Solid and gaseous fuels - Analytical Chemistry (ACS Publications)

Chem. , 1981, 53 (5), pp 233–241. DOI: 10.1021/ac00228a015. Publication Date: April 1981. ACS Legacy Archive. Cite this:Anal. Chem. 53, 5, 233-241. ...
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(16J) Ladenson, J. H., McDonald, J. M., Landt, M., Schwartz, M. K., Colorectal Carclnoma and Carclnoembryonlc Antlgen (CEA). Clln. Chem., 26, 1213 (1980). 117J) Natelson, S., Mlletich, D. J., Seals, C. F., Vlsintlne, D. J., Albrecht, R. F., Cllnical Biochemistry of Epilepsy. I. Nature of the Disease and a Review of the Chemical f:indings in Epilepsy. Ciin. Chem., 25, 889 (1979). (l8J) Natelson, S., Mlletlch, D. J., Seals, C. F.. Vislntine, D. J., Albrecht, R. F., Clinical Biochemistry of Epilepsy. 11. Observations on Two Types of Epileptiform Convulsions Induced in Rabbits with Corticotropin. Clln. Chem., 25, 898 (1979). (19J) Natelson, S., Sherwin, J. E., Proposed Mechanlsm for Urea Nitrogen Reutilization: Relationship between Urea and Proposed Guanidine Cycles. Ciln. Chem., 25, 1343 (1979). (20J) Nerenberg, S. T.. Prasad, R., Pedersen, L. D., Biskup, N. S., Radlolmmunoassay for Detection of Latent Chronic Alcoholic Pancreatis, an Unrecognized Cllnlcal Syndrome. Clin. Chem., 26, 214 (1980). (21J) O'Reilly, Dennis St. J., Delamere, J. P., Cause of Alkalosis in "Diabetic Ketoalkalosis. Clin. Chem., 26, 171 (1980). (22J) Porter, C. J., Curnow, D. H., IFCC ProvisionalRecomrnendatlon (1979) on a Scheme for a Two-Year Postgraduate Course in Clinical Chemlstry. Clin. Chem., 26, 1748 (1980).

(23J) Pottgen, P., Salvatore, R., AntCDNA Binding Activity in Systemlc Lupus Ervthematosus, Rheumatoid Arthritis, and Normal Subjects. Ciin. Chem., 25, 1342 (1979). (24J) Pragay, D. A,, Howard, S. F., Gill, E. S., Cllnlcal Laboratory Accidents, and Some Recommended Remedies. Ciln. Chem., 26, 1107 (1980). (25J) PrzyJemskl,C. J.; Fike, S. S., Frow, E., Comments on a Case Report on Myocardial Infarction, (Reply), Borer, W., Wdlener, J., Papadopoulos, N. Clin. Chem., 26, 534 (1980). (26J) Rice E. W., Quarter-Century Bibliographic Review of Clinical Chemisfry. Clin. Chem., 26, 790 (1980). (27J) Schwertner, H. A., Hawthorne, S. E., Albumin-Bound Fluorescence In Serum of Patlents with Chronlc Renal Fallure., Ciin. Chern., 26, 649 (1980). (26J) Sheehan, M., Salmon, J., Haythorn, P., Quality Control of Measurements of Total Iron-Blndlng Capaclty. Ciin. Chem., 25, 1335 (1979). (29J) Steinmetz, J., Panek. E., Siest, G., Personal and Familial Factors In Cholesterolemia: Criteria for Selection of a Reference Population. Ciin. Chem., 26, 219 (1980). (30J) Trawick, W. G., OPINION: A Model Program for Educatlon and Training of Cllnlcai Chemists. Ciin. Chem., 25, 1885 (1979). (31J) Worsfold, M., Care in Use of Phenazlne Methosulfate in the Laboratory. Clin. Chem., 26, 1622 (1980).

Solid and Gaseous Fuels Hyman Schultz," Arthur W. Wells, and Tlmothy W. Bergstresser Department

of Energy, Pittsburgh Energy Technology Center, P. 0,Box 10940, Pittsburgh, Pennsylvania 15236

SOLID FUELS This section covers methods of sampling, analyzing, and testing coal, coke, and related materials. Energy Research Abstracts and ChemicalAbstracts were used as the primary reference sources. In most categories the volume of material available made it necessary to limit the number of publications in the review.

SAMPLING ANI) PROXIMATE ANALYSIS Sampling. The South African Bureau of Standards published a two-part code of practice concerning the sampling and preparation of a coal sample for analysis (29A) (30A). Colombo and Scholz, (IOA) reported on a collaborative investigation aimed at ascertaining the long-term preservability of coal samples. Proximate Analysis. Rapid methods for proximate analysis were reported by Vedana and Bristoti (34A) using derivatograph and by Fyans (IIA) using thermogravimetric analysis and Jfferential scannin calorimetry. Bryres et al. (8A) discussed using thermal andytical techniques for proximate analysis. Tustanovskii (33A) irradiated coals and coke with fast neutrons and subsequently measured 16N radiation to determine moisture and ash content. Coal streams were analyzed for moisture and ash by Worster (36A)and Sowerby ( 3 1 4 using neutron capture y-ray analysis. Sowerby used 4.43-MeV I2C y-rays from elastic scattering and separate 6oCoy-ray scattering measurements to correct for sample variations. Moisture content of coal was determined by low-resolution nuclear magnetic resonance by Robertson et al. (25A)and by pulse NMR by Kurotu et al. (17A). The suitability of the microwave method of determining moisture was investigated by Hoberg and Klein (15A). They discussed various prociedures for the reduction of errors encountered. Schaefer and Jansen (26A)determined water content in coal using multiple regression calculations to calibrate a capacitive moisture meter. Bevan et al. (2A)and Brown (6A)examined electromagnetic techniques for moisture content determination. Bevan gave a list of manufacturers of moisture analyzers. Brown et al. (5A) discussed the use of capacitance response, NMR, and microwave absorption fior on-line moisture monitoring of coal. Allardice and Evans (IA)reviewed 23 references concerning moisture content determinations and moisture holding capacity. This

article not subject to US.

Ash. Clayton and Wormald (9A) described an ash monitoring device comprised of a neutron source, a specific energy y-ray detector, and a readout device. Induced y-ray spectroscopic methods were used by Borushko et al. (4A) and Simon et al. (28A) for high-speed determination of ash content. Mathew (18A) found that the natural y-ray activity of brown coal is strongly correlated with ash content. An accuracy of 1.1%ash was reported for samples from a single seam. The ratio of coherent and noncoherent scattered soft y-and X-ray radiation was used to determine ash content by Meier et al. (19A). They also discussed the possible improvement of the determination by considering matrix affects and the influence of variable measurement distances. Rapid determination of ash by XRF was discussed by Brown and Jones (7A) and Renault (24A). A technique for ash determination by neutron-activation analysis utilizing a 252Cfsource was described by Wormald et al. (35A). Radioisotopic methods for ash determinations were used by Srivastava et al. (32A), Onishchenko et al. (22A), and Mokrzycki and Wykrota (20A). The parr formula, normative analysis, LTA, and X-ray diffraction were compared by Pollack (23A) for their ability to estimate mineral matter content of coal from its major inorganic elements. Computer y logging for the estimation of coal ash content was described by Kulinkovich et al. (16A). Errors in ash determination by radioisotopic methods were discussed by Bochenin (3A) and by Grabov et al. (14A). Volatile Matter. The effects of small sample size on the accuracy of volatile and ash determinations were investigated by Gorelov and Butina (13A). They found that the results were acceptable when analytical rules for small samples are observed. Scholz (27A) showed a correlation between the volatile matter content and mineral matter in hard coals. He proposed methods for calculating volatile matter content (DMMF) of coal from a particular mine and a general equation to be used for classification. A procedure for forecasting the volatile matter content of coal, correcting for the pro ortions of vitrinite, semivitrinite, and fusinite, was presentecfby Nesterov and Andreeva (21A). Gold (12A) used differential scanning calorimetry to show the occurrence of exothermic reactions associated with the production of volatile matter. The heating rate and the sample

Copyright. Published 1981 by the American Chemlcal Society

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mass affected the temperature and magnitude of the exothermic peak. Weathering effects due to oxidation also influenced the thermal properties of coal.

ULTIMATE ANALYSIS AND SULFUR FORMS Macias and Barker (31B) used proton induced y-ray analysis to measure C, N, 0, and S in coal. They reported an accuracy of approximately 5% and a precision of approximately 4%. Failey et al. (9B) measured C, H, N, and S by neutroncapture prompt y-ray activation analysis (PGAA) of several SRMs. Californium-252 was used as a neutron source for PGAA to determine C, H, S, and N by Lagarias et al. (26B), Herzenberg et al. (19B),and Reynolds et al. (37B). On-stream analysis of coal by neutron-y spectrometry was reported by Rhodes (38B). He discussed the choice of instrumentation and the best reactions to use. He reported precisions of *0.01% H, f0.2% C, *0.1% N, and f0.03% S with a measurement time of 10 min or less. Gas-liquid chromatographyof coal combustion gas was used by Batina and Gorelov (4B) to determine C, H, N, and 0 content. Gontsov and Kurbatova (11B) used gas chromatography to determine C and N of pyrolyzed coal. Hanson and Vanderborgh (16B) reviewed 33 references concerning the use of laser pyrolysis-gas chromatography as a rapid method for determing coal constituents. Carbon. A prototype automated macro apparatus for the determination of carbon and hydrogen in coals is described by Takacs-Ivanics (42B). Saitoh and Ishii (39B) described a procedure for the quick analysis of C and H in coal. Hydrogen. Gozani et al. (12B)reviewed nuclear techniques for determining the total hydrogen content of coal. The study has shown that hydrogen is most accurately determined by measuring the leakage of epithermal neutrons from a 30 cm thick slab sample. The average relative error was less than 1.5%. Higher accuracy is obtainable if coal type variations are limited. Nitrogen. Doolan and Belcher (8B) and Li et al. (30B) described methods of determining nitrogen in coal by digesting the sample and then determining the N content with an ammonia dectrode. The Dumas and Kjeldahl methods and their modifications were compared by Krzyzarowska and Kubica (25B)and Hata and Kono (17B). Hata and Kono attributed the lower values obtained with the Kjeldahl method to the existence of nitrogenous radicals that do not easily change into NH3. They only found considerable differences in the two methods for bituminous coal and coke. Banerjee et al. (3B)reported that a H2SO4-H3PO4digestion mixture gives higher N values than the unmodified Kjeldahl method. They credited the difference to the higher digestion temperature: Oxygen. Volborth (44B)gave a review with 48 references concerning the use of neutron activation analysis for the accurate monitoring of oxygen and nitrogen. Charged article activation analysis was used by Schlyer et al. (40BPto determine 0 content. Hamrin et al. (15B) studied the use of instrumental activation analysis for 0 and N in coal. Volborth (45B) in discussing the probIem of determining the oxygen content of coal by difference recommended the use of fast neutron activation analysis as the most accurate, inexpensive, and rapid method. Sulfur. Ahmed and Whalley (IB)reviewed 33 references regarding the oxygen-flask method of determining total sulfur in coal. Analytical procedures for determining the sulfur content of coal desulfurization products were reviewed by Chakrabarti (6B). Methods were described by Cooper et al. (7B) and Sofilic et al. (4IB)to determine sulfur content bv X-rav fluorescence analysis. An average deviation of 0.1%"for Swas reported by Cooper. Van Grondelle and Zeen (43B)and Ivanov (21B)described total sulfur analysis by coulometric titration. The method is useful for sulfur concentrations up to 5 % . Lathouse and Heffelfinger (27B) and Mizisin et al. (33B) used ion chromatography to determine sulfur content. The problem of nitrogen interference is discussed. An on-line elemental analyzer is described by Cekorich et al. (5B)that uses prompt y-ray analysis to determine total sulfur, secondarily ash content, and possibly BTU content. I

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Layfield (28B) describes in his thesis the design, construction, and characterization of a facility for neutron capture y-ray analysis of coal. Total sulfur was determined by usin californium-252as the source by Layfield and by Ghavi and Cogburn (IOB). Neavel and Keller (34B)described a procedure to estimate sulfur content from the titration of the calorimeter bomb washing. Ninty-three percent of 768 samples used differed by less than 1% from values determined by standard procedures. Sulfur Forms. A new technique for sulfur forms analysis based on low-temperatureoxygen plasma ashing was described by Hamersma and Kraft (14B). The procedure has been tested on 25 coals and compared with ASTM analyses with excellent results. The data indicate that it is significantly more accurate and precise than the ASTM test D2492. A review by Jacobs et al. (22B)with 43 references concludes that Moessbauer spectroscopic characterization of coal has much to offer as an improved analytical method for determining forms of sulfur in coal. Attar (2B)gives a discussion on novel methods of coal sulfur analysis. A rapid technique combining XRF and XRD for total, sulfate, and pyritic sulfur determination is described by Paris and Schumacher (36B). Sources of analytical error in the forms of sulfur determination were identified by Greer (13B). Pyritic sulfur determination by Moessbauer spectroscopy is described by Huffman and Higgins (20B),Jag et al. (23B), and Levinson (29B). Panek et al. (35B)describefan apparatus for a fast determination of sulfur bound in pyrite and marcasite based upon y-ray absorption. Madec et al. (32B)reported on a method and apparatus for determining organic sulfur content. Harris et al. (18B)reported that petroleum coke is a suitable standard for the analysis of organic sulfur content of coal, since it is stable under an electron beam and contains a uniform sulfur content. Kuehn and Davis (24B) described a rapid scan system of automated reflectance microscopy capable of characterizing the pyrite content of coal.

CALORIC VALUE Linear correlations on a dry basis between lower calorific values, ash content, and either volatile matter or hydrogen content of Ruhr coals were given by Scholtz (2C). Regression curves for a given deposit can be used to approximate lower calorific values on a dry ash-free basis based on the volatile matter content. Ringen et al. ( I C ) found that the Boie equation was far superior to the Dulong equation for calculating heating values of fossil fuels.

PETROGRAPHY Stanton and Finkelman (150) reviewed 17 references on coal petrographic data and the implications of these data in evaluating the behavior of coal in physical cleaning, gasification, coking, and liquefaction. Chemical and petrographic characterizations used for evaluating electrical generation boiler and coking coals were discussed by Day et al. (30). Juckes and Pitt ( 6 0 ) described some aspects of a proposed standard method for petrographic analysis. Speight (120) reviewed 193 references that assessed the structures in coal by spectroscopic techniques. Thin sections of eastern Kentucky coal were studied by using transmitted IR microscopy by Harris and Yust ( 4 0 ) . This technique can be valuable in studies of seam profiles and correlations. NMR was used by Lynch and Webster (100)to study the plasticity of coal. Characterization of coal in its plastic state by isothermal Gieseler plastometry was examined by Lloyd (90). Scanning-electron and optical microscopy were combined by Stanton and Finkelman (140)to determine the total petrographic composition of coal. Harris and Yust ( 5 0 ) determined the ultrafine structure of coal by electron microscopy. Small-angleX-ray scattering and transmission electron microscopy were used by Lin et al. ( 7 0 ) to study the microporosity and the micromineralogy of vitrinite in a high-volatile bituminous coal. Spitzer et al. (130) did analysis of coal micropore structure based on methanol adsorption isotherms.

SOLID AND GASEOUS FUELS

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Marsh and Smith (130 on the formation and properties of anisotropic cokes that were studied hy optical and scanning electron microsco y Vanpoulle ( 2 1 8 published the first results that were obtained from the I S 0 combined test (Micum-IRSID) on coke over 20 mm in size. The coking strength of a coal was determined by Fujiio and Kato (7E)based on the sulfur content of the vitmite and the amount of exinite, fusinite, etc. in the coal. The British Carbonization Research Association (2E) studied the changes in the properties of coke arising from partial oxidation. Painter et al. ( 1 7 0 studied variations in the oxidation of coking coals with FIlR s p e c t m p y . The results suggest that the formation of ester cross-links is responsible for the loss of swelling characteristics and coking properties in oxidized Mhw W. W e b k a Cbernlsl h mS A m W coal. mi Chernblry Branch. Pmsburgh Energy Wachowska et al. ( 2 2 0 studied the effects of preheating Technoloey Center He recebd his B A coals on some of their properties. and M A decrees in chemistry horn ma The dependence of the caking and coking properties of Unlversny 01 Northem Cohnado In 1969 and '+ * slightly metamorphized coals on their chemical and petro1973. respecllveb Before bining me pmsgraphic composition is discussed by Ulanov (2OE). bugh Energy Technoksy Cenler. he was an Jasienko (8E)gave a renew of 109 references on the nature Analytical Chemist tor m e Occupational of coking coals. Slety and Heath Adrnlnklraiion. U S De- I( panmanl of Labar He is presently engaged Miyazawa et al. ( 1 4 0 described the use of the spin-lattice in research an the Cbracterizatbn 01 the , relaxation time of coal to characterize the size, shape, and prcducts Of Coal mverslo" optical texture of the resultant coke. The physicochemical properties of activated coke were studied by Nefedov e t al. (15E). Additions of alkali metals and ferric chloride increased the porosity of the cokes and improved their wetting by the slag. Brown (3E)discussed the mechanisms b which additives lhothy W. k@um k a chrmkl h the affect coking. The principles of blending Coal Anaiyis kanch. Plttsbwgh Energy are discussed by Callcott (4E). Sakawa and Uno for coke (19E)us Techrdqy Canter. He received hls 0.A. in ESR to evaluate the quality of coke binders. physhx from Gellysbvg College in 1974 Pacheco and Marsh (16E) characterized and related the and studied chemisny ai optical texture of cokes to topographic changes induced by Pmsburgh. He is pesenily engagad in reaction with KOH and oxygen. methods dewlopmen1 for me determinalkn Cokin properties and coke quality were used by Crelling of me lnaganic CwIslnuBnts of coal and et al. ( 6 h to quantify the effects of weathered coal on coke c w l ash. making. Akhmetov et al. ( I E ) used the coefficients of thermal expansion to evaluate coke quality. Karboviac ( 9 0 discussed the c o k i n ~ o m the~estimating ~ Vickers microhardness impressions were used by Das and of coking roperties of coals, and the c actenzation of cokes. Hucka (ID) to evaluate the elasticity, plasticity, brittleness, The cofability of coal was determined by Chatterjee et al. durtility. and hardness of different ranks and types of coal. ( 5 0 by measuring their plasticity with the L. M. Sapozhnikov Macmillan and Rickerby ( I I D ) . using Vickers microhardness test. measurements, found that the hardness values were not affected by the angle of the coal surfare to the bedding plane INORGANIC CONSTITUENTS hut that they were influenced by the extent of coalification. Methods of measuring the surface area of coal and evaluJenkins and Walker (23nreviewed many reference on the ating the internal surface area of Illinois coal were discussed analysis of mineral matter in coal. Ash com osition was by Thomas and Damberger (161)). Correlations were shown correlated to the melting point of ash by BarysEev ( 2 0 and between internal surface area and coal rank parameters. Mehnert (33F). Vol'pova et al. (IRDI reported that the vitrinite anisotropy Ion exchange chromatography (IC) was applied to the index can be used to predict the degree of coal reduction. analysis of anions derived from fuels by Butler et al. ( 3 0 . No A new technique for measuring the maximum reflectanre significant differences were observed between the results of vitrinite was reponed by Ting and La (170). The maximum obtained by IC and ASTM methods. Methods of determining reflectance was calculated from three separate reflectance chlorine in coal were reviewed by Chakrabarti (7F). Heunisch readings on the same vitrinite grain at 45' angular intervnls. ( 2 0 0 determined chlorine by potentiometric titration after Davis 120) employed several techniques to determine the decomposition with sodium biphenyl. A rapid general mioptical properties of coal runstituents. Various equipment crodetermination of fluorine was given by Van Leuven et al. modifications and accessories were employed to improve the (460. Fluorine was liberated from the sample as HF by means ease of measuring maximum reflectance. An automated reof ovrohvdrolvsis with steam at 1120 "C and then measured flectance microscope (ARM)was examined by Liscinsky and hy'an ion-sel&tive electrode. Vastola !bD,. HeaLtime algorithm enhancement o i the data Hothenberg and DeNee i 4 I 0 chacterized fly ash by using allowed some of the inherent limitations to be redured. ESCA. SK\l. and EI)XA. 'l'wentv-eight elements in coal and coal ash were analyzed by Nadkarni (:KOwing inductively coupled lasma emission COKING PROCESS AND COKE TESTING spectruscopy. Hajdus and Chowaniec ( 1 7 8 used emission A renew of sampling. ,mm le reparation, and analysis of spectrography to analyze coal ash for its major components. metallurgical cokes was pvengy {atrick and Wilkinson ( I B E ) . A procedure for the analysis of coal ash by atomic abKosina ( I I E ) gave a review on roal mirropetrographic methods so tion spectroscopy was 'ven by h a et al. (220. OReiiy and their application for the evaluation of coal coking propanTHicks (37O describefa method of analnine whole coal erties. Kimura llOE) reviewed 23 references on the properties by aqueous slurry-injection into a conventconaiatomic abof coal and metallurgical coke. The estimation of coke aornt.ion . . ~ ~.~~ . snectronhotometer. roperties from its microscopic examination was renewed by Flertron probe mirroanalysis of coal particles was reviewed ackowsky (12Ej. A review of 86 references was given by by Rnvmond and Gunky (?OF). Mom et al. (350described the use of computer-controlled scanning electron microscopy to determine the inorganic composition of coal particles.

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A comparison of energy dispersive X-ray fluorescence and atomic absorption s ectrometry for the analysis of fly ash was given by Wegscheigr et al. (50F). Ersepke and Luzar (12F) reviewed 208 references on determining inorganic constituents of coal by X-ray fluorescence and atomic absorption spectrometry. The use of FTIR for the study of organic structure and inorganic components of coal was given by Painter and Coleman (38F). Lyons et al. (31F) compared data for 41 elements in coal that were determined by instrumental neutron activation analysis, isotope dilution spark-source mass spectroscopy, and atomic absorption spectroscopy. The present status of elemental analysis of coal and coal ash by instrumental neutron activation was given by Steinnes (44F). On-line analysis of the major elements in coal ash by neutron mduced y spectrometry was described by Stewart and Hall (43F) and Herzenberg et al. (I9F). Clark (SF) described the use of instrumental neutron activation analysis for determining minor and trace elements in coal. Huggins and Huffman (21F) reviewed the use of Moessbauer spectroscopy to characterize the iron containing minerals in coal and coal products. Reports on determining iron containing minerals by Moessbauer spectroscopy were given by Keisch et al. (24F) and Russell and Montan0 (42F). Lee et al. (299 correlated Moessbauer and SEM studies of coal to identify the principal mineral transformations during carbonization. Trace Elements. Cavallaro et al. (6F)determined trace elements in the various specific gravity fractions of U.S. coals. Most of the trace elements were concentrated in the heavier specific gravity fractions. Egorov et al. ( 1 I F ) studied the effect of temperature on the loss of trace elements in the combustion of brown and bituminous coal. The distribution and fate of 34 trace elements in the SRC process were studied by Filby et al. (13F) using instrumental neutron activation analysis (INAA). Manchuk et al. (32F) studied trace elements in coal dust using INAA. Ting and Manahan (45F) used INAA to determine the volatilities of eight environmental1 important trace elements. The method, instrumentation, an advantages of INAA for trace element analysis of coal, fly ash, and fuel oils are described by Weaver (49F). Energy dispersive X-ray fluorescence (EDXRF) was used by Prather et al. (39F) to determine trace elements in coal and SRC. Coleman et al. (9F) used flameless atomic absorption spectroscopy to determine trace elements in SRC fractions. These data were compared with previously reported EDXRF data from the analysis of similar material. Several articles were written on the use of spark-sourcemass spectrometry to determine trace elements in coal and coal products. Koppenaal (26F) reported on its use on coal gasification process streams. Lett et al. (30F) used SSMS to analyze coal liquefaction products. Guidoboni (16F)gave a review of 23 references on SSMS and AAS. Koppenaal et al. (25F) used isotope dilutipn SSMS to determine Ni, Cu, Se, Cd, T1, and Pb in coal gasification products. Carter et al. (4F) reviewed the use of isotope dilution SSMS and thermal emission spectrometry. Beryllium. Gladney (15F) reported a technique for direct measurement of Be in coal by flameless atomic absorption spectroscopy. Lead. y-ray spectroscopywas used by Coles and Meadows ( 1 O F ) to determine lead-210 content of coal and fl ash and by Morris and Bobrowski (3487 to determine leaJ214, bismuth-214, and radium-226. Mercury. Flameless atomic absor tion spectrometry was used by Hejtmanek and Dolezal (18Jto determine Hg after it was thermally released from a Au amalgamator. A method to determine H by destructive neutron activation analysis is described by Ifostadinov and Dzhingova (27F). The method is based on the decomposition of an irradiated sample, precipitation of the Hg as HgS, and subsequent monitoring of the Hg. The total error of analysis is f 7 % . Nickel. Wang (47F) reported on a polarographic method that avoids the vanadium interference. Atomic absorption spectrometric determination of nickel, vanadium, and copper by solid sampling was used by Langmyhr and Aadalen (28F). Selenium. Wangen et al. (48F) used a y-y coincidence technique to determine low levels of Se in SRMs. Detection limits of 50-100 ng/g were reported for fly ash and coal.

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Uranium. INAA was used by Fujii et al. (14F) to determine trace amounts of U. Cassella et al. ( 5 0 used a radiochemical procedure to determine U, Th, and lead-210 in coal and coal ash. Alderman et al. (IF) reviewed 63 references on uranium in coal and carbonaceous rocks in the U.S. and Canada.

STANDARD METHODS The American Society of Testing Materials (ASTM) (IG) coordinates the development and standarization of test procedures for coal and coke through the D-5 committee. Standards that were adopted, revised, or reapproved during this review period include the following: D 167-73(1979), Test for Specific Gravity and Porosity of Lump Coke; D 197-30 (19801, Sam ling and Fineness Test of Pulverized Coal; D 291-60 (19807, Test for Cubic Foot Weight of Crushed Bituminous Coal; D 293-69 (1980),Sieve Analysis of Coke; D 310-69 (1980), Test for Size of Anthracite; D 440-49 (1980), Drop Shatter Test for Coal; D 441-45 (1980), Tumbler Test for Coal, D 547-41 (1980),Test for Index of Dustiness of Coal and Coke; D 1412-74 (1979), Test for Equilibrium Moisture of Coal at 96 to 97% Relative Humidity and 30 "C; D 1756-62 (19791, Test for Carbon Dioxide in Coal; D 1757-80, Test for Sulfur in Ash from Coal and Coke; D 2492-79, Test for Forms of Sulfur in Coal; D 2795-69 (1980), Analysis of Coal and Coke Ash; D 2797-72 (19801, Preparing Coal Samples for Microscopical Analysis by Reflected Light; D 2798-79, Microscopical Determination of the Reflectanceof the Organic Components in a'Polished Specimen of Coal; D 2799-72 (1980), Microscopical Determination of Volume Percent of Physical Comonents of Coal; D 2961-79, Test for Total Moisture in Coal keduced to No. 8 (2.38 mm) Top Sieve Size (Limited-Purpose Method); D 3172-73 (1979), Proximate Analysis of Coal and Coke; D 3173-73 (1979), Test for Moisture in the Anal sis Sam le of Coal and Coke; D 3174-73 (1979), Test for Asg in the Wnalysis Sample of Coal and Coke; D 3176-74 (1979), Ultimate Analysis of Coal and Coke; D 3178-73 (1979), Test for Carbon and Hydrogen in the Analysis Sample of Coal and Coke; D 3179-73 (1979), Test for Nitrogen in the Anal sis Sample of Coal and Coke; D 3180-74 (1979), Calculatin 8oal and Coke Analyses from As-Determined to Different bases; D 3302-74 (1980), Test for Total Moisture in Coal.

MISCELLANEOUS Standard laboratory test methods for coal and coke are discussed by Montgomer (21H). Miyazu (20H) reviewed some problems in the an&sis and testing of coal. Problems inherent in current methods of coal analysis and possible solutions using instrumental techniques are reviewed by Volborth (34H). Karr (16H) edited a book on analytical methods for coal and coal products. Thomas and Noles (3IH) reported on the equipment, procedures, and techniques used in coal liquefaction analyses. Bartle et al. (2H) reviewed 183 references on recent advances in the analysis of coal-derived products. Ulanovskii et al. (32H) reviewed procedures and experimental technology for the analysis of coal extracts. Various nuclear magnetic resonance (NMR) techniques were reviewed by Gerstein (12H),Lang et al. (17H), Petrakis and Edelheit (23H), Retcofsk and Link (25H), and Yokono (3723. Alemany et al. (IH), {chwager et al. (29H), and Yokoyama et al. (38H) used NMR to characterize coal products that were separated by gel-permeation chromatogra hy. Dorn et al. (7H) studied solvent-refined coal by elevateltem erature carbon-13 fourier transform NMR spectrometry. gait0 et al. (27H) evaluated solvents that are used for NMR analysis of solvent-refined coals. Lumpkin and Aczel(I9H) characterized coal products by using mass spectrometric techni ues. Gas chromatographymass s ectrometrytechniques (G8-MS) were used b Hayatsu et al. b5H) to characterize organic acids trappe in coals. Fishel and Longo (9H) used GC-MS to determine nitrogen heterocycles in coal liquids. Polynuclear aromatic and alihatic hydrocarbon fractions of SRC were characterized by gchultz et al. (28H) using g1as.s capillary GC-MS. St. John et al. (26H) described the field ionization and field desorptlon mass spectrometricmethods that they applied to coal research. Sturdier et al. (30H) reviewed 82 references on the analysis of organic compounds trapped in coal and coal oxidation products.

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Products of coal hydrogenation and deuteration were studied by Goldberg et al. (13H) using electron paramagnetic resonance. The behavioral characteristics of the width of the EPR signal of pyrolyzed coals was studied by Ravilov et al.

WH).

Brown et al. (3H) studied coal-derived products with gelpermeation chromatogrriphy and an on-line infrared detector. Room-temperature phosphorimetry was used by Vo-Dinh (33H) for the rapid analysis of polynuclear aromatic compounds. Likhtenshtein et al. (18H) suggested a procedure for measuring the infrared spectra of coal that is free from the distorting effects of HzO. Bubnovskaya, et al. (4H)studied the effect of the crushing of coals on their IR spectra. IR and NMR spectral analysis of low-quality coal was performed by Florea et al. (1OH). FTI[R was applied to the characterization of fractionated coal liquids by Painter and Coleman (22"). Wachowska (35H) and Wachowska et rd. (36H) studied the chemical structure of coals with reductive alkylation. Den0 et al. (6H) used oxidative degradation as a new method for elucidating the structure of coal. The use of size exclusion chromatographyfor the separation of whole coal liquids is described by Hausler et al. (14H). Drake et al. (SH)usedl Shpol'skii luminescence spectroscopy to study extracts of coal and coal-tar pitch. Camier and Siemon (5H) reviewed 37 references on the use of X-ray crystallographyto study brown and bituminous coal. Fourier analysis of X-ray sorption s ectrums was used by Fujino and Kat0 (11H) to determine t f e chemical structures of the organic constituents in coal.

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 Abstracts 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 fuel gas, natural gas, and refinery gases were included in a review by Fraser (11). The gas chromatographicanalysiis of fuel gases wag reviewed by Kogan and Markacheva (41).Kavan (21) reviewed analytical methods for town and natural gas. The determination of impurities in fuel gases by titration, gas chromatography, colorimetry, and coulometry were also discussed. A review of coke oven gas analysis was given by Manka (51) and includes analysis of sulfur compounds and hydrogen cyanide in the treated gas. Russo (SI) reviewed classical and conventional methods of liquid petroleum gas sulfur analysis. King and Magee (31) reviewed the analyriis and remote sampling of gas components from an underground coal gasification test. The monitoring of natural gas composition in piping systems by gas chromatography was reviewed by Van Rossum and Wolkotte (71).

GAS CHROMATOGRAPHY 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 Cram et al. (54 in the 1980 Analytical Reviews. This review covers only those publications directly related to gaseous fuels. A fully automated, multisample, gag chromatographic analysis of fossil fuel gases was described b y Rohler et al. (104. An automated gas Chromatographic method for the complete analysis of natural gas using a ten-port gas sampling and column-switchin valve with multi le columns was described by Johansen (7d.Coquand and Eharron (44reported the automatic monitoring of natural gas composition by chromatography. An automatic gas chromatogram reader-recorder for anal zing natural gas samples was reported by the Societe Anon. Jeoservices ( 1 4 The analysis of ligniite-derived gases by automatic gas chromatography was described by Philip et al. (94. Ganglwal et al. ( 6 4 described the automatic gas chromatographic analysis of semi-batch coal gasifier product.

Zamulinskii (15J, 1 6 4 reported an economical and rapid analysis for complex gas mixtures using two sequentially joined chromatographs. A rapid two-column chromatographic analysis of pyrolysis and methane conversion gases was described by Aref eva et al. (24. Shevtsov et al. (124 used a two-column gas chromatograph to analyze a mixture of coke oven-blast furnace and natural gases. Fuel and Flue gases were analyzed by Ruvinskii et al. (114 with a two-column gas chromatograph. The sensitivity was 0.01% for 0, N,H, and CH3 and 0.1% for CO and COD Vlckova (144 determined hydrocarbons from C1 throu h CI3 in natural gas pipelines with gas chromatography. T e gas chromatographic analysis of natural as for C I 13 hydrocarbonswas standardized by Olacsi et a f ( 8 4 with thermal conductivity and flame ionization detectors. The gas chromato raphic analysis methods for fuel gases used in iron and steefmaking were discussed by Castello t)"d Riccio (34. Sumbaev (134 analyzed the ethylene fraction from coke gas with automatic gas chromatography.

fl

SULFUR COMPOUNDS A flame photometric detector was used by Butusova et al. (5K) to determine total sulfur in natural gas by gas chromatography using the difference in signals from natural gas and high-purity methane. A report from the Szechwan Institute of Chemistry ( I K ) described the determination by flame photometry of total sulfur in natural gas using the 394-L% wavelength. Below (4K) described an apparatus for the continuousdetermination of the total sulfur content of natural gas. A special platinum catal st was used to convert organic sulfur to hydrogen sulfide. ?he use of gas chromato raphy with flame hotometric detectors was also discussecf A methoffor determining the hydrogen sulfide content of natural gas wa5 reported by Rhodes (11K) for samples containing 0.01 ppm to 5000 ppm hydrogen sulfide usin a gas chromatograph with a flame photometric detector. mass spectrometerwas used to analyze samples with more than 5OOO ppm hydrogen sulfide. Sample collection and standardization were also discussed. Galivets and Shuleshko (7K) determined low concentrations of hydrogen sulfide in purified coke oven gas photometrically. Hydrogen sulfide was determined in water gas by Wu (14K) using a colorimetric method. Gibbons (8K) described the continuous determination of EtSH, Me3CSH,MeEtS, and Et2S in natural gas using a gas chromatograph and flame photometric detector. An ultraviolet filter and a controlled reducing flame were used in the detector. Wittmann et al. (13K) determined low concentrations of mercaptans, disulfides, tetrahydrothiophene, and butanoic acid in fuel gases after absorption in alcohol solutions by simple and rapid amperometric and gas chromatographic methods. Demczak et al. (6K) reported the gas chromatographic determination of hydrogen sulfide, thiocarbonyl oxide, sulfur dioxide, and carbon disulfide in gaseous fuels using a flame-photometric detector. Price ( I O K ) described a flame photometric detector for the gas chromatogra hic determination of sulfur compounds in natural as anzliquid petroleum gas using a cool hydrogen flame an$ selective light filter. Hydrogen sulfide and total sulfur were determined by Austin and Robison (3K) in natural gas, li uid petroleum gas, stack gases, sewage gases, etc. using an e?ectrolytic titrator. The titrator can also be used to detect thiols, sulfides, disulfides, and sulfur dioxide in gases. The continuous measurement of the mercaptan sulfur contents in natural gases was reported by Herbst and Romanski (9K) using the ITTBarton sulfur titrator. A colorimetric odorant test for fuel gases was reported by Verma and Knight (12K). An infrared spectroscopicmethod was used by the Szechwan Institute of Chemistry (2K) to determine dimethyl sulfide in natural gas following the separation of hydrogen sulfide.

1

WATER VAPOR An automated apparatus for the determination of moisture content in natural gas was described and evaluated by Ratard (3L). The repeatability was of the order of 10%. A method and apparatus for the continuous monitoring of the moisture content of natural gas using a Karl Fischer titrant was given by Bozeman ( I L ) and was unaffected by contaminants. Lurvey (2L) discussed methods for determining the water ANALYTICAL CHEMISTRY, VOL. 53, NO. 5, APRIL 1981

237 R

SOLID AND GASEOUS FUELS

vapor content and hydrocarbon dewpoint in natural gases. The sampling of natural gas in pipelines was also discussed. A preferred method was discussed for determining the water vapor content in natural gas by electrolytic absorption in which water vapor was absorbed by P,O to form H9P04,and the current needed to destroy the acid by electrolysis was measured.

CALORIMETRY The calorific value of natural gas was determined by Howard (SM) using a method based upon the proportionality of calorific value to the air-fuel ratio required to maximize the adiabatic flame temperature. Clingman ( I M , 2M) used a pair of flames while measuring the ratio of combustible to combustion-supportinggases at maximum average temperatures to determine the calorific value of combustible gases, Rosko et al. (IOM) described a microprocessor-based chromatographic analysis for both the calorific value and real specific gravity of natural gas. Cuculat and Voinescu (4M) calculated the calorific value of a gas with >99 volume percent methane from gas chromatographicanalysis and found it more accurate than a calorimeter. A microflow calorimeter for enthalpy measurements in natural gas liquefaction was reported on and evaluated by Lammers et al. (8M). Kersey (7M) described the principles, operation, accuracy, and maintenance of the Cutler-Hammer recording Calorimeter. Moore (9M)described a gas calorimeter designed to produce outputs of Btu/ft3, Btu/lb, Wobbe index, and specific gravity. An infrared calorimeter was described by Fraim et al. (5M) as accurate, low maintenance, and fast responding. The round robin testing of three calorific value methods on six natural gas samples was reported by Clingman et al. (3M). The three methods were Therm-Titrator, CutlerHammer calorimeter, and gas chromato raph. Dynamic calorimetry was used by Volesky et al. ( I I b to determine the heat of fermentation in natural gas.

DENSITY The advantages of an on-line density meter and microprocessor for rapid and reliable solutions to flow and ener equations for natural gas were discussed by Agar and Ba Is ( I N ,2N). A magnetic suspension densitometer was used by Haynes and McCarty (3N) to obtain density data for liquefied natural gas with a total uncertainty of less than 0.1%. Mathematical models for predicting density within 0.1 % accuracy were also discussed. Orrit and Laupretre (5N) reported on studies directed toward the determination of the density of liquefied natural as as a function of composition and temperature. Hiza an8 Haynes (4N) reported that a magnetic suspension densimeter with com onent determination by chromatography can be used to ohain orthobaric liquid densities for the major components of liquefied natural gas and their mixtures.

P

SAMPLING The sampling and analyzing of liquefied natural gas from flowing streams was evaluated by Parrish et al. (9P). ThFee sample probes, two vaporizer designs, and ten operating variables were considered. A technique was developed by Kavan (7P) of sampling natural gas for pressure tanks with a single valve. Sampling techniques for determining the heating value of natural gas were discussed by Drake (3P). Gas sampling for in situ coal gasification was discussed by Hommert et al. (6P) and by Magee (8P). Bump and Chang (IF)reported on hi h temperature and pressure gas sampling in coal gasifiers. T t e raw roduct from coal gasification was sampled for aerosols by Earpenter et al. (2P) and for the condensible portion by Hajicek and Paulson (5P). An on-line gas sampling and analyzing system for a coal gasification reactor was described by Fuchs et al. (4P).

MISCELLANEOUS Mercury in natural gas was determined by Ratard (20Q) with an automatic detector-analyzer to a detection limit of 0.2 ng/m3. Mohnke and Hoefling ( I 7Q)described a method to preconcentrate the noble gases from natural gas prior to their analysis. Equchi and Hamada (7Q)devised a simple semiquantitative test for ammonia in fuel gases using a so238 R * ANALYTICAL CHEMISTRY, VOL. 53, NO. 5, APRIL 1981

lution of silver and manganous nitrate plus glycerine, impregnated on a support of pa er, silica gel, etc., and timin the reaction with test gases. 8arbon dioxide was determine3 in hydrocarbon pyrolysis gases by Bondarenko et al. (5Q)using gas chromatography. Analytical methods for methanol determination in natural as were evaluated b Kavan (12Q). Lakeev and Vyalkina b 4 Q ) determined metianol in natural gas by photocolorimetry after oxidation of the methanol with chromotropic acid. N uyen (18Q)described an ap aratus for determining the confensation temperature of ligit hydrocarbons in natural gas. An apparatus for determining the Wobbe index of a gas or gas mixture was reported by Krij sman (136). Combustion data for three low-Btu ases were fetermined and compared with natural gas by Waitel and Fleming (WQ)to demonstrate the feasibility of retrofitting existin burner equipment to use low-Btu gas. Grill0 (98)described t i e applications of a boiling point analyzer, including those for a natural gas plant. Operational aspects of turbine as flowmeterswere discussed by Schmittner (22Q),Schlager hIQ), and Espinosa Manero (8Q). The application of mass s ectrometry to coal gasification was included in discussionsiy Sharkey (23Q)and Zielinski et al. (264). Mass spectrometry and as chromatography were utilized by Herlan and Mayer ( 1 0 4 to analyze natural gas for higher hydrocarbons. A report from TRW (IQ)described the raw-gas compositions from the major classes of coal gasifiers including major gas constituents and contaminants, and trace element contaminants. Traces of heavy metals in German natural gas were investigated by Tunn (24Q). Instruments for liquefied natural gas s ill detection were described by Bingham et al. (4Q),Lev (15$), Hinckley ( I I Q ) , and Dewey et al. (SQ). The British Gas Corporation (2Q) described a portable gas detector. Portable flammable gas detectors were surveyed by Palmer (196). Loh (I@) described a gas detector sensitive to l % methane in air. Austin and Moen (3Q) developed an electrolytic titrator for sulfur monitoring of natural gas, hydrogen sulfide monitoring of liquefied petroleum gas, and other sulfur monitoring applications.

STANDARDS Current activities in the characterization of liquefied natural gas as related to custody transfer were outlined by Parrish et al. (3R). A standardized program of quality determination for the sampling and analysis of natural gas was outlined by Williams (4R). Izutsu and Harada (ZR)gave revisions for the standardized fuel gas analysis methods. The American Society for Testing and Materials develo s and standardizes procedures for the analysis of gaseous fueE. These standards ( I R ) are published annually. ASTM standards that have been adopted or revised during this review period include the following: D1070-73 (1979) Tests for Specific Gravity (Relative Density) of Gaseous Fuels, D1071-78a Measurement of Gaseous Fuel Samples, D3588-79 Calculating Calorific Value and Specific Gravity of Gaseous Fuels. LITERATURE CITED SOLID FUELS Sampllng and Proxlmale Analysls (1A) Allardice, D. J.; Evans, D.G. Anal. Methods Coal, Coal Prod. 1978, 1. 247-62 (Eng). (2A) Bevan, R.; Luckie, P.; Gozanl, T.; Brown, D. R.; Bozorgmanesh, H.; Elias, E. (EPRI-FP--969(VoL 4)) Jan 1979, 61 p. (3A) Bochenln, V. I. Sold Fuel Chem. (USSR) (Engl. Trans/.);10; No. 5 , 145-147 (1976). (4A) Borushko, N: I.; Krylov, R. A.; Starchik, L. P.; Kiryanov, G. I.; Novoseltsev, V. A. Zavod. Lab. 1979, 45(8), 729-30 (Russ). (5A) Brown, D. R.; Bozorgmanesh, H.; Elias, E.; Gozani, T.; Luckie, P. (ANL78-62, Pp 514-539) 1978. (6A) Brown, D.R. (EPRt-FP-989(Vol 5)) Sept 1979, 79 p. Avail. NTIS. (7A) Brown, F. V.; Jones, S. A. Adv. X-Ray Anal. 1980, 23, 57-63 (Eng). (EA) Bryers, R. W.; Blswas, B. K.; Taylor, T. E. Coal Technol ' 78 Int. Coal Utll. Conv. 1978, 2, 583-623 (Eng). (9A) Clayton, Colin Geoffrey; Wormald, Malcolm Roderic Ger. Offen. 2939817; Brlt. Appl. 78/39,011, 02 Oct 1978; 25 pp, (10A) Colombo. A.: Scholz. A. Comm. Eur. Communities. EUR 1978, EUR ' 6039, 12 pp. (Eng). (11A) Fyans, Richard L. Therm. Anal. Appl. Study 1977, 21, 5 pp. (Eng). (12A) Gold, Philip I. Avail. NTIS. From Sci Tech. Aerosp. Rep. 1978, 16(14), Abstr. No. N78-23535. '

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(2P) Carpehter, R. L.; Weissman, S. H.; Newton, G. J.; Hanson, R. L.; Royer, R. E. Report 1977, LF-58, pp 251-6; E.R.A. 4(10), 27757. (3P) Drake, C. F. Proc. Int. Sch. Hydrocarbon Meas. 1979. 54, 186-98. 14PI Fuchs. W.: Hickev. R. F.: Gibbon. G. A,: Bovce. ' , . R. E. Reoort 1978. ANL-78-62, pp 542-58; E.R.A. 4(15); 40079. (5P) Haiicek. D. R.: Paulson. L. E. Reoort 1979, ANL-79-62, .DD . 110-123: ' ERA: 5(14), 21595. (6P) Hornmert, P. J.; Beard, S. G.; Reed, R. P.; Beyeler, J. A.; Northrop, D. A. In snu 1978, z(3), 143-172. (7P) Kavan, I.Plyn 1978, 58(12), 373 (Czech); Chem. Absfr. 1979, 97,

.

41635. .

(8P) Magee, R. A. Report 1978, SAND-78-0941, pp 269-279; E R A . 4(5), 9476. (9P) Parrlsh, W. R.; Arvidson, J. M.; LaBrecque, J. F. Report 1978, NBSIR78-887; Order No. PB-289938, 201 pp. Avail. NTIS.

( l a ) Anon. (TRW, mc.) Report 1979, METC-8085-T2. 91 pp. Avail. NTIS. (2Q) Anon. (British Gas Corp.) Fr. Demande 2 430 611 (GI. GOIN27/14), 01 Feb 1980. (3Q) Austin, R. R.; Moen, A. Proc. Int. Sch. Hydrocarbon Meas. 1979, 54, pp 169-73. (4Q) Blngham, G. E.; Glllespie, C. H.; McQuaid, J. H. Report 1979, UCRL83317 (CONF-790887-1), 21 pp, Avail. NTIS. (5Q) Bondarenko, L. L.; Fatkulllna, A. F.; Zakharova, N. V.; Ellzarova, A. D. Khim. Prom-st., Ser.: Metody Anal. Kontrolya Kach. Prod'. Khim. Promsfi. 1980, (3), 1-4 (Russ); Chem. Abstr. 1980, 93, 75202. (6Q) Dewey, C. F., Jr.; Flint, J. H.; Russ, R. M.. Jr.; Dezmelyk, R.; Fenner, R.; Stein, M. I. Report 1979, DOElEV-0036. Report I,32 pp; E.R.A. 4(18), 47365 ..

(7Q) Eguchi, H.; Hamada. H. Jpn. Kokal Tokkyo Koho 78 110 892 (Cl. GOlN31/22), 27 Sep 1978. (8Q) Espinosa Manero, R. Ing. Quim. (Madru) 1979, 77(125), 61-90 ISDank Chem. Absfr. 1980. 93. 10452. (9d) ' G r i h P. H. Anal. Instrum. 1978, 76,73-80. (loa) Herlan, A.; Mayer, J. Gas- Wasserfach: GaslErdgas 1978, 179(8), 364-70 (Ger); E R A . 4(8), 18006. (11Q) Hinckley, E. D. Reoort 1979, USCG-D-71-79 (Order No. AD-A078494), 85 pp. Avail. NTIS. . (12Q) Kavan, I. Sb. Pr. UVP 1978, 36, 213-40 (Czech); Chem. Absfr. 1980. 93. 75160. - -(13Q) Krljgsman, A. Eur. Pat. Appl. 8 151 (Cl. GOlN33100), 20 Feb 1980. (14Q) Lakeev, V. P.; Vyalklna, G. V. Podgot. Pererab. Gaze Gazov. Kondens. 1978, (7), 8-12 (Russ); Chem. Absfr. 1979, 97, 142852. (15Q) Lev, Y. J . Phys. E 1979, 72(8), pp 694-8. (16Q) Loh, J. C. Ger. Offen. 2738867 (CI. G01N27/12), 22 Mar 1979. (17Q) Mohnke, M.; Hoefling, R. Z . Angew. Geol. 1978, 24(4), 166-8 (Ger); Chem. Abstr. 1978, 89, 156820. (I8Q) Nguyen, V. L. Ger. Offen. 2933825 (Cl. GOlN25/12), 06 Mar 1980. (190) Palmer, K. N. Ber. Int. Koiloq. VerhuetungArbeksunfaellen Berufskr. Chem. Ind. 1976, (3), pp 435-50 (Eng). (20Q) Ratard, M. D. Gar Aulourd'hui 1978, 702(6), 199-204 (Fr); Chem. Abstr. 1978, 89. 217630. (21Q) Schlager, M. Gas-Wasserfach: GaslErdgas 1978, 7 79(2), 61-3 (Ger); E R A . 4(2), 2520. (22Q) Schmlttner, D. Gas- Wasserfach: GaslErdgas 1978, 779(2), 51-6 (Ger); E R A . 4(2), 2519. (230) Sharkey, A. G., Jr. "Carclnogenesis: a comprehensive survey"; Freudenthal, R.; Jones, P. W., Eds.; Raven Press: New York, 1976, Vol. I,pp 341-7. (24Q) Tunn. W. Erdoel Kohle 1976, 29, 211 (Ger); E R A . 3(22), 52062. (25Q) Waibel, R. T.; Fleming, E. S. Report 1979, FE-2489-48, 251 p. Avail. NTIS. (26Q) Zlelinskl, R. E.; Seabaugh, P. W.; Martin, J. W.; Libertore, A. J. Report 1978, SAND-78-0941, pp 367-78; E.R.A. 4(5), 9420.

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Standards ( I R ) ASTM Standards, Part 26, Philadelphia, Pa. 1979.

(2R) Izutsu, W.; Harada, S. Nippon Gasu Kyokaishll979, 32(5), 41-9 (Japan); Chem. Abstr. 1979. 91, 160127. (3R) Parrish, W. R.; Brennan, J. A.; Slegwarth, J. D. Oper. Sect. Proc.-Am. Gas Assoc. 1978, T1243-Tl249. (4R) Williams, M. L. Oper. Sect. Proc.-Am. Gas Assoc. 1979, T/377-T/ 382. ANALYTICAL CHEMISTRY, VOL. 53, NO. 5, APRIL 1981

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