A direct sample injection technique was developed for supercritical fluid chromatography in a packed capillary column, with carbon dioxide as mobile phase and a flame ionization detector. The method allowed solutions, neat liquids, and even solids to be introduced as samples. Also, extraction with supercritical carbon dioxide was combined with this method to separate polymer additives.
AbstractA method for preparation of capillary columns and traps with a very thick film (up to 100 μm) of stationary phase is described. The principle of this method is based on an immediate fixation of a film of prepolymer, formed during dynamic coating. Thus, the development of film irregularities, such as are caused by Rayleigh instability is avoided. Fixation of the film is conveniently accomplished by heat‐accelerated crosslinking as was demonstrated in this work, where a commercially available silicone prepolymer (Sylgard 184, Dow Corning) was employed.The low phase ratio columns which thus can be prepared are interesting both in chromatography with dense mobile phases and as enrichment devices. Examples of the latter application are shown, where trace organic components from air and water were concentrated.
AbstractDue to their high polarity and unique selectivity, cyanopropyl silicones are basic stationary phases for high resolution capillary gas chromatography. Different OH‐terminated cyanopropyl silicones, containing a high cyanopropyl content, were synthesized and chromatographically evaluated. Special attention was paid to the degree of immobilization of the phases in FSOT columns. Depending on the problem at hand, a choice has to be made between immobilization and maximum selectivity.
Aromatic solvents are involved in manifold areas of industry and craft. Inhaled solvent vapors are a known health hazard to workers. For medical prevention and toxicological assay specific laboratory methods for urinary metabolites are necessary. An economical capillary gas chromatographic procedure is described which is suitable for routine analysis of major metabolites, sensitive for the determination of minor metabolites, and effective for the separation of chiral metabolic intermediates.
AbstractA method for the determination of individual free and conjugated bile acids in serum using microcolumn liquid chromatography coupled with a laser‐induced fluorescence detector is described. Bile acids are separated into free/glycine‐conjugate and taurine‐conjugate fractions using a Sep‐Pak SIL cartridge. The taurine‐conjugated bile acid fraction is subjected to enzymatic hydrolysis. Subsequently, free and conjugated bile acids are labeled using 4‐(bromomethyl)‐7‐methoxycoumarin as a fluorogenic reagent, producing stable derivatives that can be excited by the 325 nm line of a He/Cd laser. Prior to their fluorimetric detection, the individual components of a bile acid serum profile are separated by reversed‐phase microcolumn liquid chromatography.
Narrow bore columns (100 μm) have successfully been applied in the analysis of commercial lemon oils. On these columns, high resolution is obtained in a short analysis time. Different Brazillian lemon oils are characterized qualitatively and quantitatively.
Journal of High Resolution ChromatographyVolume 11, Issue 4 p. 352-353 Short Communication Rapid and efficient separation of PTH-amino acids employing supercritical CO2 and an ion pairing agent M. Ashraf-Khorassani, M. Ashraf-Khorassani Virginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USASearch for more papers by this authorM. G. Fessahaie, M. G. Fessahaie Virginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USASearch for more papers by this authorL. T. Taylor, Corresponding Author L. T. Taylor Virginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USAVirginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USASearch for more papers by this authorT. A. Berger, T. A. Berger Hewlett Packard, Inc. Avondale Division Route 41, P.O. Box 900, Avondale, PA 19311–0900, USASearch for more papers by this authorJ. F. Deye, J. F. Deye Hewlett Packard, Inc. Avondale Division Route 41, P.O. Box 900, Avondale, PA 19311–0900, USASearch for more papers by this author M. Ashraf-Khorassani, M. Ashraf-Khorassani Virginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USASearch for more papers by this authorM. G. Fessahaie, M. G. Fessahaie Virginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USASearch for more papers by this authorL. T. Taylor, Corresponding Author L. T. Taylor Virginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USAVirginia Polytechnic Institute and State University, Department of Chemistry, Blacksburg, VA 24061–0212, USASearch for more papers by this authorT. A. Berger, T. A. Berger Hewlett Packard, Inc. Avondale Division Route 41, P.O. Box 900, Avondale, PA 19311–0900, USASearch for more papers by this authorJ. F. Deye, J. F. Deye Hewlett Packard, Inc. Avondale Division Route 41, P.O. Box 900, Avondale, PA 19311–0900, USASearch for more papers by this author First published: April 1988 https://doi.org/10.1002/jhrc.1240110414Citations: 37AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL No abstract is available for this article.Citing Literature Volume11, Issue4April 1988Pages 352-353 RelatedInformation
Journal of High Resolution ChromatographyVolume 11, Issue 9 p. 673-675 Short Communication Separation of polycyclic aromatic hydrocarbons in microcolumn liquid chromatography using dicoronylene as stationary phase K. Jinno, Corresponding Author K. Jinno School of Materials Science, Toyohashi University of Technology, Toyohashi 440, JapanSchool of Materials Science, Toyohashi University of Technology, Toyohashi 440, JapanSearch for more papers by this authorH. Shimura, H. Shimura School of Materials Science, Toyohashi University of Technology, Toyohashi 440, JapanSearch for more papers by this authorJ. C. Fetzer, J. C. Fetzer Chevron Research Company, Richmond, CA 94802, USASearch for more papers by this authorW. R. Biggs, W. R. Biggs Chevron Research Company, Richmond, CA 94802, USASearch for more papers by this author K. Jinno, Corresponding Author K. Jinno School of Materials Science, Toyohashi University of Technology, Toyohashi 440, JapanSchool of Materials Science, Toyohashi University of Technology, Toyohashi 440, JapanSearch for more papers by this authorH. Shimura, H. Shimura School of Materials Science, Toyohashi University of Technology, Toyohashi 440, JapanSearch for more papers by this authorJ. C. Fetzer, J. C. Fetzer Chevron Research Company, Richmond, CA 94802, USASearch for more papers by this authorW. R. Biggs, W. R. Biggs Chevron Research Company, Richmond, CA 94802, USASearch for more papers by this author First published: September 1988 https://doi.org/10.1002/jhrc.1240110914Citations: 8AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat Citing Literature Volume11, Issue9September 1988Pages 673-675 RelatedInformation
AbstractSoil fumigants, like 1,3‐dichloropropene and metham‐sodium (forming methyl isothiocyanate) diffuse into the atmosphere, thus presenting a hazard to people in the surroundings. A method is described in which a large volume (50 μl) of extractant, used to desorb the compounds from charcoal, is injected into a GC, equipped with two capillary columns. By way of Deans switching, the solvent is separated from the compounds of interest. Modification of a GC sampler makes unattended analyses possible.
Journal of High Resolution ChromatographyVolume 11, Issue 8 p. 605-607 Short Communication Methyl p-hydroxyphenyllactate: Identification in rat liver extracts B. M. Markaverich, B. M. Markaverich Center for Biotechnology, Baylor College of Medicine, 4000 Research Forest Drive, The Woodlands, Texas 77381, USASearch for more papers by this authorR. R. Gregory, R. R. Gregory Center for Biotechnology, Baylor College of Medicine, 4000 Research Forest Drive, The Woodlands, Texas 77381, USASearch for more papers by this authorM. A. Alejandro, M. A. Alejandro Center for Biotechnology, Baylor College of Medicine, 4000 Research Forest Drive, The Woodlands, Texas 77381, USASearch for more papers by this authorG. A. Johnson, G. A. Johnson Department of Biochemical and Biophysical Sciences, University of Houston, Houston, Texas 77204, USASearch for more papers by this authorB. S. Middleditch, Corresponding Author B. S. Middleditch Department of Biochemical and Biophysical Sciences, University of Houston, Houston, Texas 77204, USADepartment of Biochemical and Biophysical Sciences, University of Houston, Houston, Texas 77204, USASearch for more papers by this author B. M. Markaverich, B. M. Markaverich Center for Biotechnology, Baylor College of Medicine, 4000 Research Forest Drive, The Woodlands, Texas 77381, USASearch for more papers by this authorR. R. Gregory, R. R. Gregory Center for Biotechnology, Baylor College of Medicine, 4000 Research Forest Drive, The Woodlands, Texas 77381, USASearch for more papers by this authorM. A. Alejandro, M. A. Alejandro Center for Biotechnology, Baylor College of Medicine, 4000 Research Forest Drive, The Woodlands, Texas 77381, USASearch for more papers by this authorG. A. Johnson, G. A. Johnson Department of Biochemical and Biophysical Sciences, University of Houston, Houston, Texas 77204, USASearch for more papers by this authorB. S. Middleditch, Corresponding Author B. S. Middleditch Department of Biochemical and Biophysical Sciences, University of Houston, Houston, Texas 77204, USADepartment of Biochemical and Biophysical Sciences, University of Houston, Houston, Texas 77204, USASearch for more papers by this author First published: August 1988 https://doi.org/10.1002/jhrc.1240110814Citations: 7AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat Citing Literature Volume11, Issue8August 1988Pages 605-607 RelatedInformation
AbstractFor a typical narrow bore (50 μm) and wide bore (320 μm) capillary column the effects of increased stationary phase film thickness (df) on the minimum detectable amount, Qo, as well as on the minimum analyte concentration, Co, are described. In treating the effect of an increased film thickness, two approaches can be followed; either the separation temperature is kept constant, resulting in larger values of the capacity ratio, k, or the column temperature is increased such as to keep k constant. For normalized chromatographic conditions the effects of both approaches on the minimum plate height, optimum carrier gas velocity, and required plate number are described, finally yielding expressions for Qo and Co for both mass flow and concentration sensitive detectors. At constant temperature, Co always increases with the film thickness for mass flow sensitive detectors (e.g. FID). Wide bore thin film columns offer the lowest value of Co attainable. For concentration sensitive detectors (e.g. TCD), Co is affected neither by column diameter nor by film thickness. The Qo–df plot for constant temperature shows a minimum, suggesting an optimum film thickness for mass flow sensitive as well as concentration sensitive detectors. The corresponding capacity ratio has a value between 0.5 and 1.5. At elevated temperatures (k constant) in combination with mass flow sensitive detectors, again an optimum film thickness exists, corresponding to a minimum value of Co. For constant capacity ratio Qo always increases with the film thickness for both types of detectors. As indicated above, in some situations the lowest values of Co and Qo are obtained at an increased film thickness, the effect being marginal. As an initial guideline, for the daily practice of capillary gas chromatography with respect to minimum values of Co and Qo, the use of thin film columns is to be preferred.
Journal of High Resolution ChromatographyVolume 11, Issue 4 p. 337-338 Short Communication Simple and versatile method for connecting fused silica and glass capillaries M. Vecchi, Corresponding Author M. Vecchi Central Research Units, F. Hoffmann-La Roche & Co. AG, CH-4002 Basel, SwitzerlandCentral Research Units, F. Hoffmann-La Roche & Co. AG, CH-4002 Basel, SwitzerlandSearch for more papers by this authorW. Walther, W. Walther Central Research Units, F. Hoffmann-La Roche & Co. AG, CH-4002 Basel, SwitzerlandSearch for more papers by this author M. Vecchi, Corresponding Author M. Vecchi Central Research Units, F. Hoffmann-La Roche & Co. AG, CH-4002 Basel, SwitzerlandCentral Research Units, F. Hoffmann-La Roche & Co. AG, CH-4002 Basel, SwitzerlandSearch for more papers by this authorW. Walther, W. Walther Central Research Units, F. Hoffmann-La Roche & Co. AG, CH-4002 Basel, SwitzerlandSearch for more papers by this author First published: April 1988 https://doi.org/10.1002/jhrc.1240110408Citations: 9AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onEmailFacebookTwitterLinkedInRedditWechat No abstract is available for this article. References 1 G. Schomburg, H. Husmann and F. Weeke, Chromatographia 10 (1977) 580. 2 G. Grob, Jr. G. Grob and K. Grob, J. Chromatogr. 156 (1978) 1. 3 K. Grob and G. Grob, HRC & CC 1 (1978) 302. 4 K. Grob, G. Grob and K. Grob, Jr. J. Chromatogr. 219 (1981) 13. 5 V. Pretorius, K. Lawson and W. Bertsch, HRC & CC 5 (1982) 568. 6 K. Grob, Jr. and R. Müller, J. Chromatogr. 244 (1982) 185. 7 P. Sandra, M. Schelfaut and M. Verzele, HRC & CC 5 (1982) 50. 8 J. Roeraade, HRC & CC 6 (1983) 140. 9 F. Etzweiler, HRC & CC 7 (1984) 578. 10 J. Roeraade, S. Blomberg and G. Flodberg, J. Chromatogr. 301 (1984) 454. 11 K. Grob, Jr. J. Chromatogr. 330 (1985) 217. 12 P. J. Apps, V. Pretorius, E. R. Rohwer and K. H. Lawson, HRC & CC 8 (1985) 77. 13 K. Grob, Jr. G. Karrer and M. Riekkola, J. Chromatogr. 334 (1985) 129. 14 F. Etzweiler, HRC & CC 8 (1985) 436. 15 E. R. Rohwer, V. Pretorius and P. J. Apps, HRC & CC 10 (1986) 595. 16 R. J. Rieder and R. E. Kaiser, HRC & CC 9 (1986) 595. 17 E. R. Rohwer and V. Pretorius, HRC & CC 10 (1987) 145. 18 G. Alexander and B. R. Gandhe, HRC & CC 10 (1987) 156. 19 K. Grob, Jr. G. Grob and K. Grob, J. Chromatogr. 219 (1981) 13. 20 M. Donike, Chromatographia 6 (1973) 190. 21 W. Blum, HRC & CC 8 (1985) 718. Citing Literature Volume11, Issue4April 1988Pages 337-338 ReferencesRelatedInformation
Journal of High Resolution ChromatographyVolume 11, Issue 2 p. 218-220 Short Communication Capillary gas chromatography of the terpenic fraction of Juniperus communis L. Black, Green, Berry, and Leaf Extracts N. Gelsomini, Corresponding Author N. Gelsomini Dipartimento di Chimica Organica – “U. Schiff”, Universita' di Firenze, Via G. Capponi. N°9, 50121 Firenze, ItalyDipartimento di Chimica Organica – “U. Schiff”, Universita' di Firenze, Via G. Capponi. N°9, 50121 Firenze, ItalySearch for more papers by this authorV. Vidrich, V. Vidrich Dipartimento di Scienza del Suolo e Nutrizione della Pianta, Universita' di Firenze, P. le delle Cascine, N° 18, 50144 Firenze, ItalySearch for more papers by this authorP. Fusi, P. Fusi Dipartimento di Scienza del Suolo e Nutrizione della Pianta, Universita' di Firenze, P. le delle Cascine, N° 18, 50144 Firenze, ItalySearch for more papers by this authorM. Michelozzi, M. Michelozzi Istituto Miglioramento Genetico delle Piante Forestali del C.N.R., Via S. Bonaventura, N° 13, 50145 Firenze, ItalySearch for more papers by this author N. Gelsomini, Corresponding Author N. Gelsomini Dipartimento di Chimica Organica – “U. Schiff”, Universita' di Firenze, Via G. Capponi. N°9, 50121 Firenze, ItalyDipartimento di Chimica Organica – “U. Schiff”, Universita' di Firenze, Via G. Capponi. N°9, 50121 Firenze, ItalySearch for more papers by this authorV. Vidrich, V. Vidrich Dipartimento di Scienza del Suolo e Nutrizione della Pianta, Universita' di Firenze, P. le delle Cascine, N° 18, 50144 Firenze, ItalySearch for more papers by this authorP. Fusi, P. Fusi Dipartimento di Scienza del Suolo e Nutrizione della Pianta, Universita' di Firenze, P. le delle Cascine, N° 18, 50144 Firenze, ItalySearch for more papers by this authorM. Michelozzi, M. Michelozzi Istituto Miglioramento Genetico delle Piante Forestali del C.N.R., Via S. Bonaventura, N° 13, 50145 Firenze, ItalySearch for more papers by this author First published: February 1988 https://doi.org/10.1002/jhrc.1240110219Citations: 6AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onEmailFacebookTwitterLinkedInRedditWechat References 1 A. Marpeau-Bezard, P. Baradat, C. Bernard-Dagan, Les terpenes du pin marittime: aspeets biologiques et genetiques. V Heredite de la teneur en limonene. Am. Sci. For. 40 (1983) 197–216. 2 A. E. Squillace, Biochemical genetics and selection composition of volatile terpenes. Presented at Meeting of IUFRO Working Parties on Forest Genetics. June 1976, Bordeaux, France (1976). 3 R. Yazdanj, J. E. Nilsson, T. Ericsson, Geographical variation in the relative proportion of monoterpenes in cortical oleoresin of Pinus sylvestris in Sweden Silvae Genetica 34 (1985) 201–208. 4 V. Vidrich, C. A. Cecconi, G. G. Ristori, P. Fusi, Chemicals from Italian biomass. Symposium on forest products research international achievements and the future. Pretoria, South Africa April 22–26, (1985). Citing Literature Volume11, Issue2February 1988Pages 218-220 ReferencesRelatedInformation
AbstractA method ist described that permits direct comparison of ion chromatograms between an isolate from a suspect fire debris sample and corresponding accelerant profiles. The system is highly automated and produces a diagnostic one page summary report for each sample. Side by side comparison of ion profiles is carried out between 4 common fuel types, e. g. gasoline, naphthenic type charcoal lighter fluid, mineral spirits, and kerosene, and the sample. Both qualitative and semiquantitative information is available. An on‐line search can also be carried out in which mass spectra are compared between components in a suspect sample and standards that are contained in an accelerant library. The system is flexible and requires only minimal interaction with the analyst.
AbstractFor the analysis of broxaterol 1‐(3‐bromoisoxazol‐5‐yl)‐2‐(tert‐butylamino)ethanol in human plasma and urine an on‐line HPLC‐GC apparatus was used applying the “concurrent solvent evaporation” technique described in previous studies. Broxaterol is quantitatively determined by capillary GC with ECD detection, after extraction from plasma and derivatization. The detection limit of 0.03 ng/ml permits pharmacokinetic studies in man after oral and intravenous administration of the drug.
Abstractβ‐Blocking drugs present in commercial pharmaceutical products are determined in present urine of volunteers between 4 and 24 hours after the administration of a therapeutical dose. The drugs are extracted, hydrolysed, derivatized with pentafluoropropionic anhydride, and analyzed by capillary gas chromatography and electron capture detection. Metabolite identification and drug confirmation is by capillary gas chromatography–negative ion chemical ionization mass spectrometry (GC‐NICIMS). This method is very specific and a sensitivity below 1 ng/ml is obtained.
AbstractIntroduction of solutions of up to several milliliters by on‐column injection of large volumes or by coupled HPLC‐GC may cause problems with GC detectors (FID, AFID, MS). For instance, dichloromethane forms large amounts of hydrochloric acid and carbon black in FIDs.A column effluent splitter was developed for keeping the major portion of the solvent vapors away from the detector; approximately 99% of the vapor is vented while the remaining 1% of vapor is used for detecting the widths of the solvent peaks. During analysis, the split ratio is reversed by a strong increase of the resistance to the gas flow through the split exit line.The system was used for the determination of di‐(2‐ethylhexyl)‐phthalate (DEHP) in triglyceride matrices of various foods. Direct determination by HPLC is not sufficiently sensitive, whereas direct analysis by GC is hindered by the triglycerides. Solutions of fats or oils were pre‐separated on a silica column using dichloro‐methanelcyclohexane 1:l with addition of 0.05 % acetonitrile as eluent. The HPLC fraction containing the DEHP was transferred to GC through a loop‐type interface using concurrent solvent evaporation. Detection limits were around 0.1 ppm.
Journal of High Resolution ChromatographyVolume 11, Issue 10 p. 723-725 Short Communication Determination of cis- and trans- 3-hydroxycotinine by high performance liquid chromatography S. O'Doherty, S. O'Doherty The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorA. Revans, A. Revans The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorC. L. Smith, C. L. Smith The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorM. McBride, M. McBride The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorM. Cookek, Corresponding Author M. Cookek The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainThe School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this author S. O'Doherty, S. O'Doherty The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorA. Revans, A. Revans The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorC. L. Smith, C. L. Smith The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorM. McBride, M. McBride The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this authorM. Cookek, Corresponding Author M. Cookek The School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainThe School of Chemistry, The University of Bristol, Bristol BS8 1 TS, Great BritainSearch for more papers by this author First published: October 1988 https://doi.org/10.1002/jhrc.1240111008Citations: 12AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat No abstract is available for this article.Citing Literature Volume11, Issue10October 1988Pages 723-725 RelatedInformation
AbstractA combined sampling and analysis technique for the determination of gas phase nicotine and 3‐ethenylpyridine, and of particulate phase nicotine in environmental tobacco smoke with capillary gas chromatography is reported. The major advantage of the technique is that all of the collected particulate phase material is analyzed by thermal desorption of the collected material rather than by analysis of only a fraction of the sample extracted from the collection medium. A Teflon filter microtube is used to collect particulate phase nicotine. This microtube is follwed by a small Tenax sorbent bed to collect gas phase nicotine and 3‐ethenylpyridine. After sampling, the Teflon filter is transferred to a clean glass tube and the tube becomes an insert for a modified packed column injector port where the material collected on the filter is heat desorbed to a cold capillary tubing trap. Gas phase nicotine and 3‐ethenylpyridine are also transferred from the Tenax to the GC column by thermal desorption from the Tenax sorbent bed. Gas phase nicotine and 3‐ethenylpyridine, and particulate phase nicotine are each determined by GC analysis of the desorbed material. Nicotine and 3‐ethenylpyridine are quantitated by the use of external standards. This technique is straightforward and can be used for semi‐real time determination of both gas and particulate phase compounds in environmental tobacco smoke. The results obtained by this technique compare well with those obtained by sampling with annular diffusion denuders.
AbstractIn this study, the cold split‐splitless injector recently introduced by Carlo Erba was optimized for the trace analysis of polycyclic aromatic hydrocarbons. Injections of hundreds of microliters of hexane solutions were performed in the solvent split mode using an autosampler programmed for large volume injection. Injection parameters such as type of insert, initial oven temperature, split time, and flow are shown to play important roles in defining the conditions for obtaining quantitative results. The loss of early eluting compounds can be minimized by achieving a solvent trapping effect, making use of n‐octane as co‐solvent in n‐hexane.
