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, d ~ 229-236. , (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
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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
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(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
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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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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
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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
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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
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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-
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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
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SOLID SUPPORTS AND ADSORPTION (Cl) Bruner, F.; Crescentinl, G.; Manganl, F. Pure Appl. Chem. 1989,67 (1 l), 1997-2000. (C2) Pankow, J. F. J. Chfomatogr. 1991,547 (1-2), 488-93. (c3) zhelvot, V. I.; Shaiaeva, M. E.; Gavrllov. V. Y.; Fenelonov, V. B.; Ovsyannikova, I. A.; Malakhov, V. V. J. Chromatogr. 1989,472(1), 155-81. (C4) Bek. W. R.; S~pina,W. R. J . ChrOmtCgf. 1989. 477. 105-12. (C5) Ludwig. S.; Schmidt, H. D. J . Chromatogr. 1990,520, 89-74. (C8) Cao. X. L.; Cdenutt, B. A,; Slng. K. S. W. J . Chromatogr. 1991,555 (1-2), 183-90. (C7) Nardln, M.; Balard, H.; Paplrer. E. Carbon 1990,28 (l), 43-8. (C8) Levlek, L.; S c h u k J. Langmuk 1991, 7 (5), 978-81. (C9) Mertltblbpklns, M. B.; Gilpln, R. K.; Jaronlec, M. J. Chromatog. Sci. 1991,29 (4), 147-52. (C10) Sldql, M.; Llgner, 0.; Jaglallo, J.; Baiard, H.; Papker, E. chrometopphle l989,28(11-12), 588-92. (C11) BHkrskl, B.; Wojclk. W.; Dawldowlcz, A. L. Appl. Surf. Scl. 1991,47 (l), 99-108. (C12) Tsutsuml. K.; ohsuga, T. colloid Polvm. Sei. 1990,268 (l), 39-44. (Cl3) C%ntOScu, C.; Jaglelb, J.; Schwarz, J. A. J . Catel. 1991, 737 (2), 433-44. (C14) Webs. E.; Dabrlo, M. V.; Herrero, C. R.; Acosta, J. L. ChromatoQr@h 1991,37 (7-8), 357-81. (C15) Mlknjic, S. K.; Ceranic, T. S.; Petkovlc, M. D. Clwometographle 1989, 27 ( 7 4 , 308-10. (C16) Paplrer, E.; Penln, J. M.; Siffert. B.; Phllipponneau, 0.J . cdlold InterftX8 &/. 1991, 7 4 4 (1). 283-70. (C17) Rybdt, T. R.; Wall, M. D.; Thomas, H. E.; Bramblett, J. W.; Phillips, M. J . cdbld Interfece scl. 1990. 738 (I), 113-21. (C18) Pushpa, K. K.; Rao, K. A.; Iyer, R. M. J. Chromatogr. Sci. 1990,28 (e), 441-4. (Cl9) Banaldr, 0. S. Zh. Anal. Khlm. 1989,44(10), 1918-18. (C20) Zlatkls, A.; JlaO, A. Chr4metogfaphle 1991. 37 @-lo), 457-64. (C21) Elceman, G. A.; h a , A. S. J. Chromatog. 1991,549 (1-2), 273-81. (C22) Lafa, A. S.; Eiceman, G. A. J . Chrometog-. 1991,549 (1-2), 283-95. (C23) Lee, H. L.; Luner, P. J . cdldd Interface Scl. 1991, 746 (l), 195-205. (C24) m v a y a , L. A.; Ekekov, Y. A.; Hradll, J.; Svec, F. J. Chromatop. 1991,552 (1-2)- 365-70. (C25) Larkrov, 0. G.; Pebenko, V. V.; Platonova, N. P. Zh. F k . Khlm. 1989,63 (9), 2533-5. (C26) ChepPeW, P. J. C.; Wllllams, D. R. J . Adhes. Sci. Techno/. 1990,4 (1). 7-18. (C27) Neyak, V. S. J . Chrometcgr. 1990,496 (2), 349-56. (C26) Nayak, V. S. J . Chrometogr. 1991,556 (1-2), 425-32. (C29) Kovakva, N. V.; Levlna, E. F.; Nikltln, Y. S.; Protonlna, 1. S. Zh. Fk. K h h . 1989,63 (10). 2887-74. (C30) Zagorevskaya, E. V.; Kovaleva, N. V.; Kullkov, N. S.; Nlkkin. Y. S.; Protomine, I. S.; Shcherbinln, B. V. Zh. Flz. Khlm. 1989, 63 (12), 3289-94. (C31) M y k T. A.; PMMps. C. S. 0. J . Chmmetop’. 1991,557(1-2). 495-99. ( a 2 1 B,J. H.; DHlard, J. 0.Langmuk 1991,7(8), 1713-8. (C33) R&. J.; QJkchon, G. J . phvs. Chem. 1991,95 (10). 4098-109. (C34) Anthony, L. J.; Molland, R. A. J . NOn-CIySt. SO/& 1990, 720 (1-3). 82-92. (cas) Tl$uck, A. C.; Manson, J. A. J. Appl. Po&m. Scl. 1991. 42 (2), 427-38. (C38) Tljbug, I.; Jaglelb, J.; Vidal, A.; Papker, E. Langmuk 1991,7 (lo), 2243-47. (C37) Katsanos. N. A.; Karaiskakls, 0.; Vasslhkos, C. Pwe Appl. Chem. 1989,67 ( l l ) , 2057-58.
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GAS CHROMATOGRAPHY SORPTIONPROCE88ESAND80LVENTS
(Dl) Hami, T. J. High Resolut. Chrometogr. 1990, 73 (3), 178-81. (02) Hanai, T.; Hong, C. J . High Resdut. Cbromatogr. 1989, 72 (5). 327-32. (D3) Gerasimnko, V. A.; Nabivach, V. M. J . Chromefogr. 1080, 498 (2), 357-66. (D4) Gerasimenko, V. A.; Nablvach, V. M. Zh. F k . Khlm. 1989, 63 (5), 1360-1. (D5) Heberger, K. chromatograph& 1990, 29 (7-8), 375-84. (D6) Kohnen, I.0. 0.; Mantykoski. K. M. J . Chfomatogr. 1989, 477(2), 237-36. (D7) Sasaki, Y.; Tekagi. T.; Kawaki, H.; Fujll, S.; Masuda, F. Chem. pharm. Bull. 1990, 38 (4), 948-50. (DE) PaDD, 0.; SzaSZ, G.;Orfl. L.; H w ~ z I. , J. Chfomato,y. - 1991, 537 ' (1-2); 371-6. (D9) Papp, 0.; Szasz, G.; Klkisi, J.; Hermecz, I. J . c h f o ~ ~ o g1991, r . 537 (1-2); 365-70. (D10) Papp, 0.; Szasz. G.; Kikisi. J.; Hermcz, 1. J . Chromatogr. 1991, 537 11-2). -,. 377-83. ( D l l ) Ligner, G.; Sidql, M.; Jagiello. J.; Balard, H.; Paplrer, E. Chromatographie 1990, 29 (1-2). 35-8. (D12) Jaroniec. M.: Lu. X.: Madev. R. J . MYS.Chem. 1990, 94 (15). . . ' 5917-21. (D13) GHpin, R. K.; Jaronk, M.; MartinHopkins, M. 8. J . Chfomatogf. 1990, 573,1-11. (D14) Haaggiund, I.; Janak, K.; Blomberg. L.; Bemgaard. A.; Claude, S. 0.; Lymann, M.; Tabacchi, R. J. Chrometogr. Scl. 1991, 29 (g), 398-402. (D15) Golovnya, R. V.; Grigor'eva. D. H.; Vasil'ev, A. V. J . High Resdut. Chfomatogr. 1990, 73 (l), 47-51. (D18) Kohoutova, A.; Smolkova-Keuiemansova. E.; Feiti, L. J . Chromatogr. 1989, 477, 139-44. (D17) Feilous, R.; LlzzaniCweller, L. Lolseau. A. M. J . High Resolut. Chromtogf.1990, 73 (11). 785-9. (D18) Osslcinl, L.; Perez, G.; Caponecchi, G.; Cristalll, A.; Sybiiaka, D.; Koscieiskl. T.; Goronowicz, J. J . Chrometogr. 1991, 547 (1-2), 283-9. (D19) Dobashi, Y.; Nakamura, K.; Saekl, T.; Matsuo, M.; Hara, S.;Dobashi. A. J. Org. Chem. 1991, 56(10), 3299-305. (D20) Jung. M.; Schmalzing, D.; Schurig, V. J. Chrometogr. 1001, 552 (1-2), 43-57. (D21) Armstrong, D. W.; LI, W.; Stalcup. A. M.; Secor, H. V.; Izac, R. R.; Seeman, J. I.Anal. Chlm. Acta 1990, 234 (2), 385-80. (D22) Golovnya, R. V.; Polanuer, B. M. J . chromatogr. 1990, 577, 51-66. (D23) Poole, S. K.; Kersten, B. R.; Poole, C. F. J. Chromatogr. 1080, 477, 9 1-103. (D24) Betts, T. J. J. Chrometogr. 1990, 504 (l), 186-90. (D25) Voelkel, A.; Janas, J. J. Chromatogr. 1991, 555 (1-2), 205-10. (D26) Munk, P.; Hattam, P.; Du, Q.; AbdaCAzlm, A. A. A. J . Appl. Potym. Sci.: Appl. Pobm. Symp. 1990, 45, 289-316. (D27) Du. Q.; Hattam, P.; Munk, P. J. Chem. Eng. Data 1990, 35 (3), 367-7 1. (D28) Evans, M. 6.; Haken, J. K. J . Chromefogr. 1989, 477, 217-26. (D29) Li, J.; Zhang, Y.; Dallas, A. J.; Can, P. W. J . Chromatogr. 1991, 550 (1-2), 101-34. (D30) Galin, M. Mecromokuhs 1990, 23 (1l), 3006-12. (D31) Larlomov, 0. G.; Petrenko, V. V.; Platonova, N. P. J . Chfomatogr. 1991. 537 (1-2), 295-303. (D32) Lee, H. L.; Luner. P. J . WoodChem. Techno/. Wl, 7 1 (2), 247-81. (D33) Oweimreen, 0.A.; AManabl, Y. T.; ACHawej. F. Y. J . Chem. Eng. Data 1990, 35 (2). 219-23. (D34) Ashraf, S. M.; Rajiah, A.; Krishna, M. R.; Rao, M. B. J . Chromatogr. 1089, 472 (l), 183-74, (D35) Cai, X.; Ma. C.; Zhu, J. " w c h l m . Acta 1990. 764, 111-8. (D36) Koppenhoefer, 6.; Lin, B. J . Chromefcgr. lS89, 487, 17-26. (D37) Galin, M. Wymer 1989, 30 (1l), 2074-9. Miyagi, R.; Sasaki, Y. Bull. Chem. Soc.Jpn (D38) Fujiwara, H.; Ohtaku, I.; 1989, 82 (1 l), 3428-32. (D39) Ghodbane, S.;Owelmreen. G. A.; Martire. D. E. J . Ckomatog. 19g1, . 556 (1-2), 317-30. (040) Golovnya. R. V. Zh. Anal. Khlm. 1991, 4 6 ( 8 ) . 1218-9. (D41) Kuningas, K.; Rang, S.;Kailas, T. Chromatogavephia 1989, 27(11-12), 544-8. \
WALL-COATED OPEN TUBULAR COLUMNS
(El) Sumpter, S. R.; WoOney. C. L.; Huang, E. C.; Markldes, K. E.; Lee, M. L. J . Chrometcgr. 1990, 577, 503-19. (E21 Abe. I.; Kameyama, K.; Wasa, T. chfOmafCgf8phk3 1989, 27(11-12), 631-2. (E3) Yln, H. F.; Huang, A. J.; Sun, Y. L. Chrometograph& 1989, 28 (5-8). 313-4. (€4) AI", 0.GIT Fachz. Lab. 198% 33 ( l l ) , 1141-2, 1144, 1146. (E5) Llu, H.; Zhang, A.; Jin, Y.; Fu. R. J . H@I Resdut. Chfomatogr. 1989, 72 (8). 537-9. (E6) Alexander, G. J . H@h Resolut. chrometogr. 1990. 73 (l), 85-8. (E7) Blum, W.; Eglinton, G. J . High Resolot. Cbromatogr. 1989, 72 (5), 290-3. (E8) Welsch, T.; Telchmann, U. J . H/gh Resolut. Cbromatcgr. 1991, 74 (3), 153-9. (E9) Femandez-Sanchez, E.; Femandez-Torres, A.; GarclaOomingwz, J. A,; Salvador-Moya. D. J . chrometogr. 1991. 556 (1-2). 485-93. (E101 Lai, 0.;Nicholson, G.; Muehleck, U.; Baver. E. J . Chrometosr. 1991. 540 (1-2), 217-23. ( E l l ) Blum, W.; Aichholz, R. J . H@I Resolut. Chromatogr. 1990, 73 (7), 515-8. (E12) Aichholz. R. J. Hk?h Resolut. &omatogr. 1990, 73 (l), 71-3. (E13) Wojcik, A. B. J . Chromafcgr. 1980, 502 (2), 393-400. 178R
ANALYTICAL CHEMISTRY, VOL. 84, NO. 12, JUNE 15, 1992
(E14) Ciganek, M.; Tesarik, K.; Horka, M.; Janak, K. Chem. Pap. 1991, 45 (I), 81-9. (E19 Broske, A. D. J. H@I Resdut. chrometogr. 1980. 73 (9,348-51. (EM) Tiernan, T. 0.;Garrett, J. H.; Wch. J. G.; Harden, L. A.; Lautamo. R. M. A.; Freemen, R. R. CapMary clvomefogmphu;Jennlngs, W. G., NIkeNy, J. 0.. Eds.; @ H & uI Heidelberg, FRO. 1991; pp 17-38. (E17) nyVer, K. J.; De Veaux, R. D. J . H@h Resdut. Chmmafogr. 1989. 12 (4), 208-12. (E18) Koppenhoefer, 6.; Laupp, G.; Hummel, M. J . Chrometogr. 1991, 547 (1-2), 239-45. (El9) Schisla, D.; Cerr, P. W. Chowtographla 1990, 29 (11-12), 608-8. (E20) Buyten, J.; Dwekot. J.; Peene. J.; Mussche. P. Am. Lab. 1991. 23 (12), 13-8, 18. (E21) DeZeeuw, J.; DeNiJs, R. C. M.; Zwiep, D.; Peene, J. A. Am. Lab. 1991, 23 (9). 44, 46-8, 50-1. INSTRUMENTATIONAND DETECTORS
Sampk lntroductlon (Fl) SihrlS, P. H. LC-OC 1989, 7 (7), 562-9. (F2) De Veeux, R. D.; Szelewski, M. J . Chfomatogr. Scl. 1989, 27 (9), 513-8. (F3) (Lob, K.; Bledermann, M. J. H/gh Resolut. Chromatogr. 1989, 72 (2), 89-95. (F4) Arrendale, R. F.; Stewart, J. T.; Martin, R. M. J . chrometogf. 1990, 576 (2), 307-18. (F5) Watanabe, C.; Hashlmoto, K. J . High Resolot. Chomatogr. 1990, 73 (9), 610-3. (F6) Hu, H.; Zhu, M.; He, Y.; Sun, K. J . Chromatogr. 1991, 547 (1-2), 494-500. (F7) Hagman, 0.;Roeraade, J. J. High Resolut. Chromefogr. 1990, 73 (7), 481-4. (F8) Marsman. J. H.; Pannenman, H. J.; Beenackera, A. A. C. M. J . Chroma-. 1989, 483, 111-20. (F9) Ballesteros, E.; (3eilego. M.; Vaicarcei, M. Anal. Chem. 1990, 62(15), 1587-91. (F10) Math" M. L.; bkkinen, V.; Rlekkola, M. L. Finn. &em. Lett. 1989, 76 (1-8), 13-7. (F11) h e d a l e , R. F.; Stewart, J. T. J. Hlgh Resdut. Chromatogr. 1989, 72 (1I), 749-52. (F12) Morablto. P. L.; Hiiier. J. F.; McCabe, T. J . High Resolut. chrometogr. 1989, 72 (5)- 347-9. (F13) Mccabe, T.; Hiller, J. F.; Mareblto, P.L. J . High Resolut. Chromatogr. 1989, 72 (8). 517-21. (F14) Ellington, J. J.; Trusty, C. D. J . High Resolut. Chfomatogr. 1989, 72 (7), 470-3. (F15) Hlnshew, J. V. LC-OC 1989, 7 (5), 388-400. (F18) Voimut, J.; Matisova, E.; Phan, T. H. J . Hlgh Resolut. Chmmafogr. 1989, 12 (1l), 760-2. (F17) Uu, G.; Xin, 2. Chromatographie 1990, 29 (7-8), 385-8. (F18) Apps, P. J.; Pretorius, V. J . Chromefogr. 1989, 477, 81-9. (F19) Bkmberg, S.; Roeraade, J. J . H@h Resolut. ChKNnetogf. 1989, 72 (5), 204-9. (F20) (Lob, K. J. H@h Resolut. Chromatcgr. 1990, 73 (8), 540-6. (F21) Munari, F.; (Lob. K. J . Cbromatogr. Scl. 1980, 28(2), 61-8. (F22) (Lob, K. TrAC, Trends Anal. Chem. 1989, 8 (9,162-8. (F23) (Lob, K.; Kaeiin, I. J. High Resolut. Cbromatogr. 1991, 740 (7), 451-4. (F24) (Lob, K.; Schmarr, H. G.; Mosandl, A. J. High Resdut. Chrometogr. 1989. 72 16). 375-82. (F25) Ltkkai, P.; Hannuksela. J.; Mattinen, M. L.; Vlrolainen, M.; Haekkinen, V. M. A.; Rlekkola, M. L. J . High Resolut. Chromatogr. 1090, 73 (3), 170-2, (F26) Hawthome, S. 8.; Miller, D. J.; Krleger, M. S. J. Cbromatogr. Scl. 1989, 2 7 (7), 347-54. (F27) Hewthorne, S. B. Anal. Chem. 1990. 62 ( l l ) , 633A-842A. (F28) Hawthorne, S. 6.; Miller, D. J.; Krleger, M. S. J . High Resdut. Chmmafogr. 1989, 72(11), 714-20. (F2S) Khg, J. W. J. chromatogr. Scl. 1989. 27(7), 355-64. (F30) Anderson. M. R.; Swanson, J. T.; Porter, N. L.; Richter, B. E. J . ChfoSCl. 1080, 2 7 (7), 371-7. (F31) Nbkn, M. W. F.; Sanderson, J. T.; Frei, R. W.; Brlnkman, U. A. T. J. Clwome-. 1989, 474 (2). 388-95. (F32) Nblsen. T. J.; Jaegerstad, I. M.; Oeste, R. E.; Sivik, B. T. G. J . Agrlc. Food chsm. 1991, 39 (7), 1234-7. (F33) Hawthorne, S. 8.; Miller, D. J.; Langenfekl, J. J. J . Chromafcgr. Scl. 1990. 28 (l), 2-8. ( F U ) LOW, J. M.; Rosselll, A. C. ChrWlWtog*eph& 1989, 28 (11-12), 613-8. (F35) Fwton, K. 0.;Rein, J. Anal. Chlm. Acfa 1991, 248 (1). 283-70. (F38) Raymer. J. H.; Velez, G. R. J . Chmmatogr. Scl. 1991, 29 (11), 487-75. (F37) Lohblt, M.; Baechmann, K. J . Cbromatogr. 1990, 505 (I), 227-35. (F38) Houben. R. J.; Janssen, H. G. M.; Leclercq, P. A.; Rijks, J. A.; Cram era. C. A. J . H@I Resdut. Chromatogr. 1990, 73 (lo), 689-73. (F39) cortes, H. J.; (Leen. L. S.; Campbell, R. M. Anal. Chem. 1991, 63 (23), 2719-24. (F40) Swanson, J. T.; Richter, 8. J. &$IResold. chrometogr. 1990, 73 (5), 385-8. (F41) Hills. J. W.; Hill, H. H.; Maeda, T. Anal. Chem. 1991. 63 (ls), 2152-5. (F42) Uu, S.; b n g . J.; Strothsr, D. L.; Carley. R. J.; Stuart, J. D. J . Hlgh Rsaolut. ChrOmefOgr. 1989, 72 (12), 779-83. (F43) Mouradlan. R. J.; Levlne, S. P.; Sacks, R. D. J . Chromatogr. Scl. 1990. 28 (12). 843-8. (F44) (7). S 518-20. h i h . M.; Shibamoto, T. J. High Resdut. Chromarogr. 1890, 73
GAS CHROMATOGRAPHY (F45) Reglero, 0.; Henalz, T.; Herralz, M. J. Chromatog*. Scl. 1990, 28 (5), 221-4. (F46) Springston, S. R. J . Chrometogr. 1990. 577, 67-75. (F47) Frank, W.; Frank, H. Chromatographla 1990, 29 (11-12), 571-4. (F48) Burger, B. V.; Le Roux, M.; Munro, Z. M.; Wllken, M. E. J . chromet q . 1991, 552(1-2). 137-51. (F49) Lanzerstorfer, C.; Puxbaum, H. Anal. Lett. 1989, 22 (5), 1375-87. (F50) Ogwi, N.; Onishl, A.; Hanai, T. J. Hlgh Redut. Chromatogr. 1991, 74 (2), 79-82. (F51) Oglno, H.; Suzukl. T.; Aomura, Y. J . Chromatog. 1989. 472 (2), 389-92. (F52) Rhoderkk, G. C.; Miller. W. R. Anal. Chem. 1990, 82 (e), 810-5. (F53) Hachenberg, H. J. Hlgh Resolut. Chromatog. 1989, 72 (1I), 742-8. (F54) Mueller, H. M.; Stan, H. J. J . Hlgh Re&. chrometogr. 1990, 73(11), 759-73. (F55) Berg, J. R. J. Hlgh Reduf. Chromatog. 1989, 72 (3), 133-7. (F56) Caspar, 0.J . Chromatog. 1991. 556 (1-2), 331-51. IF57) Arnold. N. S.: McClennen, W. H.; Meuzelaar. H. L. C. Anal. Chem. ’
H@ Resdut. -2mnatogr. 1989, 72 (3), 142-8. (F59) Uu, Z.; Phllllps, J. B. J . Microcolumn Sep. 1989, 7 (9, 249-56. lF60I 2.:.Phlliias. E. -J .. Mlcrocolumn Sen. $990. ? ,()I. 33-40. ~.--, Llu. -., ......r_.J. -. -. . .~. (FBI) Mltra, S.; Phillips, J. B. Anal. Instrum: 1989, 78(2); i27-45. (F62) Klemp, M.; Sacks, R. J. Hlgh Resolut. Chromatogr. 1991. 74 (4), 235-40. (F63) Engelsma, M.; De Graff, J.; Smk, H. C. Anal. Chlm. Acta 1991, 252 (I-2), 187-200.
___.
~
DETECTORS
Ionizatlon Detecton
(GI) Hlnshaw, J. V. LC-GC 1990, 8 (2), 104-14.
(G2) Slgsby, J. E., Jr.; Dropkin, D. L.; Snow, R. Envkon. Scl. Technd. 1990, 24 (a),818-21.
(G3)Jorgensen, A. D.; Plcel. K. C.; Stamoudis, V. C. Anal. Chem. 1990, 62 (7). 683-9.
(G4)Huang, Y.; Ou, Q.; Yu, W. Anal. Chem. 1990, 82(18), 2063-4. (G5) Hausmann, M.; Homann, K. H. Ber. Bunsen-Oes. phvs. Chem. 1990, 94 ( l l ) , 1308-12.
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QUALITATIVE AND OUANTITATIVE ANALYSIS (KI) St. Louis, R. H.; Hill. H. H.. Jr. Chem. Anal. (N.Y.)1990, 7 7 7 , 109-27. (K2) Sandra. P.; David. F. J. Chromatogr. Scl. 1990, 50, 145-89. (K3) Davies, N. W. J . Chromatogr. 1990, 503 (l), 1-24. (K4) Vgdergauz, M. S.; Belyaev, N. F. Chromatograph& 1990, 30 (3-4). 163-70. (K5) Guan, Y.; Kiraly, J.; Rijks, J. A. J . Chromatogr. 1989. 472(1), 129-43. (K6) Peng, C. T.; Yang. Z. C.; Maltby, D. J . Chromatogr. 1991, 586 (l), 113-29. (K7) Rice, G. J.; Dent, M. R. J. Chromatogr. 1989, 483, 1-19. (K8) Rice, G. J.; Dent, M. R. J . Chromatogr. 1991, 585(1), 83-92. (K9) Messadi, D.; Helaimla, F.; A I l h n a c h e , S. C. R . Acad. Scl., Ser. 2 1990, 370 (Il), 1447-51. (K10) Garcia. D. J. A.; Santiuste, J. M. Chromatographie 1991, 32 (3-4). 116-24. (K11) Messedi, D.; Helalma, F.; AIWhnache, S.; Boumahraz, M. Chromatograph& 1990, 29 (9-10). 429-34. (K12) Fernandez-Sanchez, E.; Garcla-hmlnguez, J. A.; Menendez, V.; Santluste, J. M. J . Chromatogr. 1990, 498 (I), 1-9. (K13) Dlmov, N.; Matisova, E. J . Chromatogr. 1991, 549 (1-2), 325-33. (K14) Hasan, M. N.; Jurs, P. C. Anal. Chem. 1990. 62(21), 2318-23. (K15) Robbat, A., Jr.; Kalogeropoulos, C. Anal. Chem. 1990, 62 (24), 2684-8. (K16) Donneily, J. R.; Munslow, W. D.; Grange, A. H.; Pettit. T. L.; Simmons, R. D.; Sovocool, G. W. J. Chromatogr. 1991, 540 (1-2), 293-310.
(K17) Oeocgakopoubs, C. G.; Tsika, 0. G.; Klburls, J. C. Anal. Chem. 1991, 63 (16). 2025-8. (K18) Wgakopouks, C. G.; Klburis, J. C.; Jurs, P. C. Anal. Chem. 1991, 63 (la), 2021-4. (Kl9) W n o , T. C.; Castelb, Q. J . Chromatogr. 1991, 537(1-2), 305-19. (K20) Mowery, R. A., Jr. J . Chromatogr. Scl. 1991, 29(5), 104-204. (K21) Jorgensen, A. D.; Picel, K. C.; Stamoudis, V. C. Anal. Chem. 1990, 62 (7), 683-9. MISCELLANEOUS INFORMATION (Ll) Ooetes, S. R.; Sin, C. H. Appl. Spectrosc. Rev. 1989, 25(2), 82-126. (L2) Cramers, C. A.; Leclercq, P. A. Crit. Rev. Anal. Chem. 1988, 20 (2), 117-47. (L3) Oszczepowlcz, J. Stud. Org. Chem. 1991, 42, 343-85. (L4) Grob, K. J . &7h Resolut. Chromatogr. 1990, 73 (E), 540-6. (L5) Watanebe, C.; Hashimoto, K. J . H/gh R e s o M . Chromatop. 1990, 73 (9), 610-3. (L6) Uu, Z.; Phillips, J. B. J . Mlcrocoumn Sep.1990, 2 (l), 33-40. (L7) &spar, 0. J. Chromtogr. 1991, 556(1-2), 331-51. (LE) Llu, Z.; Zhang, M.; Phillips, J. B. J . Chromatogr. Scl. 1990, 28 (1I), 567-7 1. (L9) W a d i a n . R. F.; Levine, S. P.; Sacks, R. D. J . Chromtew. Scl. 1990. 28 (12). 643-8. (L10) Klemp, M.; Sacks, R. J . High Resolut. Chromatogr. 1991, 74 (4), 235-40. ___ (L11) Hubball, J. LC-GC 1990, 8 (I), 12, 14. 16. (L12) Charleux, P.; Forest, M.; Bonnaud, A. Spectra 2000 1991, 758, 23-8. (L13) Hinshaw, J. V. LC-OC 1991, 9 (2). 94, 96-8. (L14) Grob, K.; Tschuor, R. J . High Resolut. Chromatogr. 1990. 73 (3), 193-4. (L15) Hevesl, T.; Krupclk, J.; Benlcka, E.; Repka. D.; Garaj, J. TrAC, Trends Anal. them. 1990, 9 (4), 132-5. (Ll8) Ioffe,B. V. Fresenlus' 2.Anal. Chem. 1989, 335(1), 77-80. (L17) Bames, R. L. J . chrometogr. Scl. 1990, 49, 140-65. (L18) Venema, A. J . H@ Resolut. Chromatogr. 1990, 73 (E), 537-9. (L19) Vltenberg, A. 0. J. Chromatogr. 1991, 556 (1-2), 1-24. (L20) Ewe, L. S.; Kolb, 8. Chromatogrephla 1991. 32 (1-2). 5-12. (L21) Tabera, J.; Reglero, 0.; Herralz, M.; Blanch, 0. P. J. H/gh Resolut. C h r m t O g r . 1991, 74 (6), 392-6. (L22) B a a , D. E.; D o h . J. W.; Raddatz, W. D.; Snyder, L. R. Anal. Chem. 1990. 62 (15), 1560-7. (L23) Wang, Q.; Zhu, C.; Yan, B. J . chrometogr. 1990, 573, 13-9. (L24) Dolan, J. W.; Snyder, L. R.; Bautz, D. E. J . Chromatogr. 1991, 547 11-2). 21-34. (L25) -L&, J. R.; Mayfleid. H. T.; Henley, M. V.; Kromann, P. R. Anal. Chem. 1991. 63 (13). 1256-61. (L26) Kdlle, T..O.; Podle, C. F. J. Chromatogr. 1991, 550 (1-2), 231-7. (L27) Len-s, F. M.; Francelin, R. A.; DeSouza, A. J. J . Hi& Resduf. ChroM t o g r . 1991. 74 (6), 407-11. (L28) Abby, 0. N.; Berry, E. F.; Leepipatpiboon, S.; Ramstad. T.; Roman, M. C. LC-GC 1991, 9 (2), 100-2, 104. 106-8, 110, 112, 114. (L29) Aishlma, T.; Nakai, S. Anal. Chlm. Acta 1991, 248 (I), 41-50. (L30) OlCJS,F. J.; Davis, J. M. J. Chromatogr. 1991. 550 (1-2), 135-54. (L31) Kdlle, T. 0.; Poole, C. F. J. Chrometogr. 1991, 556(1-2). 457-84. (L32) Bemgeard, A. K.;Coimsjoe, A. L. J. H/gh R d u t . Chronmtogr. 1990, 73 (lo), 689-93. (L33) Belfer, A. J.; Locke, D. C.; Landau, 1. Anal. Chem. 1990, 62 (4), 347-9.
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
