Briefs D e p e n d e n c e of S o l u t e R e t e n t i o n P a r a m e t e r s on S t a t i o n a r y P h a s e M o l e c u l a r W e i g h t in G a s Liquid C h r o m a t o g r a p h y A refined version of Prigogine's theory of c h a i n molecule m i x t u r e s is successfully employed for i n t e r p r e t a t i o n a n d prediction. T h e i m p o r t a n c e of t h e usually neglected struc t u r a l effect is d e m o n s t r a t e d . Daniel E. Martire, Department of Chemistry, Georgetown Uni versity, Washington, D.C. 20007 Anal. Chem. 46, 626 (1974)
D e t e r m i n a t i o n of Iron in G l a s s a n d C o b a l t via Charged Particle Activation Analysis P r o t o n activation m e t h o d s for b o t h destructive a n d non destructive d e t e r m i n a t i o n s of iron a r e developed w i t h d e tection limits e s t i m a t e d a t 50 p p b . Dale L. Swindle, Leo R. Novak, and Emile A. Schweikert, Center for Trace Characterization, Department of Chemistry, Texas A&M University, College Station, Texas 77843 Anal. Chem., 46, 655 (1974)
R o l e of N i t r i c O x i d e in P o s i t i v e R e a c t a n t I o n s in Plasma Chromatography Addition of nitric oxide t o t h e carrier gas in t h e p l a s m a c h r o m a t o g r a p h changes relative c o n c e n t r a t i o n s of t h e ( H 2 0 ) N O + a n d ( Η 2 θ ) η Η + positive r e a c t a n t ions a n d al ters t h e mobility s p e c t r a a n d sensitivity for organic prod u c t ions. Francis W. Karasek and Donald W. Denney, Department of Chemistry, University of Waterloo, Waterloo, Ontario Anal. Chem., 46, 633 (1974)
S i m p l e A p p a r a t u s for O n - S i t e C o n t i n u o u s L i q u i d Liquid E x t r a c t i o n of O r g a n i c C o m p o u n d s from Natural Waters A c o n t i n u o u s solvent extractor, designed for t h e extraction of organic trace s u b s t a n c e s a t field, is described. Polychlor i n a t e d b i p h e n y l s ( P C B ) in river waters a r e d e t e r m i n e d a t sub-pptrange. Martin Ahnoff and Bjorn Josefsson, Department of Analytical Chemistry, University of Gothenburg, Fack, S-402 20 Goteborg 5, Sweden Anal. Chem., 46, 658 (1974)
A p p l i c a t i o n s of F o u r i e r T r a n s f o r m T e c h n i q u e s to Steric-Exclusion Chromatography Substantial correction for peak broadening is made using the peak for a non-retained species. Signal-to-noise en hancement and data reduction are also examined. T. A. Maldacker, J . E. Davis, and L. B. Rogers, Department of Chemistry, Purdue University, West Lafayette, Ind. 47907 Anal. Chem., 46, 637(1974)
P r e l i m i n a r y S t u d i e s of t h e S h o c k T u b e a s a n E x c i t a t i o n S o u r c e for t h e A n a l y s i s of S e l e c t e d Trace Metals in Aqueous Media The bursting-diaphragm shock tube is presented as a new thermal excitation source for the analysis of selected trace metals at the sub ppm level in 100-μ1 aqueous samples of metal salts. Richard D . Sacks and Vincent T. Cordasco, Department of Chemistry, University of Michigan, Ann Arbor, Mich. 48104 Anal. Chem., 46, 663 (1974)
D e t e r m i n a t i o n of E l e c t r o c h e m i c a l K i n e t i c P a r a m e t e r s in H i g h R e s i s t a n c e S o l u t i o n s U s i n g Semiintegration The electrochemical kinetic parameters, ks and a, for the reduction of 2-methyl-2-nitropropane are evaluated using semiintegration of current-potential curves obtained with uncompensated solution resistance. H. W, VandenBorn and Dennis H. Evans, Department of Chemistry, University of Wisconsin-Madison, Madison, Wis. 53706 Anal. Chem., 46, 643 (1974) O n the Instability of Current F o l l o w e r s in Potentiostat Circuits E q u i v a l e n t circuits for several configurations of t h e cur r e n t follower a r e developed. S m a l l signal a n d t r a n s i e n t effects are discussed. T h e i m p u t i m p e d a n c e is shown to have a n inductive c o m p o n e n t . J . E. Davis, Departments of Pathology and Medicine, Washing ton University; Division of Laboratory Medicine, Barnes Hospi tal, St. Louis, Mo. 63110, and E. Clifford Toren, J r . , Departments of Medicine and Pathology, University of Wisconsin, Madison, Wis. 53706 Anal Chem., 46, 647(1974) P r e s e n t S t a t u s of t h e N-Silicon/Stainless Steel C o m b i n a t i o n E l e c t r o d e for Acid D e t e r m i n a t i o n s T h e electrode is critically e x a m i n e d as a general acid m o n i t o r a n d selective H F analyzer with a p p l i c a t i o n to m e t a l bearing acid b a t h s ( H F , HC1, H N 0 3 , H 2 S 0 4 , H3PO4). J. P . McKaveney, Garrett Research and Development Company, Inc., Division of Occidental Petroleum Corporation, La Verne, Calif. 91750, and M. D. Buck, Hach Chemical Company, P.O. Box 907, 713 South Duff, Ames, Iowa 50010 Anal. Chem., 46, 650 (1974)
N e w S p e c t r o p h o t o m e t r y R e a g e n t for the D e t e r m i n a t i o n of O s m i u m - 2 , 3 - Q u i n o x a l i n e d i t h i o l The method presented allows determination of osmium with a sensitivity (for A = 0.001) of 0.011 μ-g cm" 2 in a water-dimethylformamide solution with a relative stan dard deviation of 2%. Harvey F. J a n o t a and Sabrina B. Choy, Department of Chem istry, California State University-Fullerton, Fullerton, Calif. 92634 Anal. Chem., 46, 670 (1974) P h o t o i n d u c e d L u m i n e s c e n c e of 9,10Anthraquinone—Secondary Photolysis Products Secondary photolysis p r o d u c t s in t h e p h o t o i n d u c e d lumi nescence of 9 , 1 0 - a n t h r a q u i n o n e are 9 - a n t h r a n o l , a n t h r o n e , 9-anthranol p h o t o d i m e r , a n t h r a p i n a c o l , a n d a "362 inter m e d i a t e . " T h e l a t t e r is t e n t a t i v e l y identified a s 7,16-dihydrodibenzo[a,o] perylene. David M. Hercules and Steven A. Carlson, Department of Chemistry, University of Georgia, Athens, Ga. 30602 Anal Chem., 46. 674 (1974) Easily Operated Direct Current Argon P l a s m a Arc for A t o m i c S p e c t r o m e t r i c A n a l y s i s An easily operated dc plasma arc is designed and studied. Detection limits are 1.5 ppm for Hf, 0.06 ppm for Cu, and 0.01 ppm for Ca. Phosphate does not interfere with Ca. D. A. Murdick, J r . , and Ε. Η. Piepmeier, Department of Chemistry, Oregon State University, Corvallis, Ore. 97331 Anal. Chem., 46, 678 (1974)
ANALYTICAL CHEMISTRY, VOL. 46, NO. 6, MAY 1974 · 497 A
Briefs Direct Determination of Heavy Elements in Biological Media by Spark Source M a s s Spectrometry
High Resolution Atomic Absorption Spectrometry Using an Echelle Grating Monochromator A comparison is m a d e between line a n d c o n t i n u u m sources in conjunction with a high resolution échelle grating m o n o c h r o m a t o r . P . N . Keliher and C. C. Wohlers, Chemistry Department, Villanova University, Villanova, Pa., 19085 Anal. Chem., 46, 682 (1974)
Utilizing calibration curves, t h e heavy e l e m e n t content of blood, tissue, a n d urine is d e t e r m i n e d by direct sampling a n d t h e use of s p a r k source m a s s s p e c t r o m e t r y . A. W. Fitchett and R. P . Buck, William Rand Kenan, Jr., Lab oratories of Chemistry, University of North Carolina, Chapel Hill, N.C. 27514, and P a u l Mushak, Department of Pathology, Uni versity of North Carolina, Chapel Hill, N.C. 27514 Anal. Chem., 46, 710(1974)
S e p a r a t i o n of T r a c e A m o u n t s of U r a n i u m a n d Thorium and Their Determination by M a s s Spectrometric Isotope Dilution Typical internal precision for a single r u n of the 238/235 ratio o b t a i n e d for t h e U-500 s t a n d a r d is ± 0 . 0 3 % a n d ± 0 . 1 2 % for t h e 238/234 ratio. J . W. Arden and Ν. Η. Gale, Department of Geology and Miner alogy, University of Oxford, Parks Road, Oxford, England Anal. Chem., 46, 687(1974)
S t r u c t u r a l I n t e r p r e t a t i o n of P r o t o n M a g n e t i c Resonance Spectra by Computer: First Order Spectra A c o m p u t e r program is described for s t r u c t u r a l interpre tation of essentially first order P M R spectra. Results are presented for t h i r t y c o m p o u n d s which contain C, Η , Ο, Ν , CI, a n d S. Graham Beech, Roger T. Jones, and Keith Miller, The Poly technic, Wolverhampton WV1 1LY, England Anal. Chem., 46, 714 (1974)
Spectrophotometric Determination of Copper and Iron Subsequent to the Simultaneous Extraction of Bis(2,9-dimethyl-1, lO-phenanthroline)copper(I) and Bis[2,4,6-tri(2-pyridyl)-l,3,5-triazine]iron(II) into Propylene Carbonate
A u t o m a t i c D i g i t a l S y s t e m for Q u a n t i t a t i v e K i n e t i c A n a l y s i s — A p p l i c a t i o n to C a t a l y t i c D e t e r m i n a t i o n of T h y r o i d H o r m o n e s T h e system is developed for t h e d e t e r m i n a t i o n of thyroid hormones a n d allows d e t e r m i n a t i o n of a s little as 0.20 na nogram of T3 a n d 0.10 n a n o g r a m of T4. Gunter Knapp, Department of General Chemistry, Micro- and Radiochemistry, Technical University, Graz, Austria, and Hans Leopold, Department of Physical Chemistry, University of Graz, Austria Anal. Chem., 46, 719(1974)
D e t e r m i n a t i o n s a t relative s t a n d a r d deviations of 0.48% (Cu) a n d 0.63% (Fe) over the ranges of m i n i m u m analysis error are reported. B. G. Stephens, H. L. Felkel, J r . , and W. M. Spinelli, Depart ment of Chemistry, Wofford College, Spartanburg, S.C. 29301 Anal. Chem., 46, 692(1974) D e t e r m i n a t i o n of P a l l a d i u m b y C o n t r o l l e d Potential Coulometry. N e w Platinum-WorkingE l e c t r o d e Cell for C o n t r o l l e d - P o t e n t i a l Coulometry Milligram a m o u n t s of p a l l a d i u m are d e t e r m i n e d with a n accuracy a n d precision of 0 . 1 % using the P d ( I V ) / P d ( I I ) couple in n e u t r a l azide m e d i u m . L. P . Rigdon and J . E. H a r r a r , General Chemistry Division, Lawrence Livermore Laboratory, University of California, Livermore, California 94550 Anal. Chem., 46, 696 (1974)
Notes S e p a r a t i o n a n d D e t e r m i n a t i o n of T h y r o i d Hormones in Blood Serum A rapid d e t e r m i n a t i o n of T 3 a n d T4 in blood serum by column c h r o m a t o g r a p h y is described. T h e T 4 content of the eluted T3 a m o u n t s to less t h a n 0.05% of the total T 4 present. Gunter Knapp and Hans Spitzy, Department of General Chem istry, Micro-, and Radiochemistry, Technical University, Graz, Austria, and Hans Leopold, Department of Physical Chemistry, University of Graz, Austria Anal. Chem., 46, 724 (1974)
Photographic Quantitation in Spark Source M a s s Spectrography Using an On-Line Densitometer and Ion Intensity Areas A digital system for acquisition of t r a n s m i t t a n c e profiles, emulsion calibration, a n d c o m p u t a t i o n of concentrations is developed, evaluated, a n d applied to peak-height, linewidth, a n d i n t e g r a t e d intensity m e a s u r e m e n t s . R. A. Burdo, J. R. Roth, and G. H. Morrison, Department of Chemistry, Cornell Universtiy, Ithaca, N.Y. 14850 Anal. Chem., 46, 701 (1974)
Subpicogram Detection System for Gas P h a s e Analysis Based upon Atmospheric P r e s s u r e Ionization (API) M a s s Spectrometry A new type of ion source for a m a s s s p e c t r o m e t e r is de scribed. A flowing s t r e a m of nitrogen a t a t m o s p h e r i c pres sure is irradiated w i t h electrons from a 6 3 N i source. Lower limits of detection are in t h e femtogram range. D. I. Carroll, I. Dzidic, R. N . Stillwell, M. G. Horning, and E. C. Horning, Institute for Lipid Research, Baylor College of Medi cine, Houston, Texas 66025 Anal. Chem., 46, 706 (1974)
I s o b u t a n e C h e m i c a l I o n i z a t i o n M a s s S p e c t r a of Lanthanide Perfluorinated β -Diketonates T h e i s o b u t a n e chemical ionization m a s s spectra of lan t h a n i d e perfluorinated β -diketonates are shown to be easi er to interpret t h a n t h e corresponding electron i m p a c t m a s s spectra. T. H. Risby, P. C. J u r s , and F. W. Lampe, Department of Chemistry, The Pennsylvania State University, University Park, Pa. 16802, A. L. Yergey, Scientific Research Instruments Corpo ration, 6707 Whitestone Road, Baltimore, Md. 21207 Anal. Chem., 46, 726(1974)
ANALYTICAL CHEMISTRY, VOL. 46, NO. 6, MAY 1974 · 499 A
Briefs Use of a New Variable Wavelength Detector in High Performance Liquid Chromatography
Charge Exchange M a s s Spectra of Trimethylsily E t h e r s of Biologically I m p o r t a n t Compounds: An Analytical Technique A c o m b i n a t i o n of high pressure m a s s s p e c t r o m e t r y a n d gas c h r o m a t o g r a p h y is used for r a p i d identification of c o m p o u n d s whose charge exchange m a s s s p e c t r a c o n t a i n more a b u n d a n t M+ ions t h a n t h e conventional electron m a s s spectra. B a r b a r a Jelus and Burnaby Munson, Chemistry Department, University of Delaware, Newark, Del. 19711, and Catherine Fenselau, Department of Pharmacology and Experimental Thera peutics, John Hopkins University School of Medicine, Baltimore, Md. 21205 Anal. Chem., 46, 729 (1974)
New Spray Reagent for the Identification of Accelerators in Unvulcanized Rubber Compounds by Thin Layer Chromatography T h i s procedure m a k e s use of a visualizing r e a g e n t n o r m a l ly used in biochemical d e t e r m i n a t i o n s which can readily distinguish accelerators from a n t i o x i d a n t s . Marjorie B. Millingen, Olympic Tyre & Rubber Company, Cross Street, West Footscray, Victoria, Australia Anal. Chem., 46, 746(1974)
Liquid Coal Compositional Analysis by M a s s Spectrometry A m a s s spectrometric group-type analysis for coal liquids is developed which a c c o u n t s for 17 h y d r o c a r b o n t y p e s found in t h e a r o m a t i c fraction J . T. Swansiger, F . E. Dickson, and H. T. Best, Gulf Research & Development Company, Pittsburgh, Pa. 15230 Anal. Chem., 46, 730(1974)
Gas Liquid Chromatographic Analysis of Alkyl Alcohols, Alkyl Cyanoacetates, and Alkyl 2Cyanoacrylates
Bead Homogeneity in the Fusion Technique for X-Ray Spectrochemical Analysis
T h e i d e n t i t y a n d a m o u n t s of u n k n o w n c o m p o u n d s in t h e same series are e v a l u a t e d on a p r e c a l i b r a t e d gas c h r o m a t o g r a p h e q u i p p e d with a hydrogen flame ionization detec tor. Ramchandra K. Kulkarni, Eric C. Johnson, and Clarence W. R. Wade, U.S. Army Medical Bioengineering Research & Devel opment Laboratory, Fort Detrick, Frederick, Md. 21701 Anal. Chem., 46, 749(1974)
M a n u a l a n d continuous agitation d u r i n g fusion in t h e p r e p a r a t i o n of b o r a x b e a d s for X - r a y fluorescence analysis are c o m p a r e d . H o m o g e n e i t y is a t t a i n e d in a m u c h shorter t i m e with c o n t i n u o u s a g i t a t i o n . Roland LeHouillier and Simon Turmel, Mineral Research Cen ter, Department of Natural Resources, Quebec, Canada Anal. Chem., 46, 734 (1974)
G a s C h r o m a t o g r a p h i c D e t e r m i n a t i o n of T h i o p e n t a l in P l a s m a U s i n g an Alkali F l a m e Ionization Detector Quantification of t h i o p e n t a l in p l a s m a is achieved to a lower limit of a b o u t 50 μ g per m l . Q u a n t i t a t i v e recoveries with precisions of ± 4 - 7 % are realized in t h e range of 0 . 4 5.0^g per m l . Lawrence T. Sennello and Fred E. Kohn, Division of Experi mental Therapy, Abbott Laboratories, North Chicago, 111. 60064 Anal. Chem., 46, 752(1974)
N e w M e t h o d of A n a l y s i s B a s e d o n R o o m Temperature Phosphorescence R o o m - t e m p e r a t u r e phosphorescence of nine ionic organic molecules absorbed on filter p a p e r is shown to have po tential analytical utility. R. A. Paynter, S. L. Wellons, and J. D. Winefordner, Depart ment of Chemistry, University of Florida, Gainesville, Fla. 32601 Anal. Chem., 46, 736 (1974) D e t e r m i n a t i o n of S o l u b l e C a d m i u m , L e a d , S i l v e r , a n d I n d i u m in R a i n w a t e r and S t r e a m W a t e r w i t h t h e U s e of F l a m e l e s s A t o m i c A b s o r p t i o n E l i m i n a t i o n of interferences in t h e d e t e r m i n a t i o n of m e t als in rain a n d s t r e a m water are described. Precision is ± 5 % for triplicate d e t e r m i n a t i o n s . Anthony Rattonetti, Illinois State Water Survey, Box 232, Urbana, 111. 61801 Anal. Chem., 46, 739 (1974) A n a l y s i s of 1 , 2 , 3 , 4 , 1 0 , 1 0 - H e x a c h l o r o l,4,4a,5,8,8a-hexahydro-l,4-e/ido-e*o-5,8-dimethanonaphthalene by N u c l e a r Quadrupole R e s o n a n c e Spectrometry T h e c o m p l e t e N Q R s p e c t r u m of aldrin is reported a t vari ous t e m p e r a t u r e s . T h e six signals recorded are t e n t a t i v e l y assigned to t h e specific chlorine a t o m s of aldrin utilizing s p e c t r a - s t r u c t u r e correlation c h a r t s . Dina Gegiou, Experimental Research Department, General State's Laboratories. 16A. TsochaSt., Athens, Greece Anal. Chem., 46, 742 (1974)
Selection of t h e d e t e c t i n g wavelength in liquid c h r o m a t o g r a p h y is shown to improve detection sensitivity for c o m p o u n d s with low a b s o r b a n c e a t 254 n m b u t high a t other w a v e l e n g t h s . C. David Carr, Varian Instrument Division, Separation Sciences Application Laboratories, 611 Hansen Way, Palo Alto, Calif. 94303 Anal. Chem., 46, 743 (1974)
Modified Electrolytic Conductivity D e t e c t o r Cell for G a s C h r o m a t o g r a p h y A new, c o m p a c t , t e m p e r a t u r e controlled electrolytic con ductivity detector with a d j u s t a b l e w a t e r flow rates is five t i m e s more sensitive t h a n the commercial Coulson cell. J a m e s F. Lawrence and Alan H. Moore, Food Research Labo ratories, Health Protection Branch, Health and Welfare Canada, Tunney's Pasture, Ottawa, Ontario K1A OL2 Anal. Chem., 46, 755(1974) E s t i m a t i o n of Choline a n d A c e t y l c h o l i n e i n T i s s u e by Pyrolysis Gas Chromatography C o n c e n t r a t i o n assay of acetylcholine a n d choline from bi ological tissue is described. Average recovery is 87% a n d positive identification of the p e a k s is provided by m a s s spectrometry. William B. Stavinoha and Susan T. Weintraub, Department of Pharmacology, The University of Texas Health Center at San Antonio, San Antonio, Texas 78284 Anal. Chem., 46, 757 (1974)
ANALYTICAL CHEMISTRY, VOL. 46, NO. 6, MAY 1974 · 501 A
Briefs G a s C h r o m a t o g r a p h i c D e t e r m i n a t i o n of Nonvolatile Fatty Acids in Cigarette Smoke T h i s procedure is b a s e d on t h e trimethylsilylation of whole condensate or p a r t i c u l a t e m a t t e r . Relative s t a n d a r d deviations of 5% or b e t t e r are typically observed for analysis of p a r t i c u l a t e m a t t e r . M. R. Guerin, Géraldine Olerich, and W. T. Rainey, Oak Ridge National Laboratory, Oak Ridge, Tenn. 37830 Anal. Chem., 46, 761 (1974)
C o n c e n t r a t i o n of H e a v y M e t a l s b y C o m p l e x a t i o n on Dithiocarbamate Resins T h e d i t h i o c a r b a m a t e resin achieves q u a n t i t a t i v e removal of a large n u m b e r of m e t a l s from aqueous m e d i a . B a t c h equilibrium followed by analysis with a t o m i c absorption spectrometry is used. Joseph F. Dingman, J r . , Kenneth M. Gloss, Ellen A. Milano, and Sidney Siggia, University of Massachusetts, Amherst, Mass. 01002 Anal. Chem., 46, 774 (1974)
A d v a n t a g e of S h o r t C o n t r o l l e d D r o p T i m e s for Alternating Current Polarography in H i g h Resistance Solvents Results confirm t h a t t h e ohmic p o t e n t i a l loss can be decreased significantly by using a short controlled drop t i m e . Useful ac p o l a r o g r a m s are recorded w i t h o u t the need for positive feedback iR c o m p e n s a t i n g circuitry. D. R. Canterford, Department of Physical Chemistry, University of Melbourne, Parkville 3052, Victoria, Australia Anal. Chem., 46, 763(1974)
M i c r o d e t e r m i n a t i o n of H y d r a z i n e S a l t s a n d Certain Derivatives with iV-Chlorosuccinimide A new m e t h o d utilizing s t a n d a r d 7V-chlorosuccinimide solution is described. T h e proposed m e t h o d is sensitive with a m o u n t s as low as 100)ig d e t e r m i n e d with a n absolute accuracy of ± 2 % . M. Z. B a r a k a t , M. A. El-Makarem, and M. A. El-Raoof, Biochemistry Department, Faculty of Medicine, Azhar University, Madina Nasr, Cairo, Egypt Anal. Chem., 46, 777 (1974)
P o t e n t i o m e t r i c M i c r o t i t r a t i o n of S u l f a t e I o n U s i n g a S o d i u m - S e l e c t i v e G l a s s Electrode in a Nonaqueous Medium A s h a r p point of inflection in t h e t i t r a t i o n of sulfate with Ba 2 + in 70% acetone is registered by t h e electrode. T h e p o t e n t i a l j u m p is a t r a n s i e n t response to t h e s u d d e n change in [Ba 2 + ]. Naoshige Akimoto, Faculty of Pharmaceutical Sciences, Kyoto University, Kyoto 606, Japan, and Keiichiro Hozumi, Kyoto College of Pharmacy, Kyoto 607, Japan Anal. Chem., 46, 766 (1974) P o l a r o g r a p h i c M e t h o d for t h e D e t e r m i n a t i o n of Hexafluorosilicate S i F 6 2 " shifts EV2 for t h e U(V) — U(III) wave. A m e t h o d of d e t e r m i n a t i o n of SiF6 2 ~ b a s e d on this shift is given, and its applicability to t h e analysis of c h r o m i u m p l a t i n g b a t h s is outlined. Indira Rajagopalan and S. R. Rajagopalan, Materials Science Division, National Aeronautical Laboratory, Bangalore 560017, India Anal. Chem., 46, 769(1974) L o s s e s o f T r a c e C o n c e n t r a t i o n s of C a d m i u m f r o m Aqueous Solution during Storage in Glass Containers C a d m i u m in aqueous solution can b e absorbed on the walls of glass containers a t p H > 7. Losses of Cd d e p e n d on container m a t e r i a l , p H , a n d concentration of Cd in water. W. G. King, J . M. Rodriguez, and C. M. Wai, Department of Chemistry, University of Idaho, Moscow, Idaho 83843 Anal. Chem., 46, 771 (1974) F u s i o n M e t h o d s for t h e D e t e r m i n a t i o n o f Intractable Organic Compounds (Including Polymers) Fusion reagents, fluxes, a n d m e a s u r i n g a p p r o a c h e s are discussed a n d t h e application of fusion reactions is explored. Sidney Siggia and David D. Schlueter, Department of Chemistry, University of Massachusetts, Amherst, Mass. 01002 Anal. Chem., 46, 773 (1974)
P l a s m a C h r o m a t o g r a p h y of I s o m e r i c H a l o g e n a t e d Nitrobenzenes T h e electron a t t a c h m e n t a n d proton transfer reaction of 15 halogenated nitrobenzenes show formation of dissociative negative product ions a n d p r o t o n a t e d molecular ions t h r o u g h mobility m e a s u r e m e n t s a t a t m o s p h e r i c pressure. Francis W. Karasek and David M. Kane, Department of Chemistry, University of Waterloo, Waterloo, Ontario, Canada Anal. Chem., 46, 780(1974) D i r e c t D e t e r m i n a t i o n of F e r r o u s I r o n in S i l i c a t e R o c k s and M i n e r a l s by Iodine Monochloride A m e t h o d is presented which is free of interferences from c h r o m i u m or m a n g a n e s e a n d h a s a precision of ± 2 % . Subrata Banerjee, Department of Geology, University of Georgia, Athens, Ga. 30602 Anal. Chem., 46, 782 (1974) A u t o m a t e d L o a d i n g of D i s c r e t e , M i c r o l i t e r V o l u m e s of L i q u i d s into a M i n i a t u r e F a s t Analyzer D e v e l o p m e n t of a versatile loader for precise ( < ± 1 . 0 % ) , accurate ( ± 1 . 0 % ) , r a p i d (5 m i n ) , a n d a u t o m a t i c introduction of microliter volumes of samples a n d reagents into t h e rotor of a m i n i a t u r e F a s t Analyzer. C. A. Burtis, W. F . Johnson, and J. B. Overton, Oak Ridge National Laboratory, Oak Ridge, Tenn. 37830 Anal. Chem., 46. 786(1974) S p e c t r o p h o t o m e t r i c D e t e r m i n a t i o n of P i c e i n a n d p - H y d r o x y a c e t o p h e n o n e i n N e e d l e s oîPicea abies with 2,4-Dinitrophenylhydrazine T h e proposed procedure allows a q u a n t i t a t i v e d e t e r m i n a tion (recovery 96-106%) of picein a n d p - h y d r o x y a c e t o phenone in p l a n t m a t e r i a l s . T h e relative s t a n d a r d deviations ranged from 0.5-6.5%. Hermann Esterbauer, Dieter Grill, and Gerhard Beck, Institut fur Biochemie und Institut fur Anatomie and Physiologie der Pflanzen, Universitat Graz, A-8010 Graz, Austria Anal. Chem., 46, 789(1974)
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Briefs S i m p l e M e t h o d for the P r e p a r a t i o n , S t o r a g e , and U s e of C h r o m o u s Chloride S o l u t i o n s When prepared in a polyethylene squeeze bottle with a long delivery tube, air-sensitive solutions of chromous chloride can be stored and dispensed for several weeks without significant reoxidation. Roger L. Williams and Claude W. Sill, Health Services Laboratory, U.S. Atomic Energy Commission, Idaho Falls, Idaho 83401 Anal. Chem., 46, 791 (1974)
R a p i d and C o n v e n i e n t L a b o r a t o r y M e t h o d for Extraction and Subsequent Spectrophotometric D e t e r m i n a t i o n of B i t u m e n Content of B i t u m i n o u s Sands Anew procedure with photometric repeatability of 1.26% and precision of 1.20% bitumen is described. Total time required for analysis ranges from 1 to 2 hours. Mahendra S. Patel, Product Research and Development Division, Research Council of Alberta, 11315—87 Avenue, Edmonton, Alberta, Canada T6G 2C2 Anal. Chem., 46, 794 (1974)
D e t e r m i n a t i o n of Iron in S e r u m by A t o m i c Fluorescence Flame Spectrometry The relative standard deviation for measurements of a 0.5 Mg/ml standard solution and a pooled serum sample is approximately 3%. No treatment of the sample is required prior to nebulization into a premixed acetylene-air flame. W. E. Rippetoe, V. I. Muscat, and T. J. Vickers, Department of Chemistry, Florida State University, Tallahassee, Fla. 32306 Anal. Chem., 46, 796(1974)
Correspondence R e l a t i v e Effect of M o l e c u l a r Absorption on A t o m i c Absorption and A t o m i c F l u o r e s c e n c e C. David West, Department of Chemistry, Occidental College, Los Angeles, Calif. 90041 Anal. Chem., 46, 797(1974)
Aids for Analytical Chemists S i m p l e a n d I n e x p e n s i v e T e m p e r a t u r e Controlled S p e c t r o p h o t o m e t r i c Cell Holder R. L. Wilson and J. D. Ingle, Jr., Department of Chemistry, Oregon State University, Corvallis, Oregon 97331 Anal. Chem., 46, 799(1974)
Optical D r o p F a l l D e t e c t o r for U s e w i t h a D r o p p i n g M e r c u r y Electrode Brian K. Hahn and C. G. Enke, Department of Chemistry, Michigan State University, East Lansing, Michigan 48823 Anal. Chem., 46, 802(1974)
A u t o m a t i c H i g h T e m p e r a t u r e V e n t V a l v e for a Gas Chromatograph/Mass Spectrometer Interface Douglas W. Kuehl, Gary E. Glass, and Frank A. Puglisi, National Water Quality Lab., EPA, 6201 Congdon Blvd., Duluth, Minn. 55804 Anal. Chem., 46, 804 (1974)
I n t e r n a l S t a n d a r d Addition M e t h o d for P r e p a r a t i o n of H o m o g e n e o u s P o w d e r M i x e s John J. Jaworski, Ronald A. Burdo, and George H. Morrison, Department of Chemistry, Cornell University, Ithaca, N.Y. 14850 Anal. Chem., 46, 805 (1974)
Split Crystal Ion S e l e c t i v e M e m b r a n e E l e c t r o d e s Ronald Wawro and G. A. Rechnitz, Department of Chemistry, State University of New York, Buffalo, N.Y. 14214 Anal. Chem., 46, 806 (1974)
ACS Reprint Collections Instrumentation in Analytical Chemistry Comprises 43 articles from Volumes 41 - 4 4 of Analytical Chemistry. Spectrometry, chromatography, electrochemistry, and other techniques. 428 pages 1973 Hardback $7.95, Paper $4.50. Collected Accounts of Transition M e t a l Chemistry Includes 29 articles from Volumes 1 - 4 , Accounts of Chemical Research. Structure, bonding, inorganic reaction mechanisms, organometallic compounds and reactions, biological aspects. 249 pages 1 973 Hardback $6.95, Paper $3.95. Air Pollution Contains 38 articles from Volumes 3 - 6 of Environmental Science & Technology. Laws and regulations, specific pollutants and standards, monitoring, control methods, transportation. 139 pages 1973 Hardback $5.95, Paper $3.50. Solid W a s t e s 25 articles that originally appeared in Environmental Science & Technology. Government, specific solids, mining, sewage sludge, technology. 87 pages 1971 Paper $2.00. Cleaning Our Environment. The Chemical Basis for Action 249 pages 1 969 Paper $2.75. Supplement to Cleaning Our Environment. The Chemical Basis for Action 20 pages 1971 Paper $1.00. All books postpaid in U.S. and Canada, plus postage elsewhere. Order from: Special Issues Sales American Chemical Society 11 55 Sixteenth St., N.W. Washington, D.C. 20036 ANALYTICAL CHEMISTRY, VOL. 46, NO. 6, MAY 1974 · 505 A
