Anal. Chem. 1983, 55, 31 R-40R (425) Hamer, P. S. J. Forensic Sci. SOC. 1982, 22 (2),187. (426) Castle, D. A. J . Forensic Sci. SOC. 1982, 22 (2),179. (427) Home, J. M.; Lalng, D. K.; Dudley, R. J. J . Forensic Sci. Sot. 1982, 22(2),147. (426)Linde, H. G. J . Forensic Sci. 1980, 25 (4),870. (429) Cardosi, P. J. Forensic Sci. 1982, 27 (3),695. (430) Sansom, P. C. Anal. R o c . (London) 1981, 78 (9),393. (431) Wheals, B. B. J . Anal. Appi. &ro/ysis 1981, 2 (4), 277. (432) Zieba, J. Forensic Sci. Int. 1981, 77 (2),101. (433) Curry, C. J.; Rendle, D. F.; Rogers, A. J. Forensic Sci. SOC.1982, 22 (2),173. (434) Audette, R. J.; Percy, R. F. E. J . Forensb Sci. 1982, 27 (3),622. (435) Ryland, S.G.; Kopec, R. J.; Somerville, P. N. J . Forensic Sci. 1981, 26 (I),64. (436) Raaschou Nlelsen, H. K. Scand. Paint Print Ink Res. Ins!. 1981, I , 13-81 W T . (437) Slater, D. P.; Fong, W J. Forensic Sci. 1982, 27 (3),474. (438) Locke, J. J. Forensic Sci. SOC. 1982, 22 (2),257. (439)Locke, J.; Sanger, D. Ci.; Roopnarlne, G. Forensic Sci. Int. 1982, 20 (3),295 (440) Daucrs, M. M.; Dudley, R. J.; Smalldon, K. W. Forensic Sci. Int. 1980, 76 (2),1125. (441) Lloyd, J. B. F. J. Forensic Sci. 1961, 26 (2), 325. (442) Eve% I.W.; Lambert, J. A. Forensic Sci. Int. 1982, 20 (3),237. (443) Grove, D. M. Forensic Sci. Int. 1981, 78 (2),169. (444)Howden, C. R.; Dudley, R. J.; Smalldon, K. W. X-Ray Spectrom. 1981, 70 (3),98. (445) Catterlck, T.; Hickman, D. A. Forensic Sci. Int. 1981, 7,7 (3),253. (446) Hlckman, D. A. Forensic Sci. Int. 1981, 77 (3),265. (447) Herod, D. W.;Menzel, E. R. J. Forensic Sci. 1982, 27 (I),200. (448) Herod, D. W.; Menzel, E. R. J. Forensic Sci. 1982, 27 (3),513. (449) Dalrymple, B. E. J . Forensic Sci. 1982, 27(4),801. (450) Menilel, E. R. J . Forensic Sci. 1982, 27 (4).918. (451) Creer, K. E. Forensic Sci. In?. 1982, 20 (2),179. (452) Feldrnan, M. A.; Meioan, C. E.; Lambert, J. L. J . Forensic Sei. 1982, 27 (4),806. (453) Almog, J.; Hlrshfeld, A.; Klug, J. T. J. Forensic Sci. 1982, 27 (4),912. (454) Kerr, F. M.; Westland, A. D.; Haque, F. Forensic Sci. Int. 1981, 78 (2),209. (455) Gupta, S. K.; Rohllla, D. R.; Jain, M. K. J . Can. Forensic Sci. SOC. 1981, 74 (I),23. (456) Ziderman, I. I. J . Forensic Scl. 1981, 26 (2),387. (457) Ziderman, I. 1. Sep. Sci. Technoi. 1982, 17(10),1253. (458) Ebare, H.; Kondo, A,; Nlschida, S. Kagaku Keisatsu Kenkyusho Hokoku, Kokcigaku Hen 1982, 35 (2),88. (459) Lyter, A. H. J . Forensic Sci. 1982, 27(1), 154. (460)Clemiant, J. L.; Ceccaldi, P. F. Int. Crim. Police Rev. 1981, 350, 186. (461) Siouffi, A.; Gulochon, G. J . Chromatogr. 1981, 209 (3),441. (462) Davls, E. A.; Lyter, A. H. J . Forensic Sci. 1982, 27 (2),424. (463) Chaperlin, K. Forensic Sci. Int. 1981, 78 (I), 79.
(464) Reuland. D. J.; Yrlnler, W. A. Forensic Sci. Int. 1981, 78 (2),201. (465) Blackledge, R. D. J . Forensic Sci. 1981, 26 (3),554. (466) Blackledge, R. D. J. Forensic Sci. 1981, 26 (3),557. (467) Baggi, T. R.; Murty, H. R. K. forensic Sci. Int. 1982, 79 (3),259. (468) Adrasko, J. Forensic Sci. Int. 1981, 77 (3),235. (469) Rendle, D. F. J. Forensic Sci. 1981, 26 (2),343. (470) Kokocinski, C. W.; Brundage, D. J.; Nicol, J. D. J. Forensic Sci. 1980, 25 (4),810. (471) Gulnn, V. P. J. Radioanal. Chem. 1982, 72 (1-2),645. (472) Lloyd, J. 8. F.; Weston, N. T. J. forensic Sci. 1962, 27 (2),352. (473)Lloyd, J. B. F. J . Forensic Sci. SOC. 1982, 22 (2),161. (474)Thorsen, K. A. J. Can. Forensic Sci. SOC. 1981, 74 (2),55. (475) Safersteln, R. "Crlminallstlcs: An Introductlon to Forensic Sclence", 2nd ed.; Prentice-Hall: Englewood Cliffs, NJ, 1981. (476) Eckert, W. G., Ed. "Introductlon to Forensic Sclences"; C. V. Mosby: St. Louis, MO, 1980. (477) Maehly, A.; Stromberg. L. "Chemical Criminalistics"; Springer-Verlag: Berlin, 1981. (478) Safersteln, R., Ed. "Forenslc Science Handbook"; Prentice-Hall: Englewood Cllffs. NJ, 1982. (479) Curran, W. J., McGarry, A. L., Petty, C. S.,Eds. "Modern Legal Medicine Psychlatry and Forenslc Science"; F. A. Davis: Philadelphla, PA,
1980. (460) Svensson, A.; Wendel, 0.; Flsher, B. A. J. "Techniques of Crime !%ene Investigation", 3rd ed.; Elsevier North Holland: New York, 1981. (481) Hilton, 0."Scientiflc Examlnation of Questioned Documents"; Elsovier North Holland: New York, 1981. (482) , Cravey. R. H., Baselt, R. C., Eds. "Introduction to Forensic Toxicology"; Biomedical Publications: Davis, CA, 1982. (483) Baselt, R. C. "Disposition of Toxlc Drugs and Chemicals in Man", 2nd ed.; Biomedlcal Publications: Davis, CA, 1982. (484)Gottschaik, I-. A.; Cravey, R. H. "Toxlcofogical and Pathological Studies on Psychoactive Drug Involved Deaths"; Biochemical Publicatlons: Drrvis, CA, 1980. (485) Goldberg, L., Ed. "Alcohol, Drugs, and Traffic Safety (Proceedings at the Eighth International Conference)"; Almgvist and Wiksell: Stockholm,
1980. (486)Emerson, V. J.; Hoileyhead, R.; Isaacs, M. D. J.; Fuller, N. A.; Hunt, D. J. "The Measurement of Breath Alcohol"; The Forensic Sclence Society: Harrogate, England, 1980. (487) Hollyhead, R. "A Bibliography on Ethyl Alcohol for Forensic Science and Medicine and the Law"; The Forensic Science Society: Harrogate, England, 1980. (488) Yinon, J.; Zltrin, !3. "The Analysis of Explosives"; Pergamon Press: New York, 1981. (489) Yallop, H. J. "Explosion Investigation"; The Forensic Science Society: Harrogate, England, 1980. (490) Grunbaum, B. W., Ed. "Handbook for Forensic Indlvidualization of Human Blood and Bloodstains"; Sartorius: Hayward, CA, 1981.
Solid and Gaseous Fuels Hyman Schultz," Arthur W. Wells, and Gary
L. Smith
Department of Energy, Pittsburgh Energy Technology Center, Pittsburgh, Pennsylvania 15236
SOLID FUELS This section covers methods of sampling, analyzing, and testing coal, coke, and related materials. Energy Research Abstracts and Chemical Abstracts were used as the primary reference iiources. In most categories the volume of material available made it necessary to limit the number of publications in the reviiew.
SAMPLING AND PROXIMATE ANALYSIS Sampling. The theory and practice of coal sampling and samplingpreparation were reviewed by Scholz (25A). Glraham (IOA)discussed quality control considerationsin coal sampling techniques for laboratory analysis. Nir-El et al. (2OA) assembled a new set of 100-kg coal standards for use with prompt neutron activation analysis (NAA) field systems. The standards were calibrated by using the American Society for Testing and Materials (ASTM) methods. Proximate Analysis. Rapid proximate analysis of coal and coke using thermogravimetry was discussed by Ottaway (22A). Althapp et al. ( I A )described equipment for thermoThis article not subject to
US. Copyright.
gravimetric analysis of coal along with the working principles and various applications. Cardillo (5A),Cumming (6A),and Ghetti (8A)compared standard ASTM methods for proximate analysis with thermogravimetric analysis techniques. Recent advances in microcomputer-controlled thermogravimetry of coal for proximate analysis were examined by Earnest and Fyans (7A). Jenke and Hannifan (14A)determined moisture and volatde content of coal by measuring the pressure change and chromatographically analyzing the gas produced in a constant temperature-volume reactor. Simultaneous determination of moisture and ash content of coal using y-emission following thermal neutron capture was demonstrated by Starchik et al. (28A). An apparatus for the determination of the moisture content of coal on a main conveyor using an infrared sensor was described by Kawatetsu (15A). Brown et al. (4A) discussed the use of various electromagnetic techniques, including capacitance, microwave attenuation, and nuclear magnetic resonance in determining moisture in coal.
Published 1983 by the American Chemical Society
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SOLID AND GASEOUS FUELS
Ash. Konovalov and Lukina (17A) related the errors associated with the gravimetric determination of ash in highsulfur coals. Neutron activation analysis was used by Starchik and Ryashchikov (29A) to determine carbon-oxygen ratios for calculating ash content. Janczyszyn and Aleksander (13A) used fast neutrons from a Pu/Be source to analyze pit coal for ash content. Radiometric analysis of brown coal for ash content was described by Bortnik (2A). Starchik et al. (30A) developed a procedure for optimizing a radioisotopic ash content monitor for a coal stream. Onishchenko and Belonozhko (21A)studied the effect of various parameters on ash analysis by radiometry. Page and Fox (23A) exposed powdered coal to primary radiation (46 keV and 9-16 keV y- and X-rays from zlOPb) for ash content determination. Watt and Gravitis (32A) measured the intensity of X-rays or low-energy y-rays to determine the concentration of ash. Sowerby (27A) used annihilation radiation techniques and Compton scattering to determine ash concentration in coal. Gozani et al. (9A) reviewed mass-flow devices for coal handling, in relation to continuous on-line NAA of coal for ash content. Watt and Gookes (33A)and Krampe (18A)described methods for determining ash or mineral content of coal by transmission or Scattering of X- or y-rays. Ash content of coal was determined by Kawatra (16A)in an aqueous slurry by measuring scattered Ag K radiation. Correction for the variation of percent solids and the iron content was necessary. Rapid estimation of percent ash in coal from percent silicon obtained vl'a fast NAA, X-ray fluorescence (XRF), and slurry injection atomic absorption spectrometry techniques (AAS) was presented by Hicks (1IA) and O'Reilly (12A). Volatile Matter. Niac et al. (19A)developed a correlation between the volatile matter and ash content of coal. The correlation coefficient is >0.99. Determination of volatile matter in coal by the diffusionreflection method was performed by Sumitomo (31A). Calculating the ratio of the intensities of the 3000-3100 cm-l and the 2870-2970 cm-l absorption bands in the infrared spectra made the method suitable for automated quality control. Procedures for the determination of volatile matter emitted from dispersed organic matter durin the analysis of pyritecontaining concentrates by thermal ecomposition were put forth by Bogorodskaya (3A). Rosenvold et al. (24A)compared differential scanning calorimetry (DSC) and nonisothermal thermogravimetry (TG) in relation to volatile matter content of coals previously analyzed by ASTM standard methods. Reliability and agreement of values for each method were discussed. Solomon (26A) studied the relation between carbon concentration and proximate analysis fixed carbon. Good agreement was obtained between measured proximate analysis values for fixed carbon and the predictions of a thermal decomposition model.
d
ULTIMATE ANALYSIS AND SULFUR FORMS Tassicker et al. (28B)determined the elemental content (C,
H. N) of coal in an on-line analvzer bv using- prompt NAA with a 252Cfsource. Kubant (14B)observed the effects of nitrogen oxides on carbon and hvdroeen analvsis in coal. Errors in the determination caused b) NO, f6rmation were corrected by use of a MnO, sorbent. A method was developed by Wystemp (34B) for determining the fate of C, H, 0, N, and S during combustion of coal, using gas chromatography. Van der Laarse and Laedrach (29B) established a microsample technique for elemental analysis of coal. Precision obtained was as good as traditional macrosample standard methods. This was accomplished by reducing the particle size of the coal sample to 85 Km or less. Carbon. Sviridenko et al. (27B) determined the carbon content of coal by means of a stepwise combustion process w d e adding an oxidizin agent in the heating area and quantitatively recording 80, in the combustion products. Sowerby (22B-24B), using a neutron and y-ray combination, developed a method for measuring the carbon content of coal. Measurements of y-ray from neutron inelastic scattering and y-ray scattering over the same sample volume were taken. Corrections for density variations and inhomogeneitiesin the 32R
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983
samples were made from the y-ray scattering measurements. Hydrogen. Gozani et al. (6B)reviewed total hydrogen content of coal determined by nuclear techniques. Hydrogen was most accurately determined by measuring the leakage of epithermal neutrons from a slab sample 30 cm thick. The average relative error was less than 1.5%. Nitrogen. A method for the rapid determination of nitrogen in coal incorporating the pyrolysis and the semimicro Kjeldahl method was presented by Nomura et al. (17B).A pulverized coal sample of 0.1 g with 1.5 g of soda lime and 2.0 g of FeC13/A1203catalyst was heated at 900-1OOO O F in a steam stream for 10 min. NHS generated was determined by conventional titration techniques. Waanders et al. (30B)evaluated procedures for determiningnitrogen in lignites. He found that digestion with concentrated HzS04in the presence of a catalyst (e.g., K2S04+ Vz05+ powdered Se) to convert the nitrogen to NH4S04,followed by distillation for 30 min in an alkaline solution and titration of the released NH3 was the most accurate and was applicable to brown coals. Oxygen. The concentration of oxygen in coal and fly ash was determined by Khalil et al. (12B)using 14-MeV instrumental NAA techniques. Preanalysis sample handling and selection of calibration standards were discussed. Sulfur. Baliza et al. (2B) developed a rapid method for the determination of sulfur in coal by oxidizing the sample in an induction furnace. The gases containing SO2 and SO3 were bubbled through a solution of H20zto form H2S04,which was determined by using Ba(C104)2in 1:l acetone. Automatic coulometry was used by Popov et al. (18B)to determine total sulfur in coal. Ignition of 1300 O F in oxygen of a 50-mg coal sample produced SO2, which was absorbed in an aqueous solution of BaCl,, HC1, and HzOz, The amount of SO2 absorbed is then determined by coulometry. Hantabal et al. (8B)determined the sulfur content of coals by titrating oxidized calorimetric bomb washings with Hg(NO& Widawska and Siess (32B)determined total sulfur in coal by XRF techniques. A method for the rapid determination of sulfur in coal for coal blending operations was developed by Baliza et al. (3B), using combustion and subsequent titration of the sulfate with Ba(CQ)?. Aleshkma and Umnyashkina (IB)determined sulfur in coal by photonephelometrictechniques. The procedure was based on the formation of BaSO,, using glycerol as the stabilizer. Grabov et al. (7B)discussed the use of BRA-9, an automated industrial analyzer for sulfur and total ash. The device tested requires a 50-g coal sample and produces an analysis in 3 min, using two X-ray sources. Klie and Sharma (13B)described a procedure for irradiation of coal samples with 14-MeV neutrons and the subsequent y-ray spectrometryof the irradiated sample for the estimation of sulfur in coal. The metrological characteristics of a coulometric rapid sulfur analyzer were studied by Ivanov and Preobrashenskii (11B).Analysis time was 3-4 min, and the error in the sulfur determination was no greater than with the conventional Eschka method. Ravaine (19B)evaluated a rapid sulfur analyzer that used infrared spectroscopy to determine the amount of SO2 liberated when the coal sample was combusted in an oxygen atmosphere. Stability, sensitivity, and detection limits for sulfur in a variety of sample types were discussed. Baur (4B) presented a review on analytical methods and analyzers for the determination of sulfur in coal. Forms of Sulfur. Simon et al. (21B) demonstrated the use of XRF spectroscopy in determining pyritic sulfur in brown coal. Hyman and Rowe (IOB) developed a method to determine pyritic sulfur in coal and lignite by combining the techniques of thermogravimetry and magnetometry and utilizing oxidizing and reducing gases. Harris et al. (9B) discussed an improved standard of petroleum pitch for use in analysis of organic sulfur in coal by an electron microprobe technique. Raymond et al. (20B) demonstrated the statistical validity of electron microprobe analysis of coal for organic sulfur. Stanton and Renton (25B) and Suhr and Given (26B) conducted pyritic iron determinations on coal according to the ASTM standard D2492-68 method to ascertain the degree
SOLID AND GASEOUS FUELS
equation from experimental data that produced a better fit for brown coal than either the Boie or the Dulong equations when predicting specific energies.
PETROGRAPHY r~
~
~~
~
~
1971. H e ~ r i c i i i dhh B.S. in~&imkby% Brooklyn Cc%m in New Ymk in I958 and his Ph.0. In 1962 a1 The Pennsyhnla State Univmtiy. He h Chlet of lhe Anatytical Suppat Section at lhe Pmsbwgh Energy Technaw Center. prior 10 lo(ning lhe US. Bureau of Mlnes. a.Schultr was engaged in indusbial research In anawcal chemistry.
of confidence and reliability of the method in determining pyritic and organic sulfur. Montano (16B) and Levinston (158) used MCasbauer spectroscopy to determine pyritic sulfur in coal. Correctiona and .. comparison with standard wet chemical methods were discussed. Giulianelli et al. (5B) and Williamson e t al. (33B) worked on using microwave dischargeactivated oxygen and M h b a u e r spectroscopy to determine the iron sulfates, iron pyrite, and total iron concentration to relate these to sulfate sulfur. pyritic .. sulfur, and total sulfur in coal. White and Lee (31B) identified elemental sulfur and thiophenic compounds in a coal extract with gas chromatopraphy and a sulfur-specific flame photometric detector.
CALORIC VALUE Jain and Sunderarajan (30developed a method for calculating the calorific value of coal from its chemical composition based on the concept that a rectilinear relation exists between the beats of reaction and the total oxidizing or reducing valences of the mixture of fuel and oxidizer. Tarjan (6C) calculated calorific value of lignites based on their ash contents. Mason and Gandhi ( 5 0 developed a new five-term formula for calculating the heating value of coal from its C, H, S, and ash content. By use of regression analysis, the standard deviation between the calculated value and the observed value was less than that observed with the Dulong, Boie, Grummel-Davis,and Matt-Spooner formulas. Benson and Schobert ( I C ) used thermal analysis techniques, specifically, pressure differential scanning calorimetry (PDSC), to determine the heating value of coals. Dubik et al. (2C) established a correlation between the carbon content of coal and its calorific value. The carbon content was used to calculate the theoretical calorific valuea of various coal. King et al. ( 4 0 derived a multiple regression
A review with five references on coal petrography and composition in relation to coal liquefaction was presented by Schweighardt (ISD). Roades e t al. (14D) reviewed 21 references on the application of microscopic techniques in the evaluation of coal, coke, and related products. Hoover and Davis (8D)developed and evaluated an automated reflectance microscope system for the petrographic characterization of bituminous coal. Quantification of size, shape, and composition in coal fine particle processing using optical microscopy and scanning electron microscopy was described by Willard (ZZD). The methodology and procedural difficulties associated with the microanalysis of coal were also discussed. The size and distribution of pores and the size, distribution, and identity of minerals in coal were determined by Harris and Yust (6D) wing transmission electron microscopy and analytical electron microscopy. Study of the structure in a coking coal vitrinite was examined by Marsh and Crawford (110) using highresolution phase contrast electron microscopy. Analysis of fringe images confirmed directly the size of crystallites predicted by X-ray diffraction studies. Sanner and Meteney (16D)evaluated an optical microscope method for pyritelmarcasite differentiation in coal. The distribution and nature of CI and Na in coal were investigated by Saunders (170)on bulk coal seam samples. using a combination of optical microscopy, SEM, and X-ray microanalysis techniques. Microanalysis of the individual maceral groups was discussed. Methods for determining coal rank, type, and grade hy light microscopy, reflectivity,electron microscopy, NMR, and Fourier-transform IR were discussed by Vleeskens (210). Bubnovskaya et al. (ID)perfected a spectmsmpic p y d u r e for coal samples to study the effect of coal metamorphism on its content of CH, CO, COC, N, and S groups, using multiple perturbed total internal reflection spectroscopy. Crelling and Dutcher ( 3 0 ) used fluorescence analyses to observe maceral composition of selected coals. Thermal analysis of petrographic lithotypes in lignites were performed by Ruscbev and Stneva (15D) using DTA, thermogravimetric, IR, and ESR techniques. Geochemical investigation of 121 coal samples from a single seam for 15 trace elements by using instrumental NAA was performed by Hart et al. ( 7 0 ) in an effort to determine lateral and vertical distribution across the seam. Carbon-13 nuclear magnetic resonance characterization of coal macer& by magic-angle spinning was reported by Marciel et al. (100). The application of coal petrography to.the evaluation of magnetically separated dry crushed coal was discussed by Harris and Hise (50). Coal petrography in combination with SEM and X-ray diffractometry was used to characterize the magnetically separated coal fractions. The petrographic evaluation of pyrite reduction in the prcduds from the DOE two-stage coal pyrite flotation proeess was presented by Tomich and Moses ( 2 0 0 ) . The effects of added Al,Os on the sintering and pyrolysis of coals of different petrographic types were discussed by Tamplon (190). Reduced permeability to gases, suppressed evolution of volatiles, and increased viscosity, strength, and yield of coke were the observed effects of these additions. Neoh et al. (120) observed the relationship of preignition volatile yields as related to coal rank, maceral content, caloric value, and particle size. Pearson and Creaney (130) calculated the degree of oxidation of a coking coal by measuring the initial and terminal reflectance values of vitrinite. Petrology of selected coals (maceral analysis and reflectance values) was used by Childs et al. (20) to determine the coking potential of those coals. Dobronravov et al. ( 4 0 ) used the international clinkering and cokeability indexes of various coal types and correlated them with the thickness of the plastic layer on the surface of the coal during coking. This thickness was then correlated with mal expansion during coking and its vitrinite and liptinite contents. ANALYTICAL CHEMISTRY, VOL. 55, NO. 5. APRIL 1983
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Le Maitre (9D)wrote a computer program to solve generalized petrological mixing model problems for coking coals and coal blending.
COKING PROCESS AND COKE TESTING Present practices for coke quality evaluation, including sampling techniques, were discussed by Hara et al. (16E). Mills and Belcher (25E)reviewed 140 references on the use of atomic spectroscopy in the analysis of coke, coal, ash, and mineral matter. Chemical, physical, and technological methods for sample preparation and testing of coke were reviewed by Scholz (31E). Kilsby (21E)reviewed 25 references on the analysis of coke, metallurgical coke, and coke-oven byproducts. Durate (IOE)examined the application of petrographic analysis of coal to determine coking properties. The effects of time and temperature on the calorific value of coal carbonization products (coke) were studied by Postrzednik (27E). Biryukov (3E, 4E) described the accuracy of the laboratory tests for determining grindability and crushability of coke. Sulfur content in coke was reduced in a process created by Schmitt and Chauaib (30E) by using group 4- and 8B metal and metal oxide additivies with the parent coal. Cardin (9E)determined As concentration in coke by using a dry method step of low-temperature organic matter removal before wet chemical methods were applied. A microprocessor-controlled analysis system was developed by Grunenberg et al. (15E)for monitoring and evaluating the moisture and carbon content in coke. Sample preparation and analysis procedures were also discussed. The use of emission spectrometry with a glow-discharge source for routine chemical analysis of coke was reported on by the European Atomic Energy Community (1IE). Cardin (8E)calculated coke yield of coal by determining the percentage distribution of silica and aluminum. Alvarez and Escudero (1E)reported on the effect of coal ash content on identification of highly expansive coals that could damage coking ovens. Optical microscopy and SEM were used by Forrest and Marsh (12E)to determine the effects of additions of petroleum coke to coals upon the strength of resultant metallurigical cokes. Hartwell et al. (18E) investigated the effects of lowvolatile additives on the structure and strength of cokes. The British Carbonization Research Association (B.C.R.A.) (6E) studied partial gasification of coke in relation to the coke tensile strength. The application of selective chromatographic and spectrofluorimetric techniques to the separation, characterization, and analysis of polycyclic aromatic hydrocarbons in coke-oven pitch was presented by the B.C.R.A. (7E). A fluidity index, indicative of the softening-melting characteristics of coal mixtures for coking, was discussed by Kawasaki (20E). A temperature-pro rammed oxidation technique to characterize coke on agecf catalysts was developed by Massoth (24E). Jasienko et al. (19E) examined the structures of cokes obtained from extracts separated from preheated vitrites of coking coals. The B.C.R.A. (5E) devised a new coal sampling and preparation techniaue to studv the effect of coking on CO and OH groups of coafthrough fR spectroscopy. Koba et al. (22E) related the effects of carbonization pressure on optical texture and porosity of cokes. Patrick (26E) discussed preheating of cokes to reduce pore size and increase the pore number for the purpose of quality coal blending. Grint and Marsh (14E) presented laboratory investigations on the strength of cokes from blends of coal incorporating petroleum pitch. Gorpinenko et al. (13E) studied the effects of the sulfur content of cokes on their electrical resistivity, and the porosity was established. A Brabender plastograph was used by Beyer and Klose (2E) to characterize coke strength in the coal softening range. Microstructural characteristics of needle cokes were examined by Qian (28E),using X-ray diffraction spectra. Marsh and Sherlock (23E) used optical microscopy and SEM to examine coke composites from the cocarbonization of coke
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grist from coal-extract solutions and coal-tar binder. Hara and Tsuchiya (17E) developed a method for testing the disintegration property of coke during gasification. Sabela and Matysik (29E) evaluated coke for metallurgical use based on partial combustion at 21700 O F . Property heterogeneity of metallurgical coke was evaluated by using the reactivity and electric resistivity by Stuchlik (32E).
INORGANIC CONSTITUENTS Two methods of expressing the results of analyses of lowrank coal-mineral-matter free and mineral free-were discussed by Gray (19F). Roscoe (42F) developed a method for determining the applicability of classical factor analysis and target transformation factor analysis to mineral matter in coal. Determination of the sources and magnitudes of the errors associated with the analysis of mineral matter in coal was presented by Stohl (44F). The qualitative and quantitative analyses of the minerals obtained from low temperature ashing techniques were carried out by means of X-ray diffraction. Analytical methods for organically and inorganically fixed elements in coal were reviewed by the Department of Mineralogy and Coal Chemistry, Federal Republic of Germany (17F). Characterization and thermal analysis of minerals in coal and coal ash were presented by Earnest et al. (14F, 15F). Determination of elements in the ash content of coal, using annihilation radiation, was performed by Sowerby and Ngo ( 4 3 0 . The technique was based on simultaneous measurement of 0.5111 MeV annihilation radiation and Compton scattered radiation. Prompt gamma NAA using a 2s2Cf source was used for elemental analysis by Reynolds et al. ( 4 0 and compared with values obtained by using ASTM wet chemical methods. McQuaid et al. (32F) developed a high count rate, timevariant Ge(Li) spectrometer for on-line coal analysis for major ash constituents. Barker (2F) discussed the advantage of real-time, continuous determination by the prompt NAA for major inorganic elements, e.g., Si, Al, Ca, Fe, Na, and K. The concentrations of Ca, Fe, Sr, Si, C, and S were determined in five borehole brown coal samples by Leonhardt et al. (28F) using NAA, y-ray activation analysis, and X-ray techniques. Various correlation functions were discussed. Multielement characterization of coal was attained by Wilde and Herzog (47F) using neutron-induced X-ray spectrometry from a 252Cfneutron source. On-line analysis of coal was possible in 10-15 min. X-ray fluorescence with Compton scattering for the determination of major inorganic elements of coal ash was presented by Pondey et al. (39F). Varying degrees of correlation were obtained between the values of ash constituents determined by conventional methods and those calculated from X-ray data. Cahill et al. (8F) conducted extensive comparisons between NAA and other analytical techniques for the determination of metallic elements in coal. Bettinelli (3F) analyzed coal ash for inorganic constituents by AAS. Preparation of samples was by lithium tetraborate fusion. Toxic chemical elements in coal fly ash were determined by Zhang (50F) using AAS. Semiquantitative ESCA examination of coal and coal ash surfaces for inorganic constituents was explored by Brown et al. (6F). A method was developed by Moza et al. (36F) to analyze the inorganic elements of individual coal grains by scanning electron microscopy. Mahoney et al. (30F, 31fl compared the general methods for the determination of phosphorus in coal and coke. The relationship between the P content of a coal and its corresponding coke was also studied. Two variants of the British standard method-the German standard method and the rapid oxygen flask method-were compared in detail. Banerjee et al. (IF) discussed a rapid method for estimating the phosphorus in coal ash by using extraction with aqueous HN03 containing NH4N03and then precipitation of phosphomolybdate. Lustigova et al. (29F)evaluated the accuracy of conventional gravimetric phosphomolybdate methods for the analysis of phosphorus in coal. A spectrophotometric method was developed to determine the phosphorus as a vanadate-molybdate-phosphate complex.
SOLID AND GASEOUS FlJELS
Mitsubishi (35F) determined the C1 and F in coal through a multistep procedure: (1) convert the C1 and F to HC1 and HF by combustion in the presence of a moist oxygen stream, (2) absorb the HCl and HF in aqueous alkali, and (3) determine the C1 and F colorimetrically. Kler (22F) discussed the relationship between potassium and sodium concentrations in coal and coal ash. Trace Elements. Investigation of coal samples for trace elements by thermal and epithermal NAA was proposed by Kostadiiiov and Djingova (24F). Trace elements in coal, coal ash, and fly ash produce short-lived nuclides that may be determined, together with some of the matrix elements, by NAA, according to Boeck et al. (43‘). An NBS coal SRM was irradiated with thermal neutrons for 12 h by Chu et al. (12F) and Suzuki et al. (45F) to obtain a y-ray spectrum for the determination of over 30 trace elements. Galantanu and Engelmann (18F)used photonuclear activation and highresolution y-spectrometry in a Bremsstrahlung beam to nondestructively determine trace elements in coal, Repeatability and reproducibility of the determination of trace elements in coal by AAS were discussed by Ihida et al. (20F). Bosshart et al. (5F) described various analyses;and test methods used by industrial laboratories to determine trace elements. AAS was the basic method selected because of sensitivity, selectivity, accuracy, precision, practicabiility, and economy. Laktionova and Egorav (25F) determined trace elements in coal by spectrophotometric methods. Combustion of a mixture of coal with a buffer substance prepared from powdered coal and a stabilizer (NaC1) additive was the means employed. Multielement proton activation analysis was carried out by Ledingham et al. (27F) on coal and cod ash with a Compton suppressed Ge(Li) detector. Nichols and D’Auria (38F) used energy dispersive XRF in an attemDt to differentiate between coal sDecimens of various seams arid locations based on trace element concentrations. Statistical analysis showed successful differentiation between samples from different seams was 80%, while between samples from different locations successful differentiation was 93%. Mills et al. (33F) reported on the use of wavelength-dispersive XRF with matrix correction, using Compton scattering radiation to determine trace elements. Volatile trace metals in coal were determined by Wilkinson et al. employing various atomic spectroscopic techniques e.g., cold-vapor atomic fluorescence (AFS), AAS, and inductively coupled plasma (ICP). Nodkarni (37F) combusted coal in an oxygen bomb and then analyzed the residues for various dements by using AAS, AFS, ICP, ion selective electrode, and chemiluminescence. Klose et al. ( 2 3 9 determined volatile trace elements in coal by volumetric methods and compared results with standard gravimetric analysis. Spark source mass spectroscopy for trace element determination in coal and fly ash was discussed by Jacolbs (21F) in relation to the usefulness of the analytical resulta for environmental pollution surveys. Chen et al. (IIF), Bujok et al. (7F),and Minkin et al. (34F) discussed proton-induced X-ray emission (PIXE) analysis and electron microprobe techniques for use in trace dement analysis of coal and coal ash. Svendsen et al. (46F)combined Rutherford backscattering (RBS) and PIXE analysis to determine trace elements in power plant ash samples. Casella et al. (9F) presented a procedure for the cletermination of uranium, thorium, and lead in coal and coal ash by anion exchange chromatography. Rigin (41F),Doolan (13F), and Ebdon et al. (163’)determined mercury in coal by nonoxidative pyrolysis and subsequent cold-vapor AFS. Castillo et al. (10F)described a procedure for the determination of germanium in coal and coal ash by hydride generation and flame AAS. Lebedev (263’)used an X-ray radiometric method to determine germanium, A simplified method was proposed by Xu et al. (49F)for determining gallium in coal with Rhodamine B. With 10 ppm gallium, the possible error in the determination is *lo%.
Lustigova (3G) evaluated the fusibility of ash temperatures under different conditions, i.e., reducing, semireducing, and oxidizing atmospheres. Edwards et al. (2G)assessed the standard method of testing for the grindability of coal by the Hardgrove machine. Painter et al. (GG),applied Fourier transform IR spectroscopy to the quantitative determination of mineral matter in coal, using least-squares curve fitting. Miknis et al. (4G) used a 13CNMR combination of cross polarization and magic-angle spinning techniques to deterrnine the aromatic-aliphatic character of coals, coke, and solid solvent-refined coal. Stadelhofer et al. (7G) reviewed recent applications of nuclear magnetic resonance spectroscopy to coal and coal-derived product analysis. A report by Williams (8G) summarized techniques used for determining the mineral content in fossil fuels. The qualitative and quantitative X-ray minerological system discussed was semiautomated and computer controlled. Neavel et al. (5G) assembled a data library to be used to define interrelations between coal properties. Coal characterization research involved sample selection, meticullous preparation, and reduction of analysis data to the mineralmatter-free basis.
MISCELLANEOUS
Gas chromatography continues to be a widely used technique for the analysis of gaseous fuels and related materials. The field of gas chromatography was reviewed extensively by Risby et al. ( 6 4 in the 1982 Analytical Reviews. This review
Bornhop et al. (1G) used tritiated water to determine the quantity of exchangeable water in coal and coal chars.
STANDARD METHODS ASTM (1H)coordinates the development and standardization for test procedures for coal and coke through the D-5 committee. Standards that were adopted, revised, or reapproved during the period covered by this review include the following: D 197-82,Sampling and Fineness Test of Pulverized Coal; D 388-82, Classification of Coals by Rank; D 1857-68 (1980), Test for Fusibility of Coal and Coke Ash; D 2639-74 (1980), Test for Plastic Properties of Coal by the ConstantTorque Gieseler Plastometer; D 2796-81, Definition of Terms Used for the Megascopic Description of Coal and Coal Beds and for Microscopical Description and Analysis of Coat D 317-82, Test for Ash in the Analysis Sample of Coal and Coke from Coal; D 3177-75 (1982), Test for Total Sulfur in the Analysis Sample of Coal and Coke; D 3302-82, Test for Total Moisture in Coal; D 3402-81, Tumbler Test for Coke; E 11-81, Specifications for Wire-Cloth Sieves for Testing Purposes; E 323-80, Specifications for Perforated-Plate Sieves for Testing Purposes.
GASEOUS FUELS This review surveys publications concerned with methods for chemical, physical, and instrumental analyses of gaseous fuels and related materials. Articles of significance appearing in foreign journals and the patent literature not available at the time of the last review are also included. Chemical .4bstracts and Energy Research Abstracts were used extensively as reference sources. Some selectivity was necessary to include the most pertinent publications in preparing this review.
GENERAL REVIEWS Analytical methods for natural gas, refinery gas, tmd manufactured gases were included in a review by Terrell(121). The use of gas chromatography in the analysis of natural gas was reviewed by Campo ( 2 0 . Kostrzewski and Koralewski (7I) reviewed the analysis of fuel gases and combustion products. Natural gas and liquefied natural gas characterization by experimental and computational methods was reviewed by Roncier and Nicaud (SI). Dumay (41) reviewed the application of analytical methods in the gas industry. Natural gas measurements were reviewed by McEntire (81) and also by Goodenough (51). Scott and Fetzer (101) reviewed the use of manometers in the gas industry. Various methods for measuring the calorific values of natural gas were reviewed by Harris (SI)and Curry (31). Boschan (10 reviewed methods for determining the sulfur content in natural gas, and Vlckova (121)reviewed the analysis of sulfur compounds in heating gases.
GAS CHROMATOGRAPHY
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983
35 R
SOLID AND GASEOUS FUELS
covers only those publications directly related to gaseous fuels. Bjarnov ( 2 4 determined the chemical composition of natural gas by gas chromatography using three separate columns. This information was used to estimate the heating value, Wobbe index, and com ressibility, and to calculate the amount of energy deliverex to the distribution network. Nesmelova et al. (54 gave procedural recommendations for natural fuel gas chromatographic analysis. Tkachenko et al. ( 9 4 determined the molar correction coefficients for the “Tsvet-1-64” chromatograph in the identification of natural gas hydrocarbon. Trifachev and Osipova (IO4 reported the chromatographic determination of argon, hydrogen, and oxygen in natural gas. A thermal conductivity detector was used, and separation was accomplished at -21” using 3-mm columns packed with CaX zeolites. Gases from coking were analyzed by Kvasova et al. ( 4 4 using two 3-mm chromatographic columns. The first was packed with NaX molecular sieve and the second with silica gel containing 1.5% petrolatum. The columns were operated in series for determining H, 0, N, CH4, and CO, and the first column was used alone for determining CzH2,C2H4,CzH6, C3H6,and C3Hs. Butina et al. ( 3 4 analyzed coke-oven gas by absorbing C02 on NaX molecular sieve prior to gas chromatography, using a thermal conductivity detector. The chemical constituents (CzHz,C2H4,CzH6, etc.) of a multiconstituent gas such as LPG and coke-oven gas were rapidly determined by Kansai Coke and Chemicals Co., Ltd. (14, using a gas-flow circuit system capable of simultaneously separating constituents. Carrier gas is mixed with the gas, and the mixture is passed through a series of columns packed with SiOz and molecular sieves. Strashilina ( 8 4 used two columns for the analysis of gases from the steam conversion of hydrocarbons. Individual Cz;Cs hydrocarbons and C02were analyzed on a column filled with Spherochrome 1containing 15% triethylene glycol butyrate; and 0, N, CH ,and CO were analyzed on a column filled with zeolite 13X. %, quick, reliable, and low-cost Carle on-stream gas chromatograph was used by Sood and Pannell(74 for the characterization of product gas from coal liquefaction. Zabranska et al. ( 2 1 4 analyzed biogas for CH4, COz, and (N 0) on Separon AE, and for 0 and N on molecular sieve 5A. Examples of chromatographs were given.
+
SULFUR COMPOUNDS The sulfur content in a fuel gas was determined photoelectrically by the Osaka Gas Co., Ltd. ( I K ,Z K ) . Samples were burned in a hydrogen flame, and the sulfur content was measured from the differential values of photoelectric currents at 390 and 500 nm. Moen ( I O K ) determined total sulfur and hydrogen sulfide in natural gas by using electrolytically generated bromine and a coulometric Br-sensing electrode for continuous sulfur monitoring. A fast-response UV absorption photometric analyzer was reported by Babiuk ( 4 K ) for hydrogen sulfide measurement and control in natural gas pipelines. Straka (I1K) demonstrated the continuous determination of hydrogen sulfide in natural gas and coking gas with an iodide-selective electrode following the reaction with potassium iodate in an alkaline medium. Hydrogen sulfide and other sulfur compounds in natural gas were determined by Zaripov et al. ( I Z K ) using gas chromatographic separation. Garai et al. (7K) determined the odorant ethanethiol in natural gas by absorbing in a silver nitrate solution, precipitating excess silver ions with potassium iodide, and coulometrically back-titrating the excess iodide ions with an iodide-selective electrode. The determination of mercaptans in natural gas through absorption and iodometric titration was reported by the Szechwan Institute of Chemistry (3K). Garai et al. (6K) used electroanalytical methods and selective precipitation for the simultaneous determination of hydrogen sulfide and the odorants tetrahydrothiophene and volatile thiols in natural gas. Gas chromatographic methods and selective chemical reactions were used by Liu and Luo (9K) for the qualitative and quantitative analysis of organic sulfur compounds in natural gas. Thiols in liquefied gas were first absorbed and then liberated for gas chromatographic/mass spectrometric identification by Zygmunt and Staszewski (13K). Balini (5K) described an electrochemical cell for measuring the mercaptan content of fuel gases. Derivatization and liquid chromatog36R
ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983
raphy were employed by Kuwata et al. (8K) to analyze domestic fuel gas for alkylthiols.
WATER VAPOR The determination of water vapor in natural gas was reviewed by Dodds (4L) and by Chandler (2L). Robinson et al. (6L) reviewed the estimation of the water content of sour natural gas. The best applications for basic methods of water vapor determination in natural gas were discussed by Dodds (3L). Bozeman ( I L )described a titration method for the continuous determination of the moisture content in natural gas. The titration equipment was also described. The titrimetric determination of moisture in liquefied natural gas was given by Shkol’nikova et al. (7L). Lee et al. (5L) used a piezoelectric crystal detector for evaluating the water content of town gas and liquefied petroleum gas. Results are compared to absorption-gravimetry. The water dew point in natural gas was monitored by Waldschmidt (8L)using specially pretreated aluminum oxide sensors.
CONDENSATES Branisova (1M) discussed the sampling and analysis of natural gas condensates. A liquid chromatographic method of gas condensate analysis was described by Kabulov et al. (3M). Gas-liquid chromatography was used by Koksharova et al. (4M) to analyze gas condensates. Methods for characterization of knockout-pot condensates from underground gasification were reported by Craven et al. (2M). Lunskii (5M) reported a rapid gas chromatographic determination for the naphtha fraction in natural gas.
CALORIMETRY Williams ( I I N ) described highly accurate instrumentation and measurement techniques useful in custody transfer for calculating the calorific value of liquefied natural gas and liquefied petroleum gas. Springer et al. (6N) reported an automated chromatograph for the Btu measurement of natural gas for custody transfer, while water vapor was accounted for by Curry ( I N ) in calculating the Btu content of natural gas. An on-line gas chromatographic system was described by Villalobos (9N) that produced 24-h averages of fuel gas Btu, specific gravity, and Wobbe index. Howard (2N) described the Therm-Titrator, which measures the calorific value of natural gas from the air to gas ratio at maximum adiabatic flame temperature. The amount of oxygen for stoichiometric combustion was used by Kude et al. (3N) for determining the heating value of gaseous fuels. Stoichiometry was maintained by the electrochemical sensing of combustion products. New methods for determining the heating value of natural gas were reviewed by Van Rossum and Benes (8N), while Watson and White ( I O N ) reported the use of acoustic measurement for the Btu content of natural gas. Maeda (4N,5N) described a calorimetric apparatus for fuel gases in which oxidation of the fuel gas and a combustion gas is carried out in the presence of a catalytic oxidizer. Szonntagh (7N) described a calorific content analyzer that measures the temperature of a metal cup heated by burning a combustible gas in an excess supply of air.
DENSITY AND SPECIFIC GRAVITY Hankinson et al. ( I P )calculated accurate liquefied natural gas densities for custody transfer with a fine-tuned version of “Costald”. Provisions for the presence of H2S, COZ, and nitrogen were considered by Rozentsvaig and Grevtsov (5P) in calculating the density and kinematic viscosity of natural gas-petroleum mixtures flowing through pipelines. Siegwarth and LaBrecque (7P) described a portable densimeter used to calibrate liquefied natural gas densimeters. A gas chromatographic system to determine density and composition of C1-Cs hydrocarbon mixtures was reported by Rybalkin et al. (6P). Liquid densities of ethane-propane mixtures were measured by Parrish et al. (4P) as a function of composition and pressure up to 1400 psi. Instruments for measuring the specific gravity of gas were reviewed by Kahmann (2P),while TerBush (8P) reviewed
SOLID AND GASEOUS FUELS
specific gravity instruments and gas sampling devices. Kinetic gas gravitometers were tested on air alone by Lewis (32').
Rate Method); and D4150-82, Terminology Relating to Gaseous Fuels.
SAMPLING
LITERATURE CITED
Techniques of natural gas sampling were reviewed by Phillips (5Q)and by Drake (3Q),while Welker ( 8 6 ) reviewed the sampling of natural gas liquids. Natural gas sampling with the Gas Processor Association separator was described by Scheperri et al. (6Q). Astrynnin (12')reported temperature regulation with a sampling device with a protective shell through which the natural gas to be sampled is first allowed to flow. The rapid sampling of gas products in coke plants and gas works for gas chromatographic analysis was described by Stepanek et al. (7Q). Wlelsch et al. (9Q) sampled natural gases for gas chromatographic analysis of high-boiling hydrocarbons. Particulate sampling of low Btu coal gas was described by Neulander et al. (4Q)and by Carpenter et al. (2Q).
MISCELLANEOUS The use of computers in natural gas measurement systems was described by Keady (9R)and Williamson (19R). A computer program by Lloyd (I1R)aided in monitoring wet gas field quality. The use of mass measurement for natural gas liquids was discussed by Caffey (2R)and Tilley (18R).Sallet and Wu (17R) discussed the use of the thermodynamic properties of several liquefied petroleum gases in predicting mass flow rates. The enthalpies of mixtures of dater vapor and sweet natural gas were determined experimentally by Eubank et al. (6R). Equations were given by Nersesova (I5R)that are useful in determining the enthalpy of natural gas. The viscosity of saturated and compressed liquid propane was meariured by Diller (3R) and compared to calculated values. Erickson et al. (5R)analyzed coal gas with Fourier-transform infrared spectrometry to quantify COS and NH[3and to identify other compounds. Laser-induced breakdown spectroscopy was applied to the detection of sodium and potassium in a coal p i f i e r stream by Loree and Radziemski (12R). Haas et al. (8R)described the monitoring of alkali and trace heavy metals in low-Btu coal gasification streams. The protection of an analyzer for determining the oxygen content in gasification mixtures was reported by Meyer et al. (13R). Kipka (IOR)measured dust and tar in a pressurized coal gasification stream by capture on a glass wool-asbestos filter. Analytical data for 310 natural gas samples in 16 states were referenced by Moore (14R). Fleischmann (7R)absorbed the mercury iin town gas in silver amalgam prior to analysis. The feasibility of using Raman spectrometry for determining natural gas composition was explored by Diller and Chang (4R). A gas radiospectrometer was used by Abdurakhmanov et al. ( I R )to determine methanol in natural and petroleum gases. Liquefied natural gas gels were characterized by Reid et al. (16R).
STANDARDS A standard sampling procedure for determining the water vapor content of natural gas was described by Curry (2s). Nagakura (4s)discussed the standardization of constants used to calculate the specific gravity and calorific value of gaseous fuels. A relative Wobbe index was proposed by Heike ( 3 s ) as a standard index for a wide range of fuel gases. The A8TM develops and standardizes procedures for the analysis of gaseous fuels. These standards ( I S )are published annually. ASTM standards that have been adopted or revised during this review period include the following: D1072-80, Test for Total Sulfur in Fuel Gases; 111145-80, Sampling Natural Gas; D1247-80, Sampling Manufactured Gas; D1266-80, Test for Sulfur in Petroleum Products (Lamp Method); D1945-81, Analysis of Natural Gas by Gas Chromatography; D1837-81, Test for Volatility of Liquefied Petroleum (ILP) Gases; D1946-82, Analysis of Reformed Gas by Gas Chromatography; D2420-81, Test for Hydrogen Sulfide in Liquefied Petroleum (LP) Gases (Lead Acetate Method); D3031-81, Test for Total Sulfur in Natural Gas b Hydrogenation; D3588-81, Calculating Calorific Value andY!3pecific Gravity (Relative Density) of Gaseous Fuels; D3956-82, Methane 'l'hermophysical Property Tables; D4084-81, Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction
SOLID FUELS
Sampllng and Proximate Analysis (1A) Aithapp, Anton; Born, Manfred; Klose, Erhard; Stoeffgen, Fritz Frelblerg. Forshungsh. A 1980, A 625, 69-81 (Ger). (2A) Bartnik, Dleter Neue Bergbautech 1981, 7 7 (4), 247-9 (Ger). (3A) Bogorodskaya, L. I.Geol. Geofiz. 1982, (4), 51-8 (Russ). (4A) Brown, D. R.; Gozanl, T.; Elias, E.; Bozorgmanesh, H.; Bevan, R.; Luckie, P. Report 1980, EPRI-CS-989 (Vol. 4), 60 pp (Eng). (5A) Cardillo, P. Rlv. Combust. 1986, 34 (4-5), 129-37 (Itai). (6A) Cumming, John W. Proc. Eur. Symp. Therm. Anal. 1981, 2nd, 512-16 (Eng). (7A) Earnest, Charles M.; Fyans, Richard L. Perkin-Elmer Therm. Anal. Appl. Study 1981, 32, 8 pp (Eng). (8A) Ghetti, P. Rlv. Combust. 1980, 34 (9-12), 403-9 (Ital). (9A) Gozani, T.; Elias, E.; Bevan, R. Report 1980, EPRI-CS-989 (Vol. €I) 43 PP (E%). (10A) Graham, R. D. J. Coal Qual. 1982, 7 (3), 7-9 (Eng). (11A) Hicks, Donald G.; O'Relliy, James E.; Koppenaal, David W. Prepr. Dlv. Fuel Chem., Am. Chem. Soc., 1980, 25 (3), 288-34 (Eng). 112A) Hlcks. Donald G.: O'Relilv, James E.; Kouuenaal, David W. Fuel 1982, .. 61 (2), 150-4 (Eng). (13A) Janczyszyn, Jerzy; Stochalskl, Aieksander J. Anal. Chlm. Acta 1982, 738, 199-205 (Eng). (14A) Jenke, Dennis R.; Hannlfan, Martin R. Anal. Chem. 1982, 54 (4), 843-5 (Eng). (15A) Kawatetsu Chemical Industry Go., Ltd. Jpn. Kokal Tokkyo Koho JP 82 42,837 10 Mar 1982, Appl. 80/117,735, 28 Aug 1980; 3 pp. (16A) Kawatra, S. K. Fine Part. Process., Proc. I n t . Symp. 198C1, 1, 583-93 (Eng). (17A) Konovalov, L. N.; Lukina, N. S.(USSR). Soversh. Tekhnol. Stredstu Ugleobogashch. 1980, 98-102 (Russ). (18A) Kramue, Geza Hung. - Teijes . 19, 28 Nov 1980, App. . . 77lBA3603, 05 . Dec 1977; 15 pp. (19A) Niac, G.; Enache, C.; Anghel, V.; Mllltan. P. Mine, Pet. Gase 1980, 31 110). 473-8 - - IRom). (20A) Nlr-El, Y.; Director, B.; Gozanl, T.; Bernatowlcz, H.; Elias, E.; Brown. D.; Bozorgmanesh, H. At. Nucl. Methods FossllEnergy Res. 7980 1982, 151-4 (Eng). (21A) Onlshchenko. A. M.; Belonozhko, V. P. Fiz. Tekh. Probl. Razaab. Polezn. Iskop 1982, (I), 90-6 (Russ). (22A) Ottaway, Martyn Fuel 1982, 61 (8), 713-16 (Eng). (23A) Page, Dannis; Fox, Edward James Brit. UK Pat. Appl. 2,056,660 18 Mar 1981, Appl. 80/21,218, 07 Aug 1979; 7 pp. (24A) Rosenvold, R. J.; Dubow, J. B.; Rajeshwar, K. Thermochlm. Acta 1982, 53 (3), 321-32 (Eng). (25A) Scholz, A. Aufbereit .-Tech. 1981, 22 (12), 647-54 (Eng/Ger). (26A) Solomon, Peter R. Fuel 1981, 60 (I), 3-6 (Eng). (27A) Sowerby, Brian David Brit. UK Pat. Appi. GB 2,065,876, 01 Jul 1981, AU Appl. 7911,797, 20 Dec 1979; 12 pp. (28A) Starchlk, L. P.: Borushko. N. I.; Krylov. R. A. Zavod. Lab. 1982, 48 (3), 31-3 (Russ). (29A) Starchik, L. P.; Ryashchikov, V. I.Zavod. Lab. 1982, 48 (4), 48-9 (Russ). (30A) Starchik, L P.; Onishchenko, A. M.; Belonozhko, V. P. Koks Khim. 1982, (e), 10-13 (Russ). (31A) Sumitomo Metal Industries, Ltd. Jed K. K. Jpn. Tokkyo Koho JP 82 05,456, 30 Jan 1982, Appi. 77/92,113, 29 Jul 1977; 5 pp. (32A) Watt, John Stanley; Gravitis, Vilis Leonlds Brit. UK Pat. Appl. GB 2,073,884, 21 Oct 1981, AU App. 8013,079, 10 Apr 1980 10 pp. ( 3 3 4 Watt, John Stanley; Gookes, Reginald Arthur; Gravltis, Viiis Leonids Ger. Offen. 3,023,453, 22 Jan 1981, Australian Appl. 7919,308, 22 Jun 1979; 18 pp.
.
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I
Ultlrnate Analyels and Sulfur Forms ( l e ) Aleshkina, T. S.; Urnnyashklna, L. M. Kim. Prom-st., Ser.: MePody Anal. Kontrolya Kach. Prod. Khim. from-sfi 1980, (12), 43-5 (Russ). (28) Baliza, Sebastiao Vitro; Soledade Lulz Edmundo Bastos; Cavalccmti, Manoel Arthur Metalurgla (Sa0 Paulo) 1982, 38 (292) 133-6 (Port). (38) Baliza, Sebastiao Vitro; Soledade, Luiz Edmundo Bastos; Cavalcanti, Manoel Arthur Congr. Anu, ABM 1981, 36th (3), 233-46 (Port). (48) Baur, Paul S. Power 1982, 126 (7), 73-5 (Eng). (58) Giullanelli, James L.; Wllllamson, D. L. At. Nucl. Methods Fossil Energy Res., 7980 1882, 443-58 (Eng). (6B) Gozanl, T.; Elias, E.; Bozorgmanesh, H. Report 1980, EPRI-CS-989(voL 3), 26 PP. (78) Grabov, P. I.; Mikhallov, G. I.;Potapov, A. 8.; Starchik, L. P.; Ivashchenko, G. A. Koks Khim. 1981, (a), 39-40 (Russ). (8B) Hantabal, Eugen; Javorkova, Magda; Slenc, Vladimir Czech. CS 209,326, 30 Nov 1981, Appl. 79/2,189, 31 Mar 1979; 3 pp. (9B) Harris, L. A.; Raymond, R., Jr.; Gooley, R. Proc., Annu. Conf. Microbeam Anal. SOC. 1980, 15th, 147-8 (Eng). ( l o g Hyman, M.; Rowe, M. W. ACS Symp. Ser. 1981, No. 769 (New Approaches Coal Chem.), 389-400 (Eng). (1 IB) Ivanov, Yu. A.; Preobrazhenskil, V. P. Teploenergetlka (Moscow) 1981, (5), 70-2 (Russ). (12B) Khalil, S. R.; Koppenaal. D. W.; Ehmann, W. D. Anal. Left. 1980, 73 (A12), 1063-71 (Eng). (138) Klie, J. H.; Sharrna, H. D. J. Radioanal. Chem. 1982, 77 (1.-2), 299-309 (Eng). ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983
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SOLID AND GASEOUS FUELS (148) Kubant, Josef Sb. Pr. UVP 1981, 41, 69-84 (Czech). (158) Levinson, Lionel M. A I P Conf. Proc. 1981, 70 (Chem. Phys. Coal UtiL 1980), 209-34 (Eng). (I6B) Montano. Pedro A. Prepr. Pap.-Am. Chem. SOC., Div. Fuel Chem. 1979, 24 (I), 218-29 (Eng). (178) Nomura, Akira; Morlta, Yazaemon; Kogure, Yukitoshi Nenryo KyokaiShl 1980, 59 (638), 377-81 (Japan). (18B) Popov, V. A.; Andronova, N. 1.; Tikhonov, I. A.; Pichugin, V. V. Koks Khlm. 1981, (12), 17-20 (Russ). (19B) Ravaine, D. Rev. Metall. 1980, 77 (8-9), 725-39 (Fr). (208) Raymond, R., Jr.; Davies, T. D.; Hagan, R. C. Proc. Annu. Conf.-MIcrobeam Anal. SOC. 1980, 15th, 149-50 (Eng). (218) Simon, Liboslav; Barcalova, Llbuse; Sok, Vilem Acta Mont. 1981, 6 7 , 113-35 (Czech). (22B) Sowerby, Brian Davld Pat. Specif. (Aust.) AU 516,362, 28 May, 1981, AU Appl. 78/4,426, 18 May 1978; 27 pp. (238) Sowerby, Brian David S. African 79 03,784, 30 Jul 1980, Appl. 79/ 3,784, 24 Jul 1979; 28 pp. (24B) Sowerby, Brian David Brit. UK Pat. Appl. 2,055,191, 25 Feb 1981, Appl. 79125,871, 24 Jul 1979; 15 pp. (258) Stanton, Ronald W.; Renton, John J. Clrc. Ser.-W. Va ., Geol. €con. Surv. 1981, (2-22, 1-22 (Eng). (26B) Suhr, N.; Given, Peter H. Fuel 1981, 60 (e), 541-2 (Eng). (27B) Svirldenko, Zh. V.; Orzhekhovskaya, A. I.;Sidenko, E. A,; Shegeda, V. B. U.S.S.R. SU 893,862, 30 Dec 1981, App. 2,914,937, 25 Apr 1980. Otkryllya, Izobret., Prom. Obrazfsy, Tovarnye Znaki 1981, (48), 116-17. (288) Tassicker, Owen J.; McConnell, James F. Proc.-Conf. Alr Qual. Management Electr. Power Ind., 2nd 1980, 2 , 1129-48 (Eng). (298) Van der Laarse, J. D.; Laedrach, W. Mlkrochim. Acta 1981, 1 (3-4), 309-16 (Eng). (308) Waanders, J.; Wail, T. F.; Roberts, J. Chem. Aust. 1980, 47 (7), 274-5 (Eng). (318) White, C. M.; Lee, M. L. Geochlm. Cosmochlm. Acta 1980, 44, 1825-32 (Eng). (328) Wldawska-Kusmierska, Janina; Siess, Krystian Zesz Nauk. Polltech. Slask., Gorn. 1979, 102,33-45 (Pol). (338) Wllllamson, D. L.; Guettinger, T. W.; Dickerhoof, D. W. Adv. Chem. Ser. 1981, No. 194, 177-208 (Eng). (348) Wystemp, Ewald (Sesz. Nauk. Polltech. Slask., Energy. 1981, 76 39-46 (Pol).
.
Calorlc Value (IC) Benson, Steven A.; Schobert, Harold H. Technol. Use Lignite 1981 1982, 1 , 442-70 (Eng). (2C) Dubik, 2. G.; Ivantsiv, 0. E.; Uzhenkov, G. A. Deposited Doc. 1979, vrNm 3434,63-73 (RUSS). (3C) Jain. SamDat R.; Sundararalan, Rajaraman Fuel 1981, 60 ( I I ) , 1079-82 (E@. (4C) King, Tom N.; Attwood, David H. Fuel 1980, 59 (8), 602-3 (Eng). (5C) Mason, D. M.; Gandhl, K. Prepr. Div. Fuel Chem., Am. Chem. SOC. 1980, 25 (3), 235-45 (Eng). (6C) Tarjan, Gusztav Banyasz. Kohasz. Lapok. Banyasz. 1981, 114 (1 I), 730-45, (Hung). Petrography (ID) Bubnovskaya, L. M.; Popov, V. K.; Rus'yanova, N. D. Koks Khlm. 1982, (5),9-13 (Russ). (2D) Chllds, Susan M.; Crelling. John C.; Dutcher, Russell R.; Gooisby, Steven M. Resour. Ser.-Colo. Geol. Surv. 1980, 55-7 (Eng). (3D) Crelllno. John C.: Dutcher, Russel R. Resour. Ser.-Colo. Geol. Surv. ' 1980. 58161 (Eng). (40) Dobronravov, V. F.; Vertikova, T. A,; Ganova, M. P. Khlm. Tverd. Topl. (MOSCOW)1982, (2),34-9 (Russ). (5D) Harrls, L. A.; Hlse, E. C. Process Mineral, Proc. Symp. 1981, 479-92 (Eng). (6D) Harris, L. A,; Yust, C. S. Adv. Chem. Ser. 1981, No. 192 (Coal Struct.), 321-36 (Eng). (7D) Hart, R. J.; Leahy, R.; Falcon, R. M. J . Radloanal. Chem. 1982, 71 (1-2). 285-97 (Eng). (8D) Hoover, D. S.; Davls A. Report 1980, FE-2030-TR23, 275 pp. (9D) Le Maltre, R. W. Comput. Geoscl. 1981, 7(3),229-47 (Eng). (10D) Maciel, Gary E.; Sullivan, Mark J.; Petrakls, Leon; Grandy, D. W. Fuel 1982, 61 (9, 411-14 (Eng). (11D) Marsh, Harry; Crawford, David Fuel 1982, 61 (9), 876-8 (Eng). (12D) Neoh, K. G.; Annamalai, K.: Gannon, R. E. Report 1981, DOE/PC/ 30290-T4. (l3D) Pearson, David E.; Creaney, Stephen Fuel 1981, 60 (3), 273-5 (Eng). (14D) Rhoades, A. H.; Gray, R. J.; Hutington, H. D. Process Mlneral., Proc. Symp. 1981, 453-78 (Eng). (15D) Ruschev, D.; Stoeva, D. Therm. Anal. 1980, 2, 437-42. (16DI Sanner. W. S.. Jr.: Metenev. D. L. ReDort 1980, DOE/PMTC/TR-I (BO), 13 pp. (Eng). (17D) Saunders, K. G. J. Inst. Energy, 1980, 53 (416), 109-15 (Eng). (18D) Schweighardt, F. K. DOESymp. Ser. 1981, 1-15 (Eng). (1%)) Tampion, V. V. Kim. Tverd. Topl. (Moscow) 1982, (2), 40-2 (Russ). (20D) Tomich, R. S.;Moses, R. S. Report 1981, DOE/PC/30134-1; 46 pp. (End. (21D) Vleeskens, J. M. Energiespectrum 1982, 6 (3), 70-9 (Neth). (22D) Willard, A. G. Fine Part. Process., Proc. Int. Symp. 1980, 1, 594-615 (Eng). Coke Process and Coke Testlng (1E) Alvarez, R.; Escudero, J. 6. fubl. INCAR 1980, 9, 12 pp (Span). (2E) Beyer, H. D.; Klose, W. ErdoelKohle, Erdgas, Pefrochem. 1981, 34 (9), 410 (Ger).
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ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983
(3E) Biryukov, Yu. V.; Nesterenko, L. L.; Yurina, L. V.; Burtsev, B. G. 23 Sep 1981, Otkryllya, Izobret., Prom. Obraztsy, Tovarnye Znaki 1981, (39, 110. (4E) Biryukov, Yu. V.; Nesterenko, L. L.: Yurlna, L. V.; Burtsev, B. G. 23 Sp 1981, Otkryllya, Izobret., Prom. Obraztsy, Tovarnye Znaki 1981, (35),
110. (5E) British Carbonization Research Asqoc. Carbonization Res. Rep. 1979, 6 4 , 23 pp (Eng). (6E) Britlsh Carbonization Research Assoc. Carbonization Res. Rep. 1981, 82,28 PP (Eng.) (7E) Brltish Carbonlzation Research Assoc. Carbonization Res. ReD. 1980, 89,25 pp (Eng.) (8E) Cardin Gonzalez, J. M. Publ. INCAR 1980, 2, 16 pp (Span). (9E) Cardln Gonzalez, J. M. Publ. INCAR 1980, 8, 11 pp (Span). (10E) Duarte, Norma Magalhaes Rev. Qulm. Ind. 1981, 50 (594), 10-13 (Part\.
(1lE< European Atomic Energy Communlty (Euratom). Report 1981, EUR71874 50 DD (Ital). (12E) Fo;rest,rMaggil Marsh, Harry Fuel 1981, 60 (5),429-33 (Eng). (13E) Gorpinenko, M. S.; Zelenlna, V. V.; Smolentseva, V. A. Khlm. Tekhno/. Top/. Masel 1981, (3), 19-21 (Russ). (14E) Grlnt, Alan; Marsh, Harry Fuel 1981, 60 (12), 1115-20 (Eng). (15E) Grunenberg, Dieter; Loose, Wilfried; Koch, Karl Heinz Stahl Elsen 1981, 101 (19), 1219-22 (Ger). (16E) Hara, Yukiaki; Mikuni, Osamu; Yamamoto, Hldeki, Yamanaka, Hiroakl McMaster Symp. Iron Steelmaklng, (Proc .) 1980, 4/1-4/38 (Eng). (17E) Hara, Yukiaki; Tsuchiya, Masaru Tetsu To Hagane 1980, 66 (13), 1810-19 (Japan). (18E) Hartweil, Richard R.; Stacey, Albert E.; Wllklnson, Herbert C. Fuel 1982, 61 (4), 329-35 (Eng). (19E) Jasienko, Stefan; Gerus-Plasecka, Irena. Fuel 1982, 61 (a), 565-9 (Eng). (20E) Kawasakl Steel Corp. 16 Dec 1981, 4 pp. (21E) Kilsby, P. E. Iron Steel Int. 1980, 53 (4), 185, 187-9 (Eng). (22E) Koba, Kelichlro; Sakata, KojI, Ida, Shlro Fuel 1981, 60 (6), 499-506 (En@. (23E) Marsh, Harry: Sherlock, Janet Fuel 1981, 60 (5),434-8 (Eng). (24E) Massoth, F. E. Fuel Process. Technol. 1981, 4 (I), 63-71 (Eng). (25E) Milis. J. C.: Beicher. C. B. Proa. Anal. At. SDectrosc. 1981. 4 (1-2), 49-80 (Eng). (26E) Patrick, J. W. Comm. Eur. Communltles, (Rep.) EUR 1981, EUR 7797, 213-47 (Eng). (27E) Pstrzednik, Stefan Z e s z . Nauk. Polltech. Slask., Energy. 1981, 7 6 , 5-14 (Pol). (28E) Qian, Shaun; Song, Xiaozhen; Fan, Renli, LI, Chenfeng Ranllao Huaxue Xuebao 1981, 9 (2), 105-22. (29E) Sabela, Wladyslaw; Matysik, Czeslaw Banyasz. Kohasz. Lapok, Kohasz. 1982, 115 (9, 195-6 (Hung). (30E) Schmitt, Hubert; Choualb, Mohammed, (Process Patent) Ger. Offen. 2,914,306 23 Oct 1980, 7 pp. (31E) Scholz, A. Tech. M l t f . 1982, 75 (2-3), 100-8 (Ger). (32E) Stuchlik, Vladimlr Hutn. Lisfy 1981, 36 (4), 226-30 (Czech).
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Inorganic Constltuents (IF) Baneriee. D. D.; Chentamarakshan, K.; Mookherjea, S. K. Indian J . fechnol.. 1981, 19 ( l l ) , 489-91 (Eng). (2F) Barker, 0. Pulse (Kloof, S . Afr.) 1981, (Sept.), 96-7, 99 (Eng). (3F) Bettinelll, M. Riv. Combust. 1981, 35 (IO-12), 446-52 (Ital). (4F) Boeck, H.; Sarac, I.; Grass, F. J . Radioanal. Chem. 1981, 61 (1-2), 329-34 (Eng). (5F) Bosshart, R. E.; Price, A. A.; Ford, C. T. Report 1980, COO-4427-35, 185 PP (En@. (6F) Brown, James, R.; Kronberg, Barbara I.; Fyfe, William S. Fuel 1981, 60 (5), 439-46 (Eng). (7F) Bujok, J.; Jarczyk, L.; Rokita, E.; Slominska, D.; Strzalkowski, A. Nucl. Phys. Methods Mater. Res., Proc. Dlv. Conf., 7th 1980, 395-7 (Eng). (8F) Cahiil, R. A.; Frost, J. K.; Camp, L. R.; Ruch, R. R. At. Nucl. Methods FossilEnergy Res., (Proc. Am. Nucl. SOC. Conf.) 1980 1982, 115-31 (Eng). (9F) Casella, V. R.; Bishop, C. T.; Glosby, A. A,; Phillips, C. A. J . Radioanal. Chem. 1981, 62 (1-2),257-66 (Eng). (IOF) Castillo, J. R.; Lanaja, J.; Aznarez, J. Analyst (London) 1982, 107 (1270), 89-95 (Eng). ( I I F ) Chen, J. R.; Kneis, H.; Martin, B.; Nobiling, R.; Traxel, K.; Chao, E. C. T.; Minkin, J. A. Nucl. Instrum. Methods 1981, 181 (1-3), 151-7 (Eng). (12F) Chu, Su-Te; Wang, Yu-Chi; Chien, Chiu-Fang; Chen, PinJu; Sun, ChiuHsln K'o Hsueh T'ung Pa0 1981, 26 (4), 256 (Ch). (13F) Doolan, K. J. Anal. Chem. Acta 1982, 140 (I), 187-95 (Eng). (14F) Earnest, C. M.; Brennan, W. P.; Fyans, R. L. Proc. Eur. Symp. Therm. Anal. 1981, Znd, 517-19 (Eng). 115FI Earnest. C. M.: Garrabe. G. Journ. Calorim. Anal. Therm. 1981, 12, ' M8,-M8* (fi). (16F) Ebdon. L.; Wilkinson, J. R.; Jackson, K. W. Analyst (London) 1982, 107 (1272), 269-75 (Eng). (17F) Deutsche Gesellschaft fuer Mineraloelwissenschaft und Kohlechemie e.V. Ber. Dtsch. Ges. Mlneraloelwlss. Kohlechem. 1980, 289-01, 52 pp (Ger). (18F) Gaiantanu, V.; Engelmann, C. J. Radloanal. Chem. 1981, 67 (I), 143-63 (Fr). (19F) Gray, Vincent, R. Fuel 1981, 60 (4), 362-4 (Eng). (20F) Ihida, Mutsumi; Ishil, Teruakl; Ohnishi, Rieko Prepr. Div. Fuel Chem., Am. Chem. SOC. 1979, 24 (I), 262-70 (Eng). (21F) Jacobs, M. Leroy J. Coal Qual. 1981, (I), 20-2, 24 (Eng). (22F) Kler, V. R. Dokl. Akad. Nauk SSSR 1981, 259 (4), 996-8 (Geochem.)(Russ).
SOLID AND GASEOUS FUELS (23F) Klo!;e, Erhard; Kaltofen, Erich; Lange, Guenter; Birndt, Herbert Freiberg. Forschungsh. A 1980, A 625, 147-55 (Ger). (24F) Kostadinov, K.; Djingova, R. Radiochem. Radioanal. Leff. 1980, 45 (4), 297-304 (Eng). (25F) Laktionova, N. V.; Egorov, A. P. U.S.S.R. 828.031, 07 May 1981, Appl. 2,738,685, 16 Mar 1979. From Otkytiya, Izohref., from. Obuaztsy, Tovarnye Znakl 1981, (17), 183. (26F) Lebtdev, A. K. Mefody Razved. Goeflz. Yader. Geofiz . Y /?ud. Geol., L . 19811, 49-54 (Russ). (27F) Ledingham. K. W. D.; Kelliher, M. G.; Robertson, S. D. J . Radioanal. Chem. 1982, 71 (I-2), 169-80 (Eng). (26F) Leonhardt, J. W.; Bothe, H. K.; Langrock, E. J.; Maul, E.; Morgenstern, P.; Mueller, D.; Thuemmel, H. W. J . Radioanal. Chem. 1982, 7 1 (1-2), 181-7 (Eng). (29F) Lustigova, Mllena; Kubant, Josef; Strnad, Vladisiav Sb. f r . UVf 1980, 40, 91-118 (Czech). (30F) Mahiony, Barbara; Moulson, Ivor; Wilkinson, Herbet C. Fuol 1981, 60 (4), 355-8 (Eng). . (31F) British Carbonization Research Assoc. Carbonization Res. l ? e ~1980, 85,9 PP (Eng). (32F) McQuaid, J. H.; Brown, D. R.; Gozani, T.; Bozorgmaneslh, H. I€€€ Trans. Nucl. Sci. 1981, NS28 (l), 304-7 (Eng). (33F) Miiis, John C.; Turner, K. E.; Roller, P. W.; Belcher, C. B. X-Ray Spectrom. 1981, 10 (3), 131-7 (Eng). (34F) Mlnkin, Jean A.; Chao, E. C. T.: Thompson, Carolyn L. frepr..Div. Fuel Chem., Am. Chem. SOC. 1979, 24 (I), 242-9 (Eng). (35F) Mitsiubishi Heavy Industries, Ltd. Jpn. Kokai Tokkyo Koho 81 37,552. 11 Apr 1961, Appl. 79/112,600, 03 Sp 1979; 4 pp, (36F) Mozta, A. K.f Strlckler. D. W.; Austln. L. 0. Scanning Electron MicrosCopy 1980 (4), 91-6 (Eng). (37F) Nadkarni, R. A. Am. Lab. (Fairfeid, Conn.) 1981, 73 (e), 22, 24, 27-9 (Enol. (36F) NkiEh&$, C. L.; D’Auria, J. M. Analyst (London) 1981. 706 (1265), 874-62 (Eng). (39F) Pandey, H. D.; Haque, R.; Ramaswamy, V. Avd. X-Ray Anal. 1981, 24, 323-7 (Eng). (40F) Reynolds, G.; Bozorgmanesh, H.; Ellas, E.; Gozanl, T.; Mauiilg. T.; Orphan, V. Report 1960, EPRI-CS-989 (Vol. l), 80 pp. (Eng). (41F) Rigiri, V. I . Zh. Anal. Khlm. 1981, 36 (E), 1522-6 (Russ). (42F) Roscoe, B. A. Report 1981, DOE/EV/10403-5, 202 pp (Eng.) (43F) Sowerby, B. D.; Ngo, V. N. Nucl. Instrum. Methods fhys. Res. 1981, 168 (2), 429-37 (Eng). (44F) Stohl, F. V. Report 1980, SAND-79-2016, 43 pp. (Eng). (45F) Suzuki, Shogo; Hirai, Shoji Eunseki Kagaku 1982, 31 (8). 443-9 (Japan). (46F) Svendsen, Leo G.; Hertel, Niels; Soerensen, Gunnar Nuci. Instrum. Methods fhys. Res. 1981, 791 (1-3), 414-18 (Eng). (47F) Wilde, H. R.; Herzog, W. J . Radioanal. Chem. 1982, 77 (I-:?), 253-64 (Eng). (48F) Wiikinson, J. R.; Ebdon, L.; Jackson, K. W. Anal. R o c . (London) 1982, 19 (6), 805-7 (Eng). (49F) Xu, Ding-Rong; Qian, Zhen-Guan, Qiu, De-Rang; LI, biog.Yan Chechiang Ta Hsueh Hsueh f a 0 1980, (l), 28-47 (Ch). (50F) Zharig, Chuanzhi Coal Sci. Technoi. (Beling) 1981, (g), 38-42 (Ch). Mlscellaneous (1G) Bornhiop, Darryl J.; Manahan, Stanley E.; Farrier, David S. Anal. Lett. 1980, 13 (A12), 1041-61 (Eng). (2G) Edwards, G. Robin; Evans, T. Michael; Robertson, Struan D.; Summers, Charles W. Fuel 1980, 59 (12), 626-30 (Eng). (3G) Lustigova, Milena Sb. f r . UVf 1980, 39,93-105 (Czech). (4G) Mikni!:, R. P.; Maclel, G. E.; Bartuska, V. J. frepr. Div. Fuel Chem., Am. Chem. SOC. 1979, 24 (2), 327-33 (Eng). (5G) Neavtrl, R. C.; Hippo, E. J.; Smith, S. E.; Miller, R. N. frepr. Dlv. Fuel Chem., Am. Chem. SOC. 1980, 25 (3), 246-57 (Eng). (6G) Paintor, Paul C.; Rimmer, Susan M.; Snyder, Randy W.; Davis, Alan. Appl. Specfrosc. 1981, 35 (l), 102-6 (Eng). (7G) Stadelhofer, Juergen W.; Bartle. Kekh D.; Matthews, Raymond S,Erdoel Kohle, Erdgas, fetrochem. Brennst.-Chem. 1981, 34 (2), 71-6 (Eng). (6G) Wllllarns, J. M. Report 1980, LA-8409-MS, 51 pp (Eng). Standard Methods (IH) ASTM Standards, Philadelphia, PA, Part 26 (1962). GASEOUSFUELS General Revlews (11) Boschan, E. Energiagazdalkodas 1980, 27 (7), 294-300 (Hung); Chem. Absfr. 1980, 93, 170555. (21) Campo, M. P. froc. I n f . Sch. Hydrocarbon Meas. 1981, 58,223-4. (31) Curry, R. N. OilGasJ. 1980, 78(29), 56-9. (41) Dumay, M. H. C . R . Congr. Ind. Gaz. 1979, 96,85-99 (Fr); Chem. Absfr. 1980, 93, 134615. (51) &&enough, R. D. f r o c . Int. Sch. Hydrocarbon Meas. 11981, 56, 309-11. (61) Harris, D. G. froc. Int. Sch. Hydrocarbon Meas. 1981, 56, 572-3. (71) Kostrzewski, T.; Koraiewskl, W. fomlaty Clepine Energ. l98‘i, 322-42 (Russ/Pol); Chem. Abstr. 1982, 96, 125663. (61) McEntire, T. F. froc. Inf. Sch. Hydrocarbon Meas. 1981, 56, 101-4. (91) Roncier, M.; Nicaud, F. C . R. Congr. Ind. &z. 1979, 96,388-415 (Fr); Chem. Absfr. 1980, 93, 134616. (101) Kearney, D. A. froc Int. Sch. Hydrocarbon Meas. 1981, 56, 389-93.
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Sulfur Compounds (1K) Anon. (Osaka Gas Co., Ltd.) Jpn. Kokai Tokkyo Koho JP 62 00,5421 (Cl. GOlN21/72), 05 Jan 1982. (2K) Anon. (Osaka Gas Co., Ltd.) Jpn. Kokai Tokkyo Koho JP 82 00,547 (Cl. GOlN21/72), 05 Jan 1982. (3K) Anon. (Szechwan Institute of Chemistry) Fen Hsi Hua Hsueh 1977, 5 (5), 355-60 (Ch); Chem. Abstr. 1980, 93, 222791. (4K) Babluk, K. F. froc. Gas Cond. Conf. 1982, 32nd, B1-B15. (5K) Baiini, T. Ger. Offen. 3,016,318 (CI. GOlN27/26), 06 Nov 1980. (6K) Garai, T.; Balint, T ; Szucs, M. Anal. Chem. Symp. Ser. 1981, No. 8 (Ion-Sel. Electrodes, 3), 225-33. (7K) Garai, T.; Szucs, M.; Devay, J. M g y . Kem. Foly. 1980, 86(7), 2691-93 (Hung); Chem. Abstr. 1980, 93, 152631. (6K) Kuwata, K.; Uebori, M.; Yamada, K.; Yamazaki, Y. Anal. Chem. 1’982, 54 (7). . , 1082-7. (9K) Liu, G.; Luo, X. Huagong Xuebao 1981, (3), 266-78 (Ch); Chem. Ahsfr. 1982, 96, 71428. (IOK) Moen, A. R o c . Int. Sch. Hydrocarbon Meas. 1981, 56,261-7. (11K) Straka, P.; Buchtele, J. Chem. frum. 1981, 37 (9).474-7 (Czech); Chem. Abstr. 1982. 96. 55067. (12K) Zarlpov, T. M.; Ganeeva, A. R.; Galeeva, R. G. Neftepromysi. Delo 1982, (I), 38-9 (Russ); Chem. Abstr. 1982, 96, 163809. (13K) Zygmunt, B.; Staszewski, R. Chem. Anal. 1981, 26 (l), 109-14. Water Vapor (IL) Bozeman, J. C. froc. Int. Sch. Hydrocarbon Meas. 1981, 56,22!5-9. (2L) Chandler, A. W. R o c . Inf. Sch. Hydrocarbon Meas. 1981, 56,549-7. (3L) Dodds, D. E. Oper Sect. Roc.-Am. Gas Assoc. 1981, D307-D:311. (4L) Dodds, D. E. R o c . Int. Sch. Hydrocarbon Meas. 1981, 56, 250-2. (5L) Lee, C. W.; Fung, Y. S.;Fung, K. W. Anal. Chim. Acta 1982, 735(2), 277-63. (6L) Robinson, J. N.; Moore, R. G.; Heldemann, R. A.; Wlchert, E. R o c . Gas Cond. Conf. 1980, 3Qth, K1-K18. (7L) Shkol’nikova, V. V.; Kosyagin, V. G.; Strokova, T. P.; Shmakova, S. V. Gazov. from-sf., Ser.: Ispol’z. Gaza Nar. Khoz. (Ref. I n f . ) 1981, (6), 31-5 (Russ); Chem. Absfr. 1981, 95, 172134. (EL) Waklschmidt, H. Process Eng. (Coburg, Fed. Repub. Ger.) 1981, (3-4), 71-7 (Ger); Chem. Absfr. 1981, 95, 117966. Condensates (1M) Branisova, M. f&n 1981, 67(11), 324-6 (Czech); Chem. Absfr. 18182, 96, 165145. (2M) Craven, S. M.; Craft, B. D.; Franchetti, V. M.;Klnard, C.; Nunn, E. 8.; Pitre, E. M.; Ryan, R. L. Report 26 Nov 1980, MLM-2783, 11 pp Avail. NTIS; ERA 6 (3), 3335. (3M) Kabulov, B. D.; Ermol’ev, A. P.; Chumakov, Yu. I.Fiz.-Khim. Issied. Slntetich. i frirod. Sodin ., Samarkand 1980, 42-6 (Russ); Chem. Abstr. 1981, 9 4 , 159355. (4M) Koksharova, A. G.; Allslevich, L. N.; Yudin, A. E. Gazov. from-sf., Ser.: fodgof. fererab. Gaza Gazov. Kondens. (Ref. I n f . ) 1981, (2), 15-21 (Russ); Chem. Abstr. 1981, 95,64703. ANALYTICAL CHEMISTRY, VOL. 55, NO. 5, APRIL 1983
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Anal. Chem. 1983, 55, 4QR-56R (5M) Lunskii, M. Kh. Zavod. Lab. 1982, 48 (5), 17-20 (Russ); Chem. Abstr. 1982, 97,58151. Calorlmetry (IN) Curry, R. N. Oil Gas J. 1981, 79 (32), 95-6, 98-9. (2N) Howard, R. L. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56, 105-8. (3N) Kude, W. B.; Youngbauer, D. L.; Pearman, A. N. J. Eur. Pat. Appl. 31,145 (Ci. GOIN25/22), 01 Jul 1981. (4N) Maeda, S. U. S. US 4,329,873 (Cl. 73-19OCV; GOIN25/30), 18 May 1982. (5N) Maeda, S. U. S. US 4,329,874 (Cl. 73-19OCV; G01K17/00), 18 May 1982. (EN) Springer, T. A.; Norris, C. G.; McCoy, R. D. Anal. Instrum. 1980, 18, 109-17. (7N) Szonntagh, E. L. Brit. UK Pat. Appl. GB 2,074,728 (Cl. GOlN25122), 04 Nov 1981. (EN) Van Rossum, G. J.; Benes, G. J. GWF, Gas-Wasserfach: GaslErdgas 1981, 122(1), 12-19 (Ger); Chem. Abstr. 1981, 94, 159346. (9N) Vlllalobos, R. ISA Trans. 1982, 21 (2), 93-100. (10N) Watson, J. W.; White, F. A. Oil Qas J. 1982, 80 (14), 217-18, 220, 225. (11N) Williams, R. A. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56, 518-22. Density and Speclflc Gravlty (1P) Hanklnson, R. W.; Coker, T. A.; Thomson, G. H. Hydrocarbon Process ., Int. Ed. 1982, 61 (4), 207-8. (2P) Kahmann, A. R. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56,501-4. (3P) Lewis, H. E. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56, 234-9. (4P) Parrish, W. R.; Pollin, A. G.; Schmidt. T. W. Proc. Annu. Conv.-Gas Process. Assoc. 1982, 61, 164-70. (5P) Rozentsvaig, A. K.; Grevtsov, V. M. Neftepromysl. Del0 1982, (4), 24-6 (Russ); Chem. Abstr. 1982, 97, 41238. (6P) Rybalkin, V. I.; Labinov, S. D.; Zhurba, A. S. Neftepererab. Neftekhim. (Moscow) 1981, (6), 47-50 (Russ); Chem. Abstr. 1981, 95, 143612. (7P) Siegwarth, J. D.; LaBrecque, J. F. NBS Tech. Note (US.)1981, 1035. (8P) TerBush. D. J. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56,230-3. Samp II ng ( l a ) Astryanln, S . N. Gazov. Prom-st. 1981, (12), 20-1 (Russ); Chem. Abstr. 1982, 96, 125762. (2Q) Carpenter, R. L.; Newton, G. J.; Cheng, Y. S.; Barr, E. B.; Yeh, H. C. Report Dec 1980, LMF-84, pp 384-6 Avail. NTIS; E R A . 6(13), 19188. (30) Drake, C. F. Oper. Sect. Proc.-Am. Gas Assoc. 1980, T175-Tl86. (4Q) Neulander, C. K.; Walmet, G. E.; Zarchy, A. S.Report 1980, ANL-8062, pp 380-7; E.R.,A. 8(6), 6830. (5Q) Phillips, J. B. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56, 107-11.
(8Q) Schepers, H. H.; Kilmer, J. W.; Bernos, J. Proc., Annu. Conv.-Gas Process. Assoc. 1982, 6 1 , 1-8. (7Q) Stepanek, A.; Wittenberg, E.; Waloschek, V. Czech. CS 189,073 (Cl. G01N1/22), 15 Dec 1961. (8Q) Welker, T. F. Proc. Int. Sch. Hydrocarbon Meas. 1981, 5 6 , 531-5. (9Q) Welsch, T.; Engewald, W.; Huenerbein, G.; Apel, G. Chem. Tech. (Leipzlg) 1981, 33 (3), 149-51 (Ger); Chem. Abstr. 1981, 95,64697.
Mlscellaneous (IR) Abdurakhmanov, A. A.; Abbasov, A. A.; Askerov, A. B.; Veliyulin, E. Yu.; Imanov, L. M. Azerb. Khim. Zh. 1980, (l), 147-52 (Russ); Chem. Abstr. 1981, 94, 124230. (2R) Caffey, W. R. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56, 132-4. (3R) Dliler, D. E. J. Chem. Eng. Data 1982, 27(3), 240-3. (4R) Diller, D. E.; Chang, R. F. Appl. Spectrosc. 1980, 34 (4), 411-14. (5R) Erickson, M. D.; Frazier, S. E.; Sparacino, C. M. Fuel 1981, 60 (3), 263-6. (6R) Eubank, P. T.; Hall, K. R.; Holste, J. C.; Scheloske, J. J. Proc., Annu. Conv.-Gas Process. ASSOC.1980, 59, 18-30. (7R) Fleischmann, D.; Schwab, H. Ger. (East) 148,503 (CI. GOlN31/06), 11 Feb 1981. (8R) Haas, W. J. Jr.; Eckels, D. E.; Kniseley, R. N.; Fassel, V. A. Report 1981, IS-M-327 Avail. NTIS; E R A . 6(16), 23032. (9R) Keady, M. J. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56, 334-5. (10R) KLpka, H. VDI-Ber. 1980, 363, 127-31 (Ger); Chem. Abstr. 1981, 94,211248. (11R) Lloyd, D. W, 011 Oas J . 1981, 79 (38), 126-8, (12R) Loree. T. R.; Radziemski, L. J. Plasma Chem. Plasma Process. 1981, 1 (3), 271-9. (13R) Meyer, B.; Goetze, R.; Eidner, D.; Mueller, R.; Mottitschka, W.; Roessler, D. Ger. (East) 142,760 (CI. GOlN27/58), 09 Jul 1980. (14R) Moore, B. J. Report 1979, PB-80-142300, 119 pp Avail. NTIS; E.R.A. 8(2), 1969. (15R) Nersesova, N. A. Izv. Vyssh. Uchebn. Zaved., Neft Gaz 1981, 24 (12), 52-5 (Russ); Chem. Abstr. 1982, 96, 145575. (16R) Reid, R. C.; Shanes, L. M.; Virk, P. S. Report Dec 1979, PB-80210685, 81 pp Avail. NTIS; E.R.A. 6 (12), 16521. (17R) Sallet, D. W.; Wu, K. F. Report Apr 1980, PB-80-189053, 111 pp Avall. NTIS; E.R.A. 6 (lo), 13402. (18R) Tilley, H. C. Proc. Int. Sch. Hydrocarbon Meas. 1980, 55, 330-1. (19R) Wllliamson, E. Proc. Int. Sch. Hydrocarbon Meas. 1981, 56, 324-5. Standards (1s) ASTM Standards, Philadelphla, PA, Part 26 (1982). (2s) Curry, R. N. OilGas J. 1981, 79(44), 121-4. (3s) Helke, T. GWF, Gas-Wasserfach; GaslErdgas 1982, 123 (3), 119-21 (Ger); Chem. Abstr. 1982, 96, 183901. (45) Nagakura, R. Nippon Gasu Kyokaishi 1980, 33 (E), 26-35 (Japan); Chem. Abstr. 1981, 94,88778.
Industrial Hygiene Richard G. Melcher The Dow Chemical Company, Michigan Applied Science and Technology Laboratories, Analytical Laboratory, 574 Building, Midland, Michigan 48640
A. INTRODUCTION This review covers a period from approximately 1978 through 1982. Earlier references are included in some cases to give a more complete picture of the technique being discussed. There has been an exponential growth in industrial hygiene over the period, and no attempt was made to cover the entire field of industrial hygiene or even the analytical aspects of industrial hygiene chemistry. For some chemicals which have come under close scrutiny, such as vinyl chloride, benzene, acrylonitrile, and formaldehyde, there are many dozens of references in the literature and anyone interested in a complete survey for a specific chemical would best be served by running a specific literature search. The intent of this review was to cover some basic concepts of the most widely used technique in personal monitoring. One in-depth review for a class of compounds, the diisocyanates, is given since, in addition to showing a multidirectional analytical approach, it may give a sense of appreciation for the degree of effort expended in the development of methods for trace amounts of reactive chemicals. To ensure a safe working environment in the laboratory and production plants, it is often necessary to determine trace 40 R
0003-2700/83/0355-40R$08.50/0
quantities of organic chemicals in the work atmosphere. For a successful program it is necessary to have good communication between the toxicologist who must assess the toxicity of the compound, the industrial hygienist who must investigate the hazard of exposure to personnel, and the analytical chemist who must determine the concentration of the compound in the environment and in biological samples for metabolism and pharmacokinetic studies. The factors which affect the collection and determination of trace quantities can be quite complex, and each specialist involved in method development, sampling, or analytical measurements must have a basic understanding of the total effort. It is beyond the scope of this review to discuss the complexities of toxicological, industrial hygiene, or analytical techniques. The main emphasis will be on collection with solid sorbents, either using ump and tube or diffusional sampling techniques, followed \y thermal desorption or solvent desorption. This includes a majority of the samples presently being collected and new methods being developed. Solid sorbent sampling tubes and dosimeters are convenient to use, can concentrate trace contaminants, and can be used for area samples as well as for employee breathing-zone samples. 0 1983 American
Chemical Society
