Bentone-34 were examined and
discussed in terms of separations of isomers (C20). The
principles for thermal stability of organo-tailored montmorillonites were elucidated (C211, and a model was developed
to rationalize behavior in gasaolid adsorption GC with
thermally stable modified montomorillonites (C22). Thermodynamic adsorption parameters for cellulose were determined as a function of surface coverage (C23),and contributions to total adsorption energy from specific contributions
were estimated (C24).
Synthetic organic polymers were characterized for surface
adsorptivity although the reporta were few in number. Con172R
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ANALYTICAL CHEMISTRY, VOL. 64, NO. 12. JUNE 15, 1992
tributions from specific intermolecular interactions for meand results from inverse
thacrylates were calculated (CW),
GC of Kevlar fabric showed the effects from surface finishes
(C26).
Active exploration of salts and metal-based adsorbents
exhibited diversity around the common theme of metalmlute
interactions. Nayak (C27, C28) characterized ammonium
molybdophosphate and ammonium tungstophosphate. Protonina and Nikitin elucidated the surface properties of ferric
oxide (1229, C30). The chromatographic consequences from
hase transitions in salt hydrates were described for salt
gydrates including copper sulfate (C31). The influence of
various surface treatments for aluminum metal was probed
usin hydrocarbons and perfluoro analogues and suggested
thatLnzene was a weak acid and that perfluorobenzene was
a weak base (C32).
Procedures. Several impressive developments occurred
in approaches to surface characterization. Guiochon ((233)
described a new method to delineate the energetics of adsorption sites from isotherm data. The methods for characterizing low surface area glasses by direct means and not from
powder samples were reviewed (C34). A model study for
approaches to acid-base surface characterization was published (C35).The dispersive component of silica was revealed
through infinite dilution measurements (C36),and methods
were given for determining rate constants for adsorption/
desorption with silica ((237).
SORPTION PROCESSES AND SOLVENTS
This section is again an area which is active in several
aspects of sorption and solubility. The topics which define
this section can be categorized into four groups with substantial overlap between sections. In some instances, the
categories are chosen on the basis of the emphasis within a
report and so divisions have been made mindfulof thiscaveat.
Structure-Retention Studies. Several broadly significant
studies on the relationship between solute structure and retention on a particular liquid hase were published by Hanai
(01, 02) who provided a m o t h for enthalpy and selectivity
and a correlation between van der Waals volumes and capacity
ratios. van der Waals volumes were also utilized in structural
models for describing retention of alkyhaphthalenes ( 0 3 ) . In
other such reports, specific compounds were often used to
highlight weaknesses in existing models and sug est imrovements. This was done for alkylanilines (047,alkylkmzenes (05),polychlorinated dibenzodioxins and dibenzohalobenzenes (On,and quinazolone derivatives
furans (B),
(08).Other such reporta from Papp were based on pyridopyrimidine derivatives (09)to probe shielding of polar centers
and a heterocyclic model (010) to test ring size on polarizability. The structural basis for adsorption was addressed for
alkanes and alkenes on crystalline silica (01I) and generally
for hetero eneous adsorbents (012). Gilpin treated the relationship &tween an energetically heterogeneous surface and
retention (013).
Structures of Phases. A subtle emphasis in this section
versus that in the section or liquid phases above is the intention to study retention through changes in liquid phases
rather than to build new liquid phases for improved separations. Conf ations of 1:l methyl henylsiliconea influenced
olarity a n g e r m a l properties ( 14). Homologues of cark nyl-containing molecules were studied, and intramolecule
interactions between neighboring methyl and CO groups were
affected by the existence of stron ly electrone ative groups
on the stationary phase (015). T%erole of incksion versus
was elucidated for crown ethers (DM),
while
hydrogen bon
inclusion can be locked to prevent chiral separations (017).
Stereospecificityfrom various forms of cyclodextrin for cistrans acyclic alkenes and cyclooctenes was reported (018).
The nature of soluholvent interactions necessary for c h i d
separations could be ascribed to hydrogen bondin (019)or
complexation concepts (020). Inclusion with cyckdextrins
was favored at elevated temperature in GC compared to liquid
chromatography (021). Particularly noteworthy was a proposal to address phase properties from a thermodynamic
perspective (022).
Aspeets of Solubility. Factors and parametem that govem
or describe solubility were actively studied in the period for
this review. Poole proposed a new solvent model for phase
8
7
QAS CHROMATOQRAPHY
classification (023),and Betta disputed some features of the
selectivity triangles of Poole (024).Polarity of phases was
. sets of polyaddressed using solubility factors (025)Two
mer-solvent interactions were complied (026,027). Dispersion and selectivity in solutesolvent interactions was
ho
clarified with homologous carbonyl compounds (028)' .
approaches proposed to measure solute-solvent interactions
)
was
included linear solvation energy relationships (029which
sensitive to polar/polarizability and partial molar enthalpy
of mixing (030)which was correlated to a wide range of
molecular parameters. Different contributions to solutesolvent interactions were also addressed using descriptors with
a four-variable equation (031). An example of the Snyder Karger-Hansen interaction model was reported (032).
'/hemodynamic and Physical Parameters. The prominant subjects in this section included the determination of
activity coefficients and the determinations of enthalpies or
free energies. Activity coefficients were compared to partition
) used to probe for surface effects at the
coefficients (033and
.
for calculating changes
gas-liquid interface (034)Equations
in enthalpies and entropies of solution were proposed (0351,
and comparisons of entropies and enthalpies were used to
rationalize separations of enantiomers (036).Dipolar interactions were thought responsible for agreement in two approaches to analysis of thermodynamics of mixing (037),while
another approach for comparable analysis was proposed using
Nematic and isotropic
scaled particle treatments (038).
phases were characterized using solutes of various size, shape
and flexibility for thermodynamics of solution and compared
to models (039).Comparable studies have been devoted to
using free energies for understanding retention (040,041).
WALL-COATED OPEN TUBULAR COLUMNS
Most developments were concerned with new ways to improve the coating and cross-linking of station phases, especially for fused-silica columns. New l i q u y phases for
WCOT columns were covered earlier in this review.
Sumpter reported on the static coating of small-diameter
WCOT columns with various phases to give efficiencies as
great as 66OOO plates m-l (El).Two new end-sealing methods
for static coating of wide-bore glass capillary (E2)and
fused-silica columns (E3)were described. The preparation
and application of fused-silica columns were reviewed (E4).
Good thermostability and inertness were obtained in the
preparation of fused silica with in situ cross-linked phases by
using a cross-linking agent composed of dicumyl peroxide and
tetra(methylviny1)cyclotetrasiloxane (E5).Colloid particles
were used to stabilize polar cyanoalkyl stationary-phase
coatings on glass capillary columns (E6).Blum described the
preparation of a high-tem erature stable glass capillary column coated with a 20% $phenyl-substituted methoxy-terminated polysiloxane (En. The column is stable at temperatures as high as 430 "C. Welsch studied the thermal
immobilization of hydroxy-terminated silicone phases in
high-temperature-silylatedglass capillaries (E8).By analysis
of the volatile reaction products formed during the bakin
procedure, a reaction scheme to explain cross-linking an
surface bonding of hydroxy-terminated silicone phases was
developed. In a comparative study of Superox 20M immobilized in different ways, columns exhibited a transition zone
from adsorption of solutes at low temperatures to absorption
at higher temperatures (E9). Immobilization of chiral phases
for enantiomer separation was studied by Lai (EIO). A tentative mechanism of the immobilization reaction was suggested, thermal immobilization was promoted by the presence
of free carboxyl groups in the stationary phase.
Other papers reported new developmenta in the preparation
of WCOT columns (Ell-El4). tert-Butyldimethylsilylated
cyclodextrin was compared to permethylated cyclodextrin as
a chiral phase (Ell).Hydroxyl-terminated (3,3,3-trifluoropropy1)methyl lysiloxane columns were found to be useful
up to 330 "C &la. The addition of alkoxysilane as polyfunctional cross-linkers resulted in an inert, stable film with
low catal ic activity. Wojcik reported preliminary results
on the G evaluation of interpenetrating polymer networks
prepared from porous polymer beads (E13).A novel derivatization technique was described that should result in
shortened analysis time and improved column performance.
Conditions of glass WCOT inner surface modification by using
d
F
an aqueous solution of ammonia were studied by Ciganek
(E14).His method of static silylation of columns was reported
to provide a mechanically stable porous layer 1-10 pm thick.
In another study, it was shown that the olarit of the
fused-silica substrate affecta the inertness antrepr0d;ucibility
of the final coated columns (E15).Computer modeling was
used to develo new stationary hases for optimum separation
of c h l o r i n a d dibenzodioxinrdibenzofuran isomers (E16).
Results were used to manufacture new fused-silica WCOT
columns for commercial sale. Factorial designs were also
employed ta optimize stationary-phasecross-linking conditions
(El7). A predictive model as a function of the variables of
the cross-hnkingreaction was developed which resulted in the
production of columns of superior performance and sisnificant
improvements in reproducibility.
Other developments included the study of temperature
dependence of dead time as determined by methane retention
(EM)and the determination of the limitations in the assumption of negligible f i i thickness in WCOT chromatography (E19).Reviews have appeared on the usefulness of
deactivated metal WCOT column in high-temperature GC
(EN)and on recent advances in the use of wide-bore PLOT
columns for the analysis of gases and volatiles (E21).
INSTRUMENTATION AND DETECTORS
In this section, recent advances in GC instrumentation and
analytical methodologies related to instrumentation are reviewed in two sections including introduction of and detection
of samples. The d o n on injection focuses on methods which
have been used for the introduction of samples in the liquid,
supercritical fluid, and vapor phasea. The section on detection
reviews ionization, optical, and miscellaneous detection
methods.
Sample Introducilon
Liquid Samples. With few exceptions, the bulk of recent
research on and development of gas chromatographic injectors
has focused on problems associatedwith increasing the volume
of sample which can be introduced onto capill
columns.
From standard methods of split and splitless liqxin'ections
to the more exotic methods of direct supercritical duid extraction onto a GC column, the emphasis has been on increasing the amount of sample applied to capillary columns
without sacrificing its resolving power.
Investigations of variables for splitless injection have been
reported and optimized to reduce effects of back-flushing (F1)
and increases performance for base/neutral determination
using EPA Method 625 (F2).To com ensate for injector
overflow in the classical s litless metho8, injector chambers
should be large comparetto the volume injected (F3).For
larger volume injections, precolumns can be employed (F4).
A packed column (F5)and retention gap method (F6)prior
to an ordinary capillary column permit 100-pL injections.
Direct sample loop injections up to 100 pL onto a 0.32-mm
capillary column were found reproducible with 1%RSD (F7,
F8). On-line coupling of gas chromato aphy with a continuous liquid-liquid extractor was possgle with an injection
valve that permitted the introduction of 4 pL of vaporized
sample directly into the injection port of a standard GC system
(F9).
Conventional split splitless injectors can be converted to
on-column injectors FlO). Higher resolution can generally
be achieved with on-column injections although the sample
capacity is usually less than splitless in'ection methods. In
a comparison of cold on-column and spiitless injections, the
on-column method was found to be more precise (F11).
Lar e-volume (up to 200 pL) on-column injections can be
mate by usin a retention gap with a solvent diversion device
(F12,F13). %uffered samples can be injected if the column
is routinely rinsed and the retention gap is periodically replaced (F14).
Although more difficult to operate quantitatively, s lit
) b g e volumes. #e
injection is still commonly used ( ~ 1 5for
use of the cking material in the injector linear aided splitting
(F16)w h i r stop-flow split injection was found to prevent
sam le vapor overflow and aerosol splitting (F17). Other
metRods for lar e volume injections include solute focusin
(F18),sustaine! chromatographic evaporation (F191,an!
ANALYTICAL CHEMISTRY, VOL. 64, NO. 12, JUNE 15, 1992
173R
GAS CHROMATOGRAPHY
programmed temperature vaporizing vapor overflow (F20).
This last method can accept large volumes of solvent from
syringe injections and also the mobile phase from a liquid
chromatograph.
Because liquid chromatography can be used as a highresolution cleanup procedure prior to as chromatography
(FZI), sample introduction from liqui chromatography is
becoming increasing popular (FZZ). For example, size-exclusion chromatography can be used to separate triglycerides
from volatile pesticides before pesticide analysis by GC (F23).
In one coupling method, a precolumn retains the solute while
the solvent is vented (F24).In another, a 10-port valve assists
in the evaporation of solvent (F25).
Supercritical Fluid Phase Injection. A highly active
area of research and development in sample introduction
methods for gas chromatography has been that conceived by
S. B. Hawthorne (F26, F27). Direct on-line coupling of supercritical fluid extraction (SFE) with gas chromatography
has been found to be rapid (I?%), ve-tile (F29,F30),sensitive
(F31),
reproducible (F32),
and quanhtative (F33,F34). effect^
of microextractor cell geometry have been correlated with
supercritical fluid chromatography (SFC) data (F35). After
extraction,the sam le must be focused onto the column. This
was accomplished i y Tenax trapping (F36)and cryofocusing
(F37).Programmed temperature vaporization made it possible
to combine solute trapping with the elimination of high extraction fluid flows (F38).On-line coupling of supercritical
fluid extraction with multidimensional microcolumn liquid
chromatography-gas chromatography was also demonstrated
(F39).Off-line, SFE is used for chromatographyby collection
of samples in suitable solvents and collection apparatus (F40).
One major advantage to SFE as the pre aration step for gas
chromatogra hy is that extraction and erivatization can be
accomplishe simultaneously (F41).
Gas Sample Injection. When large volumes of vapor are
injected into a gas chromato aph, methods to focus or concentrate the sample onto the ead of the column are required.
The most common method is cryofocusing. One new configuration for cryogenic focusing of vapors onto capillary
columns recommends modifyinga split/splitlesa injection
by plugging the carrier gas and septum purge lines an inserting a cryogenic focusing interface through the septum
(3'42).Cryogenic focusing can be very efficient. For exam le,
a nitrogen-cooled cold trap produced injection band wi ths
of 10-20 ms (F43).Although cryofocusing with nitrogen is
considered to be the most efficient, the use of ice-acetone is
recommended if a sample has a high-moisture content (8'44).
Sample focusing can also be accomplished during the desorption step if the effect of the thermal gradient is optimized
(F45).Coupled with cryofocusing, this produces a simultaneous double thermal focusin effect. Resistive ohmically
heating of a thin layer of me&, gold applied to the column
near its inlet provided one method for thermally desorbing
solutes which have been cryogenically trapped on a capillary
column (F46).
For field analysis and applications where cryofocusing is
inconvenient, microtraps packed with suitable sorbents rowhile membranes &ow
vide efficient band-focusing (F47,F48)
the focusing and injection of highly volatile compounds (3'49).
Purge and trap methods can be used for headspace analysis
from a Curie-point pyrolyzer (F50), but reduced ressure
injections require special valving to compensate for aseline
variation (F51).
Other developments in vapor-phase injections pertain to
calibration methods, high-temperature gas chromatopaphy,
and high-speed chromatography. Cryotrapping for dlfferent
periods of time enabled multipoint calibration with a single
gas standard (F52). Investigations of multiway sampling
valves of various volumes can also be used to simplify the
calibration process (F53). Quantitative investigation of the
thermal degradation which occurs in various in'ectors was
investigated with thermolabile compounds (F54). expectad,
cold on-column injections were more effective than hot
splitless injections. However, rogrammed temperature vaalso prove to be an effective
porizin injections up to 200
methocf for injecting thermolabile compounds. Temperature-pro ammed injectors have been developed for use up
to 450 OF(F55).
The current challenge to the development of novel injection
methods is for high-speed chromatography (F56). In high-
t
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8""
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08
174R * ANALYTICAL CHEMISTRY, VOL. 64, NO. 12, JUNE 15, 1992
speed gas chromatography, resolution and detectability are
usually limited by the injection method. Although direct vapor
(8'57)and liquid (F58)injection devices have been investigated,
interest has also been on modulated thermal desorption
methods (F59).,Signal averaging of a series of modulated
injections provides a total sample chromatogram (F60)which
can be used for continuous on-line analysis (F61).Problems
associated with thermal modulation include thermal decomposition (F62),although thermal decomposition modulation
can be used as a chemical modulation device for correlation
chromatography (F63).
DETECTORS
Ionization Detectors
Flame Ionization Detector. The flame ionization detector
(FID) is the most common GC detedor (GI).Although widely
used for chromatographic detection for over 30 years, the
mechanism of FID response is still not completely understood.
For example, in a m n t study flame ionization responses were
23% lower for total hydrocarbons than for the same compounds separated by as chromato aphy ((2).Although
some of this effect can %e contribut$to sample introduction
methodology, FID response differences among specific hydrocarbons may also be important. Earlier concepts on FID
response factors based on effective carbon number were updated usin naphthalene as the internal standard (C3). In
addition,e!t use of carbon weight factors provides a novel
approach for quantitative analysis with FID (G4).A method
for the analysis of h drocarbon radicals in flames by scavenging with dimethyrdisulfide was developed and may prove
useful for the investigation of the FID mechanism (G5).
Other investigations of flame ionization included fast response detectors (G6),operation with autosampler injection
(G7),and the use of nontraditional flame-formingagents (G8),
especially as they relate to the selective detection of halogen-containing compounds. Investigations of an oxygenspecific flame ionization detector found that response was
proportional to percent oxygen and that response factors
remained constant in the 0.5-10% volume range (G9).
Hydrogen Atmosphere Flame Ionization Detector
(HAFID). The HAFID is a selective detection method for
organometallic compounds and was investigated with mass
spectrometry (GIO). Response ions were found to be ion
cluster series involving Si0 and SiOz and their hydrates. Even
though the detedor reaponds to metal-con
no metal-containing ion species were observe in the mass
spectrometer. On the basis of these observations and the
conclusion that selectivity in the detector was based on differences in ion mobilities, a novel modification to the HAFID
was made which significantly enhanced selectivity toward
organometalliccompounds (G11).In addition hydrogen flow
requirements were reduced with a sheathed-flowconfiguration
7
(G12).
Ion Mobility Detector. Differences in gas-phase ion
mobilities can be measured directly and are used as the basis
for selective gas chromatographic detection with an ion mobility detector (IMD). By monitoring of the mobility of
chloride and bromide ions, selective detection of a brominated
species is possible in a complex mixture of polychlorinated
biphenyls (G13).Direct axial sample introduction of analytea
into the IMDwas found to decrease detector dead volume and
to increase sensitivity (G14). Detection limita for this direct
axial sample introduction method was found to be below 1
fmol s-* for several compounds (G15). Ion mobility de+$ion
of C1-CI hydrocarbons (G16)and of polydimethylsilicone
oli omers (1317)was also reported.
klectron Capture Detector. For electronegative compounds, the electron capture detector (ECD) provides responses similar to those of the IMD without the added selectivity of mobility but with an extended linear operating
range. Investigations of s ace char e effects, which limit
detector linearity, cast dou% upon t f e general assumption
of the complete removal of electrons from the detector by the
voltage pulse (G18).Effeds of tem rature on response for
CSz were studied (G19)while phodtachment after electron
capture was found to offer promise for the selective detection
of iodinated hydrocarbons (C20). Radiefrequency modulation
of a e3Nielectron capture detector with argon as carrier gas
provided detection limits down to 0.1 ppm for organic com-
GAS CHROMATOQRAPHY
pounds and 1 ppm for inorganic gases (G21).
Photoionization Detectors. Although the photoionization
detector (PID) is regarded as a nonselective detector (G22),
sulfur-specific detection in a r can be attained by converting
organic compounds into H2S, acid halides, NH3, water, and
methane with a reductive pyrolyzer (G23).Of these reductive
products, only HzS provides photoionization response. For
aromatic hydrocarbons and n-alkanes, photoionization response is independent of both reasure (G24)and temperature,
although there is correlation etween UV lamp emission and
detector temperature (G25).
Nitrogen-Phosphorus Detector. Through the years, one
of the more mechanistically controversial detectors has been
the nitrogen-phosphorus detector (NPD). Producing n ative
ions as charge carriers for the response, it is the on y gas
chromato aphic detector selective for nitrogen-containing
compoun s (G26,G27). Recent investigations indicate that
the response curve for the NPD may not be as linear as once
and a more thorough investigation of the dethought (GB),
tedor’s response mechanism indicated that all steps leading
to the formation of ionic species may occur only on the surface
of the alkali-ceramic bead (G29).
The realization that the NPD is a surface ionization process
has led to the development of the surface ionization detector
(SID) (G30).This detector, in contrast to the NPD, is normally operated in the positive mode, although both positive
and negative ions can be detected with good selectivity for
compounds having a low ionization potential (G31).Using
both the positive and negative mode, it serves as a selective
and sensitive GC detector for molecules containing I, Br, F,
PO2,NOz, CN, NH2, polycyclic aromatic hydrocarbons and
organometallics (G32).
Other Ionization Detectors. Other ionization detection
methods which have been investigated include glow discharge
(G33)and laser-enhanced ionization spectrometry (G34).
t
7
f
Optical Detectors
The greateat interest in GC detection over the past few years
has been in the use of the plasma emission detector (PED).
While there are a variety of PEDs, many are based on miOne PED is called
crowave-induced plasmas (MIPs) (HI).
an element-specific detector (ESD) and at 450 OC provides
simultaneous measurements of four elements at a picogram
per second detection limit (H2).These detectors are also
referred to as atomic emission detectors (AED) (H3).
Plasma Emission Detectors. PEDS provide specific detection for a variety of elements (H4)such as organometallic-containing compounds (H5-H8), halogenated comand hydrogen-containing organic compounds (H9-H11),
The lowest detection limits reported were 1,
pounds (H12).
7,9, and 4 pg s-* for carbon, hydrogen, chlorine, and bromine,
At the nanogram level, the PED appears
res ectively (H13).
toe! a powerful tool for both metal and non-metal containing
compounds. It proved to be highly selective in a comparison
among other selective GC detectors for the determination of
10 peaticides in agricultural commodities (H14).
Investigations
of a computerized photodiode array for use with PED produced selectivities for chlorine and bromine with respect to
carbon of 24000 and 13000, respectively (H15).
In addition to element-selective detection, PEDs can be
used for the determination of empirical formulas (H16).
Structure, however, can have an effect on the determination
H18). The largest errors in moof empirical formulas (H17,
lecular formula coefficients were found for hydrogen (H19).
Chromatographic interfacing parameters and instrumental
operating parameters of PEDS have been studied in detail
(H20,
H21).A solvenbventing interface was developed on the
basis of fluid logic in which interference from the solvent could
be eliminated without baseline shifts or increased dead volume
(H22).Laminar flow cells were also evaluated (H23).
Other Plasma Emission Sources. The analytical behavior of a modulated power MIP was best at a pressure of
50 Torr (If241but noise was found to be similar to convenThe reflected power from an MIP was
tional MIPs (H25).
reported to have potential for GC detection but detection
limits for carbon and hydrogen were in the u per nanogram
Inductively couplef (H27)
and caper second range (H26).
plasmas were evaluated, and depacitively coupled (HB)
tection limits for several non-metallic elements ranged from
0.2 to 50 pg s-l when radio-frequency plasmas were used
Microplasmas, produced
instead of microwave plasmas (H29).
by ArF excimer lasers, were found to have a photometric
detection limit of 10 ng of acetylene after gas chromatography
(H30).
Fourier Transform Infrared (FTIR) Absorption Detectors. Detectors based on FTIR principles for gas chroH32).For
matography also received some attention (H31,
convenience and the detection of unstable compounds, on-he
Although detailed studies were
methods are preferred (H33).
completed to enhance sensitivity for on-line detection (H34),
off-line detection appears to be more sensitive and versatile
(H35).Other advantages to off-line detection is that the
and that the low-temperasample can be cryotrapped (H36)
ture spectra more closely compare to conventionally recorded
spectra (H37).Spectral identification of target compounds
after gas chromatographicseparation can be accomplished for
fully separated compounds but spectral subtraction or corroborating detection methods are needed for coeluting comThe Gram-Schmidt construction method was
pounds (H38).
found to roduce a better si nal-to-noise ratio for FTIR
compountfidentification (H397.
Flame Infrared Emission (FIRE). This spectrometer
is a relatively new method of detection for GC (H40).
Dual-channel detection reduces the adverse effects of flame
although HCl and
background on signal to noise ratio (H41),
HF emissions in a hydrogen/& flame result in detection limits
of only 200 ng s-l with selectivity ratios of 760 for F and 100
for C1 (H42).
Even though these detection limits and selectivities are not competitive with other selective detection
methods, one advantage of FIRE is that it can be used with
A theoretical model has
nonselective FID detection (H43).
been developed to calculate the detector’s response (H44).
Gas-Phase Fluorescence (GPF). Fluorescence induced
by electron impact can produce both selective and universal
response as a gas chromatographic detector (H45).Laserexcited fluorescence provided high spectral resolution moand the addition of
lecular fluorescence of GC eluates (H46),
naphthalene va r to the effluent from a GC column provided
a means for i n g e c t fluorescence detection of nonfluorescent
species (H47).
Chemiluminescence Detector (CD). This detector has
and is commonly used
a variety of modes of operation (H48)
when the excited species is formed in a flame to produce a
phoshorus- or sulfur-selective response. This flame photometric detector (FPD) will also respond to ammonia but is
selective against other nitrogenous interferences (H49).
Modification of another commercially available CD, the
thermal energy analyzer (TEA), permitted the detection of
trace explosives after GC (H50). Also, a commercial instrument for the detection of NO, was interfaced to GC and
compared with GC/ECD for the determination of peroxyacetyl
nitrate (H51). Reactions with ozone can produce chemiluminescence for the detection of sulfur compounds (H52) and
The sulfur detector produces a
nitrogen compounds (H53).
linear response, has a sulfur-to-carbon selectivity greater than
106,is not appreciably affected by solvent quenching, and has
a nearly equimolar response to various sulfur species (H54).
Fluorine-induced chemiluminescence has also been investiated. This method appeared promising for the detection of
iologically methylated tellurium, selenium, and sulfur compounds (H55) and for the detection of phosphine, alkylphosphines, and monophosphinate esters (H56).Surfacecatalyzed reactions were found to produce redox chemiluminescence for GC detection (H57).
E
Mlwelianeous Detectors
Electrochemical Detectors. The best known of the
electrochemical detectors (EDs) is the Hall electrolytic conductivity detector (HECD) (ZI). Factorial optimization of the
HECD provided maximum sensitivity for organochlorine
compounds (12).Thin gap microelectrodes (13)and a theory
for the sensitivity and selectivity of microelectrode voltammetric detection (14)were reported.
Other Detectors. Other detection methods which appeared in the literature during this review period include
a surface acoustic wave dephotoacoustic detectors (Z5,16),
and a sonar detector
tector ( I n ,radioactivity detectors (Z8,19),
(110).A general discussion of principles of operation, charANALYTICAL CHEMISTRY, VOL. 64, NO. 12, JUNE 15, 1992
* 175R
GAS CHROMATOGRAPHY
acteristics, and detection limits of many GC detectors was
provided (111).
GAS CHROMATOGRAPHY-MASS
SPECTROMETRY
As was the case in the previous review of this series, not
many developments occurred in the field of GC-MS that could
be considered fundamental in nature, although a large number
of applications continue to be reported. Many of these have
been summarized in a recent review (JI).A few papers reported developments in the GC-MS interface (J2-J4). Ligon
constructed an open-split-type interface that provides complete solvent diversion and relatively invariant ion source
conditions (J2). This is important to obtain reproducible
negative chemical ionization results. A simple, direct GC-MS
interface was designed for the Finnigan-MAT ion trap detedor
by Stout (53). Modifications to an open-split interface based
on friction-typeeffluent splitters were also reported (54). Two
different groups showed how an aluminum-clad WCOT column can be connected to a high-resolutionmass spectrometer
to avoid electrical arcing but maintain GC performance (J5,
J6). Tong described the advantages of GC-MS selected-ion
?e
monitoring analysis in the mass profile ( M P )mode (57)..
examination of MP peak shape and central mass shlft in
addition to changes during GC elution reveals the presence
of interfering compounds and can ive accurate mass measurements for those interferences. pplication of time array
detection to WCOT column GC was demonstrated by Erickson (J8). By using a conventional time-of-flight mass
spectrometer, up to 20 mass spectra per second were generated; which gave accurate reconstructed chromatograms and
no distortion of mass spectra in spite of rapidly changing
analyte concentrations in the WCOT column peak. Tandem-in-s ace and tandem-in-time mass spectrometers were
compareffor the detection of GC effluents (J9). It was shown
that Taguchi design experiments can be used to o timize
GC-MS performance (J10).Karjalainen (JII)descriged the
computer-assisted alternating regression method for the reconstructionof pure spectra in GC-MS analysis. This method
can be used to locate novel compounds that have overlapping
spectra. Ligon demonstrates new methods for postcolumn
derivatization in GC-MS analysis by connecting the output
of a conventional split-type WCOT column injector to the
region between a capillary gas chromatograph and the mass
spectrometer (J12). Derivatizations can be performed on a
peak-by-peak basis. Abdel-Baky demonstrated the use of
GC-negative ion MS for the detection of as low as 150 ag of
strong electrophores (J13).
x
QUALITATIVE AND QUANTITATIVE ANALYSIS
Recent reviews have discussed qualitative and quantitative
analysis in GC ( K I )and selectivity tuning (K2). Few papers
concerning new develo menta in quantitative analysis were
encountered; most stufies were concerned with refinements
to various retention index schemes and structure-retention
correlations. A review listing some 900 Kovats indices for 400
monoterpenes and sesquiterpenes on methylsilicone and
Carbowax 20M phases has appeared (K3). Methods were
presented for the determination of the universal retention
index (K4). A procedure was described that allowed the
calculation of linear temperature-programmed retention
indices from Kovats retention indices on a given stationary
phase (K5). In most cases, calculation accuracy was better
than 0.5 retention index units. Pen discussed the prediction
of retention indices for silylated Jerivatives of polar compounds (K6).The use of the UNIFAC group contribution
method to predict retention on low molecular-weight stationary phases (K7)
and on polymer phases (K8)was studied.
Several studies examined the use of cubic splines to calculate
temperature-programmed retention indices (K9-Kl1). Fernandez-Sanchez tested several methods of calculating programmed temperature retention indices and preferred the
cubic spline approach (K12). Prediction of retention data
and/or structureretention correlations were presented for
the Cg-Cl2alkylbenzenes (K13), PCBs (K14), chlorinated
bromo- and bromochloro dioxins and
dibenzofurans (K15),
and for stimulants and
furans (K16),anabolic steroids (K17),
narcotics (K18). Gerbino reported the GC identification of
176R
ANALYTICAL CHEMISTRY, VOL. 64, NO. 12, JUNE 15, 1992
complex mixtures of halomethanes and haloethanes by correlating retention with vapor pressure (K19). Practical
guidelines for generating a simulated as chromatogram and
a new approach for the chromatograptic indexing of organic
compounds were presented by Mowery (K20). Jorgensen
described a model that could be used to accurately predict
GC-flame ionization detector response factors from molecular
structures (K21).
MISCELLANEOUS INFORMATION
Recent developments in supersonic jet spectrosco y were
reviewed by Goates (L1).Cramers reviewed recent Lvelopmenta relating to speed of separation, detection, and identification limits in WCOT GC and GC-MS (L2). Additivity
rules and correlation methods in GC were also reviewed (L3).
New developments were described for large-volume in'ection
Grob outlined a solvent evaporation tec'kuque
in GC (U-U).
that involves a modified programmed temperature vaporizing
injector (L4). The technique automatically optimizes operation parameters, and the loss of volatile materials is minimized. Watanabe developed a direct injection method for
large-volume m p l e s that avoids severe tailing of the solvent
peak by usin a packed column injector leading into an ordinary WCO% column (L5). Another approach to largevolume injection was described by Liu, who employed thermal
High-speed
desorption modulation and signal averagin (U).
GC was investi ated in several studies &.7-L10). Gaspar
discussed the tteoretical and practical aspects (L7). Liu
generated chromatagrams in as little as 4 s by using on-column
A prototype cryofocusing
thermal desorption modulation (U).
system for producin narrow injection bands for high-speed
GC was described 6 9 ) . Thermal decomposition of some
hydrocarbons and chlorinated hydrocarbons in metal capillary
tubes used for high-speed GC was studied by Klemp (L10).
Reviews on high-temperature GC analysis have been published
(LI1,L12). Optimization of column temperature in isothermal
separations (L13),and optimal carrier gas velocities in highspeed GC (L14) have been studied. Havesi described the
application of Fourier transformations in high-resolution GC
for trace analysis (L15).There were several papers that de.
scribed developments in headspace analysis ( ~ 5 1 6 4 2 3 ) A
critical review on heads ace analysis was repared by Ioffe
(L16).Other reviews ckcussed the headpace analysis of
pharmaceuticals (L17) and solid samples (L18).Methods of
equilibrium concentration for the GC determination of trace
volatiles were also reviewed (L19). Ettre discussed the influence of sample volume on headspace GC results (L20).
Tabera used a programmed-temperature vaporizing injector
to optimize the dynamic headspace sampling of trace volatile
components of grape juice (1521). Reliable quantitation for
compounds at concentrations of 0.005 mg L-l with an average
relative standard deviation of 15% was reported. The use of
chemometrics for optimization of GC performance was reported in several studies ( L 2 2 4 2 9 ) . Bautz described the
performance of a computer method to predict retention,
bandwidth, and resolution for programmed temperature GC
separations with average error better than 10% (L22). A
simplex method was used to optimize selectivity for the separation of 10 compounds by GC (L23). Dolan investigated
the changes in band spacing as a function of temperature
through computer simulations (L24). Artificial neural networks as a pattern recognition tool for chromatographic data
were described by Long (L25). Other chemometrics studies
included the application of multivariate analysis to the selection of test solutes for characterizing stationary-phase selectivity (L26),simples optimization of a temperature-programmed WCOT GC separation (L27),the use of computer
simulation for GC method development (L28),and the use
of the simplex algorithm for the deconvolution of complex GC
profiles (L29). Oroe reported on the effect of stationary phase
on predictions of the statistical model of overlap from gas
chromatograms (L30). Internally consistent results could be
obtained unless the polarities of the sample components and
stationary phase were highly mismatched. Kollie introduced
a new parameter for the determination of the capacity of a
stationary phase to enter into orientation and hydrogenbonding interactions (L31). Bemgaard introduced four new
terms to the Golay-Giddings equation and evaluated them
for their significance (L32). Belfer described non-steady-state
GAS CHROMATOGRAPHY
GC using WCOT columns (L33).
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X-ray Spectrometry
Szabina B . Torok
Central Research Institute for Physics, P.O.Box 49, H-1525 Budapest, Hungary
Ren6 E . Van Grieken*
Department of Chemistry, University of Antwerp (UIA),B-2610 Antwerpen- Wilrijk, Belgium
A. OVERVIEW
During this review period covering 1990 and 1991, about
500 publications appeared about X-ray spectroscopy (XRS)
measurements, and a few hundred more concerning X-ray
instrumentation, optical elements, and the use of X-rays in
plasma diagnostics. Since this set of publications is nowadays
easily accessible by abstracting services, this review will not
aim to be complete and will consider exclusively those papers
that discuss novelties of most interest for X-ray spectroscopists. During the preparation of this review, we screened
about 400 publications in various languages; non-English
180 R
articles are only included if they are acceptably accessible.
Also, we will only exceptionally refer to conference abstracts.
At the beginning of many paragraphs the reader will find
references to books and conference proceedings as well as to
review articles, where extended information will be available
on each particular subject.
the review period,major developments in XRS were
triggere by the improvement of beam techniques related to
charge particle accelerators, and the availability of intense
small size beams. For this reason, se arate ara a he will
be devoted to synchrotron radiation &R) in%ced[rXP1S and
00Q3-270Ql92l0364-18QR$1Q.0010 0 1992 American Chemical Society