Briefs
Determination of n-Butylated Trialkyllead Compounds by Gas Chromatography with Microwave Plasma Emission Detection 2402 T r i a l k y l l e a d chlorides a r e c o n v e r t e d q u a n t i t a t i v e l y i n t o rc-butyltrialkyllead derivatives with a Grignard reagent after e x t r a c t i o n . P r e c o l u m n t r a p e n r i c h m e n t allows for d e t e r m i n a t i o n a t t h e low p a r t s - p e r - b i l l i o n level. Scott A. Estes, P . C. Uden*, a n d R. M. B a r n e s , Department of Chemistry, GRC Towers, University of Massachusetts, Amherst, Mass. 01003 Anal. Chem., 54 (1982) Trace Gas Chromatographic Analysis by Use of Large Sample On-Column Injection with Bonded Phase Capillary Columns 2406 Analyses below t h e p a r t - p e r - b i l l i o n level a r e possible w i t h a single c o l u m n a n d a c o n v e n t i o n a l flame ionization d e t e c t o r . As m u c h as 100 μ-L can b e injected o n t o t h e bonded phase column. A. Zlatkis*, F.-S. Wang, a n d H. Shanfield, Chemistry Department, University of Houston, Houston, Tex. 77004 Anal. Chem., 54 (1982) Adsorption Isotherm at the Liquid-Solid Interface and the Interpretation of Chromatographic Data 2410 T h e m e t h o d is b a s e d o n t h e i n t e r p r e t a t i o n of t h e r e t e n t i o n d a t a of l a b e l e d c o m p o u n d s a n d of c o n c e n t r a t i o n p e r t u r b a t i o n s of t h e e l u e n t . M o d e l s a r e p r e s e n t e d for t h e h o l d u p v o l u m e a n d for a "surface p h a s e " a t t h e l i q u i d solid interface. Ngoc Le Ha, J â n o s U n g v â r a i , a n d E r v i n sz. Kovâts*, Laboratoire de Chimie Technique de l'Ecole Polytechnique Fédérale de Lausanne, 1015 Lausanne, Switzerland Anal. Chem., 54 (1982) Chromatographic Retention Mechanism of Organic Ions on a Low-Capacity Ion Exchange Adsorbent 2422 C h r o m a t o g r a p h i c r e t e n t i o n of a c o u n t e r i o n arises from b o t h ion e x c h a n g e a n d surface a d s o r p t i o n . T h e l a t t e r is d e p e n d e n t u p o n t h e electrical p o t e n t i a l of t h e surface. S h a p o u r Afrashtehfar and F r e d e r i c k F . Cantwell*, Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada T6G 2G2 Anal. Chem. ,54(1982) Ion Interaction Chromatography of Inorganic Anions on a Poly (sty rene-divinylbenzene) Adsorbent in the Presence of Tetraalkylammonium Salts 2427 R e t e n t i o n of t h e R4N"1" s a l t as a d o u b l e layer o n t h e s t a t i o n a r y p h a s e surface a n d a n i o n selectivity b e t w e e n a n a l y t e a n i o n s a n d t h o s e occupying t h e s e c o n d a r y layer of t h e d o u b l e layer c o n t r i b u t e t o t h e e n h a n c e d r e t e n t i o n of inorganic ions o n t h e a d s o r b e n t . Ziad I s k a n d a r a n i a n d Donald J . Pietrzyk*, Department of Chemistry, The University of Iowa, Iowa City, Iowa 52242 Anal. Chem., 54 (1982)
Comparison of Ion Chromatography and Titrimetry for Determination of Sulfur in Fuel Oils 2431 T h e t w o m e t h o d s a r e c o m p a r a b l e in precision a n d accuracy. T i t r i m e t r y is p r e f e r r e d w h e n r a p i d sulfur d e t e r m i n a t i o n in a n u m b e r of s a m p l e s is r e q u i r e d . Puligandla Viswanadham*, Donald R. Smick, J e r o m e J . Pisney, a n d W a l t e r F . Dilworth, IBM System Products Division, Rochester, Minn. 55901 Anal. Chem., 54 (1982) Gas Chromatographic Determination of Lower Fatty Acids in Air at Part-per-Trillion Levels 2433 S a m p l e s a r e collected w i t h 1% Sr(OH>2 coated on glass b e a d s . T h e m i n i m u m d e t e c t a b l e c o n c e n t r a t i o n is ~ 0 . 5 p a r t s - p e r - t r i l l i o n for n- a n d i s o b u t y r i c acids a n d n- a n d isovaleric acids. Precision is less t h a n 15%. Yasuyuki Hoshika, Aichi Environmental Research Center, 7-6, Nagare, Tsuji-machi, Kita-ku, Nagoya-shi, Aichi, 462, Japan Anal. Chem., 54 (1982) Comparison of Methods Used for the Determination of Void Volume in Reversed-Phase Liquid Chromatography 2438 E x i s t i n g m e t h o d s for V 0 d e t e r m i n a t i o n a r e e v a l u a t e d . A p r o c e d u r e for linearization of r e t e n t i o n d a t a of homologous series b a s e d o n a convergence t e s t is p r o p o s e d a n d compared with other methods. Ante M. Krstulovic*, H e n r i Colin, a n d Georges Guiochon, Ecole Polytechnique, Laboratoire de Chimie Analytique Physique, 91128 Palaiseau Cedex, France Anal. Chem., 54 (1982) Capillary Gas Chromatography/Fourier Transform Mass Spectrometry 2443 A j e t s e p a r a t o r interface is used. R a p i d p e a k switching a t high r e s o l u t i o n over a r b i t r a r i l y wide m a s s ranges is possible. W i t h n o c h a n g e s in i n s t r u m e n t a t i o n , F T M S can b e o p e r a t e d in a C I m o d e for G C / M S . R o b e r t L. White and Charles L. Wilkins*, Department of Chemistry, University of California—Riverside, Riverside, Calif. 92521 Anal. Chem., 54 (1982) Improvement of Speed of Separation in Packed Column Gas Chromatography
2447
L i m i t i n g factors such a s s a m p l e capacity, m a s s transfer in t h e s t a t i o n a r y p h a s e , d e t e c t i o n , a n d injection a r e discussed. O p t i m i z a t i o n allows significant m i n i a t u r i z a t i o n of t h e chromatographic system. R o b e r t J . J o n k e r a n d H a n s Poppe*, Laboratory for Analytical Chemistry, University of Amsterdam, Nieuwe Achtergracht 166, 1018 WV Amsterdam, The Netherlands, and J . F . K. H u b e r , Institute of Analytical Chemistry, University of Vienna, Wâhringer Strasse 38, Vienna, Austria Anal. Chem., 54 (1982)
* Corresponding author 1444 A · ANALYTICAL CHEMISTRY, VOL. 54, NO. 14, DECEMBER 1982
Briefs Characterization of Glucuronides by Chemical Ionization Mass Spectrometry with Ammonia as Reagent Gas
Determination of Uranium in Aqueous Samples by Laser-Induced Fluorescence Spectrometry 2475 2456
T h e m o v i n g b e l t L C interface is u s e d for p r o b e s a m p l e i n t r o d u c t i o n . F r a g m e n t a t i o n p r o c e e d s via cleavage of t h e glucuronic b o n d w i t h t h e c o n s t i t u e n t aglycone m o i e t y being identified a s either a n a d d u c t or p r o t o n a t e d species. T h o m a s Cairns* a n d Emil G. Siegmund, Department of Health and Human Services, Food and Drug Administration, Office of the Executive Director of Regional Operations, 1521 West Pico Boulevard, Los Angeles, Calif. 90015 Anal. Chem., 54 (1982)
U r a n i u m is e x t r a c t e d i n t o t r i - η -butyl p h o s p h a t e a n d t h e n b a c k e x t r a c t e d i n t o p h o s p h o r i c acid. T h e d e t e c t i o n l i m i t is 1 p p b w i t h a precision of ± 7 % R S D . V a r i a t i o n of r e s u l t s w i t h s a m p l e m a t r i x a n d a n a l y t i c a l p r o c e d u r e is discussed. P e t e r G. Whitkop, E. I. du Pont de Nemours & Company, Savannah River Laboratory, Aiken, S.C. 29808 Anal. Chem., 54 (1982)
Matrix and Solvent Effects on the Room-Temperature Phosphorescence of Nitrogen Heterocycles 2477 Determination of Double Bond Position and Geometry of Olefins by Mass Spectrometry of Their Diels-Alder Adducts 2462 T h e s p e c t r a a r e s i m p l e r t h a n t h e s p e c t r a of o t h e r d e r i v a t i v e s u s e d for t h i s p u r p o s e . T h e ions indicative of t h e m o l e c u l a r weight of t h e a d d u c t a r e very p r o m i n e n t even t h o u g h t h e m o l e c u l a r ion is a b s e n t . David A. Kidwell and K. Biemann*, Department of Chemistry, Massachusetts Institute of Technology, Cambridge, Mass. 02139 Anal. Chem., 54 (1982)
Analysis of the Chemical Ionization Reagent Plasma Produced in Liquid Chromatography/Mass Spectrometry by Direct Liquid Introduction Mass Spectrometry/Mass Spectrometry 2465 T h e empirical f o r m u l a s a n d s t r u c t u r e s a r e p o s t u l a t e d for t h e p r o t o n - b o u n d cluster ions f o u n d in a c e t o n i t r i l e / w a t e r a n d m e t h a n o l / w a t e r . T h e solvent effects on p r o t o n a t i o n a n d f r a g m e n t a t i o n a r e discussed. R. D. Voyksner* a n d J . Ronald Hass, Laboratory of Environmental Chemistry, National Institute of Environmental Health Sciences, P.O. Box 12233, Research Triangle Park, N.C. 27709, and M a u r i c e M. Bursey, Department of Chemistry, University of North Carolina, Chapel Hill, N.C. 27514 Anal. Chem., 54 (1982) Spin Trapping of Hydroxyl Radical in the Troposphere for Determination by Electron Spin Resonance and Gas Chromatography/Mass Spectrometry 2470 H y d r o x y l radical is t r a p p e d in s i t u w i t h α - 4 - p y r i d y l - i V - i e r t - b u t y l n i t r o n e α-1-oxide. L i m i t of d e t e c t i o n is ~ 5 Χ 10 5 m o l e c u l e s / c m 3 for a 2 0 0 - m 3 air s a m p l e . U n c e r t a i n t y is glassy carbon > stainless steel. Exchange current densities are also solvent dependent. J. F. Coetzee* and C. W. Gardner, Jr., Department of Chemistry, University of Pittsburgh, Pittsburgh, Pa. 15260 Anal. Chem.,54 (1982) Flow Rate Independent Amperometric Cell 2532 An electrode consisting of 100 disks, each of 5-μηι radius, is constructed with carbon fibers. The electrode is assembled into an electrochemical cell designed to minimize convective effects on the faradaic current. W. Lowry Caudill, Jonathon O. Howell, and R. Mark Wightman*, Department of Chemistry, Indiana University, Bloomington, Ind. 47405 Anal. Chem.,54 (1982) Solvent Extraction of Dithiocarbamate Complexes and Back-Extraction with Mercury(ll) for Determination of Trace Metals in Seawater by Atomic Absorption Spectrometry 2536 The back-extraction procedure is based on the fact that the extraction constant of Hg(II) dithiocarbamate is much greater than those of other trace metals in seawater. The presence of a low concentration of Hg(II) in the backextracted solution does not interfere in GFAAS. J. M. Lo, Institute of Nuclear Science, National Tsing Hua University, Hsinchu, Taiwan, Republic of China, and J. C. Yu, F. I. Hutchison, and C. M. Wai*, Department of Chemistry, University of Idaho, Moscow, Idaho 83843 Anal. Chem.,54 (1982) Dimethyl Ether as a Reagent Gas for Organic Functional Group Determination by Chemical Ionization Mass Spectrometry
2540
The method allows differentiation of isomeric alkenes and cycloalkanes, conjugated and nonconjugated dienes, some polycyclic aromatic hydrocarbons, aldehydes and ketones, acids and esters, alcohols and ethers, and primary and secondary alcohols. T. Keough, The Procter & Gamble Company, Miami Valley Laboratories, P.O. Box 39175, Cincinnati, Ohio 45247 Anal. Chem.,54 (1982)
1448 A · ANALYTICAL CHEMISTRY, VOL. 54, NO. 14, DECEMBER 1982
Briefs Measurement of Carbon Monoxide in Combustion Emissions with a Low-Pressure Sampling System and Low-Resolution Mass Spectrometry 2547 The sampling system includes a liquid-nitrogen-cooled cryogenic trap and a platinum oxidation catalyst. The method is accurate to ±1.2 ppm for the concentration range of 10 to 100 ppm CO. Larry P. Haack*, James W. Butler, and Alex D. Colvin, Ford Motor Company, Scientific Research Laboratory, Rm. S-3061, P.O. Box 2053, Dearborn, Mich. 48121-2053 Anal.Chem.,54 (1982) Determination of Isoniazid in Drugs with 2-lodoxybenzoate 2550 Sample solution is treated with sulfuric acid and a measured excess of 2-iodoxybenzoate. Potassium iodide is added and the liberated iodide titrated with thiosulfate. Krishna K. Verma* and Anil K. Gulati, Department of Chemistry, University of Jabalpur, Jabalpur 482001, India Anal.Chem.,54 (1982) Separation of Tervalent Lanthanides from Actinides by Extraction Chromatography 2552 Actinide recovery from a mixture of 5 mg cerium, 3 mg lanthanum, and 2 mg neodymium is 86% for californium and 96% for americium and curium. Average overall recovery of americium separated from 131 soil samples is 84 ± 6%. Don B. Martin* and Dennis G. Pope, Radiological and Environmental Sciences Laboratory, U.S. Department of Energy, 550 Second Street, Idaho Palls, Idaho 83401 Anal. Chem.,54 (1982) Electrochemical Determination of Adriamycin Compounds in Urine by Preconcentration at Carbon Paste Electrodes 2556 -8 Sensitivities are less than Ι Ο Μ, linear response is in the range of 10~ 5 M to ΙΟ - 7 Μ, and reproducibility is 10% for a 3-miri adsorption period. No sample pretreatment is required. Edward N. Chaney, Jr., and Richard P. Baldwin*, Department of Chemistry, University of Louisville, Louisville, Ky. 40292 Anal. Chem.,54 (1982) Fiber Optic Thin-Layer Spectroelectrochemlstry with Long Optical Path 2560 A thin-layer spectroelectrochemical cell with, volume
