149345N(1975), (P90) Spectroscopic Determination of the Molecular Weight and Degree of Hydrolytic Degradation of Polyamides, Bershtein, V. A,, Egorova, L. M., Kabrits, E. I., Zh. Prikl. Spektrosk., 23,254-9( 1975) (Russ), Chem. Abstr., 83, 164746N(1975). (P9 1) Measurement of Molecular Orientation in Uniaxially Drawn Polyacrylonitrile Films, Siesler, Heinz W., Makromol. Chem., 176,2451-8(1975) (Ger), Chem. Abstr., 83, 180084A(1975). (P92) Analysis of PVC Compounds, Helmuth, Josef. Polim. Vehomarim Plast., 3,7-8( 1973) (Hebrew). Chem. Abstr., 83, 1936870(1975). (P93) Quantitative Analysis of Cation-Exchange Resins by Infrared Spectrophotometry and Pyrolysis-Gas Chromatography, Parrish, J. R., Anal. Chem., 47,1999-2003(1975) (Eng). Chem. Abstr., 83. 194166R(1975). (P94) Different Types of Hydrogen in Coal anId its Derivatives Determined by IR and High-Resolution NMR Spectroscopy. II, Yokoyama, Susumu, Ito, Mitsuomi, Takeya, Gen, Nenryo Kyokai-Shi, 54,340-8(1975) (Japan), Chem. Abstr., 83, 196085N(1975). (P95) Profiles of Hydrogen Stretching IR Bands of Molecules with Hydrogen Bonds. Stochastic Theory. I. Weak and Medium Strength Hydrogen Bonds, Bratos, S.,J. Chem. Phys.. 63.3499-509( 1975) (Eng), Chem. Abstr., 83, 199568Q(1975). (P96) Fourier Transform Infrared Study of Plasticized and LJnplasticized Poiy(Vinyi Chloride), Tabb, D. L.. Koenig, J. L., Macromolecules, 8.929-34(1975) (Eng), Chem. Absfr., 83, 2067410(1975).
IR Combined with Separallons ( S l ) Combining Infrared and Gas Chromatography for on-Line Analysis, Penzias, G. J., Boyle, M. J., Amer. Lab., 53-9(1973) (Eng), Chem. Abstr., 80, 1011lC(1974). (S2) Use of an infared Laser in a Detection System for Liquid Chromatography, Freeman, Norman K.. Upham, Frank T., Windsor, Alfred
A,, Anal. Left., 6,943-50(1973) (Eng), Chem. Abstr., 80, 336130(1974). (S3) Reproducibility of Molecular Weight Measurements b GPC [Gel Permeation Chromatography[ with Infrared Detectors, Ross, J. H., Jr., Shank, R. L., Advan. Chem. Ser., No. 125,106-16(1973) (Eng), Chem. Abstr., 80, 60321S( 1974). (S4) High Speed Liquid Chromatographic Separations of Thermally Labile High Energy Compounds. Ii. Infrared Spectral Characterization of Micropreparative HPLC Fractions, Juhasz. Arpad A,, Doall, J. Omar, U. S. Nat. Tech. Inform. Serv., AD Rep., 1973, No. 769713/9GA, 24 pp., Eng. Avail. NTIS, Chem. Abstr., 80, 85368A(1974). (S5)Spectral Characterization of Micropreparative HPLC (High Performance Liquid Chromatography) Fractions, Juhasz. A. A,, Doali. J. Omar, Rocchio, J. J., Amer. Lab., 8,23-4, 26, 28-9(1974) (Eng), Chem. Abstr.. 80, 115761T(1974). (S6)Coupling of a Gas Chromatograph [with an Infrared Spectrometer], Dijkstra, G., Lab Instrum., 10,19-20, 23(1974) (Neth), Chem. Abstr., 80, 115763V(1974). (S7) GC [Gas Chromatography]-IR System for Identification of Multicomponent Mixtures, Mercaldo, Frederick D., Amer. Lab., 6,63-7(1974) (Eng), Chem. Abstr., 80, 127883X(1974). (S8)Infrared Spectrometer Coupled with a Gas Chromatograph, Renema, J., Lab Instrum., 10,111-12, 115(1974) (Neth), Chem. Absfr., 81. 85472A( 1974). (S9) Infrared Spectroscopic Identification of Micro Amounts of Thin-Layer Chromatographically Separated Substances, Adrian, P.. Beckman Rep., 50-4(1974) (Ger), Chem. Abstr.. 81, 116698K(1974). (S10) Direct Measurement of the Infrared Spectra of Compounds Separated by Thin-Layer Chromatography, Percival. Carlisie J., Griffiths, Peter R., Anal. Chem., 47,154-6(1975) (Eng), Chem. Abstr., 82, 67896H(1975). ( S l l ) Convenient Method for Collecting Gas Chromatographic Effluents for Microscale infrared Spectrophotometric Analysis in the Gas Phase, Norin, K. Harald, Analyst (London), 99,717-23(1974) (Eng), Chem. Abstr., 62, 92707E( 1975). (S12) infrared Fourier Transform
Spectrometry of Gas Chromatography Effluents, Azarraga, Leo V.. McCall, Ann C., Environ. Plot. Techno/. Ser., 1974, EPA-660/2-73-034, 61 pp., Eng. , Chem. Absfr.. 82, 105985W(1975), (S13) Simple Directly Combined Gas Chromatographic-Infrared Spectrometric System for Identification of Low Molecular Weight Hydrocarbons, Louw, C. W., Richards, J. F., Appl. Spectrosc.. 29,15-24(1975) (Eng), Chem. Abstr., 82. 115513E(1975), (S14) On Line Infrared Identification of Gas Chromatography Effluents, Katlafsky, B., Pietrich, M. W., Appl. Spectrosc., 29,24-8(1975) (Eng), Chem. Abstr., 82, 1326012(1975). (S15) Interrupted High-speed Liquid Chromatography wlth Simultaneous Spectroscopic identification, Dimov, N. P., Dokl. aBolg. Akad. Nauk, 27,1407-9(1974) (Eng), Chem. Abstr., 82, 149021H(1975). (S16) Direct Combination of Intensive Liquid Chromatography with Ultraviolet and Infrared Spectrometry, Decsy, Z., Giuck, L., Belafi-Rethy, K.. Magy. Asvanyolaj- Foldgaz Kiserl. Inter. KOA, 15,49-53(1974) (Hung), Chem. Abstr.. 83, 711608(1975), (S17) Analysis of Microgram Quantities of Organic Vapors by Combined Capillary-Column Gas Chromatography and Vapor Phase Infrared Spectrometry, Brady, Robert F., Jr., Anal. Chem., 47,142541975) (Eng), Chem. Abstr., 83, 107974M( 1975). (S18) Liquid Chromatography/lnfrared Spectroscopy on-Line Analysis, Kizer, Kenneth L., Mantz, Arian W.. Bonar, Laurence C., Am. Lab., 7,856, 88,90-2, 94, 96-7(1975) (Eng), Chem. Abstr., 83, 141479P(1975). (S19) Spectral Characterization of Micropreparative HPLC [High Performance Liquid Chromatography] Fractions, Juhasz, A. A,, Doali, J. Omar, Rocchio, J. J., lnt. Lab., 21-2, 24, 26(1974) (Eng), Chem. Absfr., 83, 141485N(1975). (520) GC [Gas Chromatography]-IR [Infrared] System for Identification of Multicomponent Mixtures, Mercaido, Frederick D., lnt. Lab., 75-6, 79-80(1974) (Eng), Chem. Abstr., 83, 157519N(1975). (S21) Infrared Detection of Polymers in Gel Permeation Chromatography, Dawkins. John V., Hemming, Malcolm, J. Appl. Polym. Sci., 19,3107-18(1975) (Eng), Chem. Absfr., 83, 193926B(1975).
Light Absorption Spectrometry’ D. F. Boltz Wayne State University, Detroit, Mich. 48202
M. G. Mellon Purdue University, Lafayetfe, Ind. 49707
This sixteenth consecutive review of light absorption spectrometry capsulates the achievements in this analytical field from November 1973 through November 1975, primarily as documented by Chemical Abstracts, and extends the continuous coverage of the literature of this topic for a 46-year period. The subject matter has been classified under the headings of Chemistry, Physics, and Applications as in previous reviews (72, 340, 341). Thus, the emphasis will be on chemical reactions, measurement of radiant energy, and analytical methodology. Because of the impossibility, as well as the inadvisability, Reprints available from R i c h a r d versity, Detroit, M i c h . 48202.
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B.
Hahn,
Wayne State Uni-
ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
to document all publications related to light absorption spectrometry, abstracts and papers have been examined carefully in an attempt to select and present succinctly those developments of most probable interest to analytical chemists. The authors recognize their fallibility in omitting some references. In the opinion of these reviewers, the publication rate of papers dealing with light absorption spectrometry has finally reached a plateau, especially with respect to papers of primary interest to analytical chemists. Particularly in the United States, there has been a noticeable diminution in the number of fundamental studies on new spectrophotometric methods. Books related to light absorption spectrometry follow: “Photometric Analysis, Methods of Determining Organic
The review on Light Absorption Spectrometry has been written by David F. Bolt2 and M. G.Mellon since 1956. In the years before 1956, Dr. Mellon prepared the review alone. This is the last review by these outstanding contributors. Dr. Bolt2 died unexpectedly on January 9, 1976, after he had prepared the bulk of the material for this issue’s review. Dr. Mellon has asked the editors to make this his last contribution. The editors and readers of ANALYTICAL C u m i s m y owe a huge vote of thanks to these workers for the many, many hours of dedicated work that has gone into the preparation of these biennial reviews over the past 20 years. Brief biographies of Drs. Boltz and Mellon appear below. Davld F. Boltz was professor of chemistry at Wayne State University and also a scielice advisor for the Detroit District Laboratory of the Food and Drug Administrations He received his B S from the University of Wisconsin in 1938, hLs M.S. from the University of Missouri-Rolla in 1940, and his Ph D. in analytical chemistry from Purdue University in 1946 His particular fields of interest were in ultraviolet and light absorption spectrometry, analytical separation methods, heteropoly chemistry, and atomic absorption spectroscopy. He was the author of many research papers, chapters in books, and reviews. In 1971, Dr. Boltz received the first Anachem Fellow Award from the Association of Analytical Chemists and the Faculty Research Award from the Sigma Xi chapter at Wayne State University. He was a member of the Advisory Board of ANALYTICAL CHEMISTRY and also served on the editorial board of Analytical Letters. Professor Boitz was member of ACS, SAS. Association of Analytical Chemists, Sigma Xi, Alpha Chi Sigma, and Phi Kappa Phi. He won the 1975 Anachem Award which was presented to him at the 2nd FACSS meeting in Indianapolis in October 1975. Melvin Guy Mellon, on the Purdue faculty since leaving Ohio State University with a PhD in 1919, has been one of the moving factors in the advancement of analytical chemistry in this country. He has published many papers, of which half have been on colorimetry. He has also written several textbooks, of which “Chemical Publications” has been widely adopted in chemical literature courses. In 1952 he was given the Fisher Award in Chemistry for his work in colorimetry and spectrophotometry. He was given the Anachem Award by the Association of Analytical Chemists in 1953, the Austin M Patterson Award in Chemical Documentation in 1957, and the annual Medal Award of the Society for Applied Spectroscopy in 1965
Compounds,” 2nd ed. (285);“Colorimetric Chemical Analytical Methods,” 8th ed. (540); “Organic Reagents in Photometric Analysis” (536);“Handbook of Photometric Analysis of Organic Compounds” (254); “Inorganic Absorption Photometry” (324); and “Photometric Analysis, Methods for Determining Nonmetals” (37).
CHEMISTRY The search for better methods continues to result in numerous investigations on the suitability of a reagent to determine a specific constituent in a particular sample. In certain cases, there has been a systematic study of reagents with modified functionality and/or structure in an endeavor to develop reagents of improved sensitivity or specificity. There has been a more extensive use of mixed ligand complexes (421) and basic dyes (312) in spectrophotometric analysis. The formation of colored extractable ternary ion-associate complexes has also increased in popularity. In this section of the review, we shall consider primarily the chemistry involved in the development of suitable colored systems and new reagents or color-forming reactions. Metals. 2,2’-Diquinoxaline has been proposed as a new reagent for tin(I1) (46). As a result of a spectrophotometric study of complexes formed by tin(1V) and either o-diphenols or o - hydroxyquinones, gallein or dihydroxyfluorescein have been recommended. These reagents give extractable colored complexes with detection limits of 1.5 wg and 0.2 wg, respectively ( 2 ) . New reagents forming metal complexes exhibiting molar
absorptivities larger than 105 have been reviewed and include 4(2-pyridylazo)- 1,3-diaminobenzene (480). Twentyfive nitrosophenol and nitrosonaphthol derivatives have been examined as potential chromogenic reagents and 2nitroso-5-dimethylaminophenol was recommended for the determination of iron in water (546). The formation and extraction of tris[3(2-pyridyl)-5,6-diphenyl-1,2,4-triazine] thiocyanate is the basis of a sensitive method ( e = 2.4 X lo4) for determination of iron in acidic solution (109). T h e interference due to iron(II1) in the determination of iron(11) using the 1,lO-phenanthroline method can be eliminated by complexation with nitrilotriacetic acid (159) or with fluoride (523). Thirty-nine new ferroin compounds were investigated as chromogenic reagents for iron(II), copper(I), and cobalt(I1) and the spectral properties of the corresponding complexes compiled. One compound, 2,6-bis[3(4-methyl-2-pyridyl)-1,2,4-triazolin-5-y1] pyridine can be used in the determination of iron giving a molar absorptivity of 3.2 X lo4 (464). In a comparison of stilbazo, eriochrome cyanine R, and catechol violet as chromogenic reagents for the determination of aluminum in water, catechol violet was the most suitable (140). 2-(2-Pyridylazo)-5-diethylaminophenol (PADAP) and three derivatives (Br-PADAP, C1-PADAP, Br-(diMe)’-PADAP) have been investigated as color-forming reagents. These reagents are generally about twice as sensitive as PAR in the determination of transition metals. The Br-PADAP is a rather specific, sensitive reagent for uranium(V1) (250). A new specific reagent for copper(II), under controlled conditions, is 6-phenyl-2,3-dihydro-as-triazine-3-thione (PDTT) which forms a 1:2 Cu-PDTT complex extractable into chloroform (321). Mercury(I1) also can be determined spectrophotometrically as a 1:4 mercury(I1)-PDTT complex (322). The formation of a ternary complex having a 1 5 2 molybdenum(V):thiocyanate:rhodamine B composition is the basis of a spectrophotomecric method for molybdenum (206). A blue ternary complex of arsenazo I, plutonium(IV), and hydrogen peroxide with a molar absorptivity of 4 X 104 has been described (411). Ion-associates of methyl orange, iron(II), and either 2,2’-bipyridine or 1,lO-phenanthroline have been investigated spectrophotometrically (226). The ethyl ester of rhodamine S has been investigated as an ion-associate forming reagent for extraction photometric methods for platinum(IV), silver(I), mercury(II), copper (I), antimony(111) gold(III), thallium(I), tellurium(IV), and indium(III), (71). Benzothiazolyl (2’-azo-6)4-methylphenol and three derivatives react with thallium(II1) to give colored complexes (204). 2-Nitroso-5-diethylaminophenol is a new sensitive reagent for cobalt ( 6 = 6.0 x lo4) (545). Dimedone oxime forms a yellow complex with cobalt in basic solution and can be extracted from acidified solution with methyl isobutyl ketone and is a specific reagent for cobalt (55). Carboxy nitrazo and 2,7-bis [(3-sulfophenyl)azo]- 1,8dihydroxynaphthalene are sensitive, selective reagents for the alkaline earths with the use of auxiliary complexants and aqueous-organic media (416). Eriochrome black T, solochrome black 6BN and calmagite are satisfactory reagents for molybdenum(V1) and erio B T and solo 6BN are suitable for tungsten(V1) (363). Orthanyi B, 2-(2-sulfophenylazo)-7-phenylazo-1,8-dihydroxy-3,6-naphthalenedisulfonic acid, gives color reactions with cerium, lanthanum, praesodymium, and neodymium ions but not with the other rare earths (271). Six platinum metals (Ru, Rh, Pd, Os, Ir, Pt) have been separated on a Weisz ring-oven and determined semi-quantitatively by visual ring-colorimetry following the application of appropriate chromogenic reagents (261). Spectrophotometric methods for bismuth using organic reagents have been reviewed (36). Nonmetals. Sulfonated alizarin fluorine blue forms a very soluble complex with lanthanum(III), which is an improved reagent for fluoride (306). An improved procedure for the purification of sulfonated alizarin fluorine blue has been described (305). The sequential determinations of chloride, bromide, and iodide are possible by extracting the corresponding mixed ligand complexes of mercury( 11) and 10, methylthymol blue with zephiramine a t pH 7.0,8.5, into chloroform and measuring the absorbance of each extract at 646 nm (379). Chloride catalyzes the reduction of ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
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nitrate to nitrite which reacts with chromotropic acid to give a colored product (6). A,N-chlorosuccinimide solution stabilized with excess succinimide has been recommended as a substitute for chloramine-T or bromine water in the oxidation of cyanide to cyanogen halide in the determination of cyanide. Pyridine solutions of barbituric acid or 2,4-quinolinediol have been used as stable coupling reagents (300). Oxidative anions (IOs-, IO4-, Fe(CN)s3-) can be determined by measuring the absorbance of the oxidation product of N,Nbis(P-hydroxypropy1)-o-phenylenediamine (500). The formation of molybdosilicic acid has been studied criticallv and other conditions than those initiallv DroDosed by Stri;kland for the a and (3 forms have been fbimdated. Thus, a-molybdosilicic acid forms at pH 3.8 to 4.8 and the 0-molybdosilicic acid forms a t pH 1.0 to 1.8 (554). 1-Phenyl-5-methyl-3-pyrazolidinoneis another suitable reductant for molybdophosphoric acid at low acidities in forming the heteropoly blue complex (132). The positive interference of mercury(I1) in the heteropoly blue method for phosphate utilizing ascorbic acid and potassium antimonyl tartrate can be eliminated by the addition of metabisulfite and thiosulfite (542). In studying seven derivatives of 2,3,7-trihydroxy-6-fluorone as reagents for tellurium(IV), it was concluded that 9,9’[methylenebis(6-hydroxy-rn-phenylene) bis [2,3,7-trihydroxy-6-fluorone] was the best reagent (374 . Organic Constituents. Aromatic hydroxy compounds react with cerium(1V) in the presence of hydroxylamine to give a stable colored complex exhibiting broad maximum absorbance in the 330- to 500-nm region (108). A new method for carboxylic acids is based on the formation of hydroxamic acid using dicyclohexylcarbodiimide and hydroxylamine with subsequent measurement of the absorbance of an iron(II1) hydroxamate complex (258). Oxidative coupling of p-phenylenediamines with phenols with the ultimate formation of an indoaniline dye has been used to determine phenols and p-phenylenediamines (118).
1
Simultaneous Spectrophotometric Determinations. Formaldehyde and acrolein are determined by measurement of absorbances a t 420 and 575 nm following reactions with chromotropic acid (51 7). Tryptophan and tyrosine have been determined simultaneously following nitration and alkali treatment (211). Primary and secondary amines react with fluorescamine to form pyrrolinones and aminoenones with characteristic absorbance maxima in the 380410 nm and 300-320 nm regions, respectively (549). Iron(II1) and aluminum(II1) form colored complexes with o-hydroxy hydroquinonephthalein having absorbance maxima at 605 and 305 nm, respectively, so that a simultaneous determination is possible (167). Simultaneous spectrophotometric determinations of metals in binary mixtures of iron-titanium, iron-uranium, molybdenum-titanium, and molybdenum-uranium using pyrocatechol have been described (367). Iron(I1) and copper(I1) (64);gold(II1) and copper(I1) (63); gold(II1) and palladium(I1) (61); and palladium(II), gold(III), and copper(I1) (62) can be determined simultaneously using syn- phenyl-a-pyridyl ketoxime and extracting the complexes into chloroform. The simultaneous spectrophotometric determination of palladium and platinum uses 1,4-diphenylthiosemicarbazide (440). Cobalt and nickel have been determined simultaneously using thiotropoline (504) as reagent. Titanium, vanadium, and iron can be determined by adjustment of pH, addition of complexant, and the measurement of absorbance at two wavelengths (510).
PHYSICS Topics related to the measurement of radiant energy and instrumentation are included in this section of the review. The apparent deviation from Beer’s law for certain metaldye complexes in the presence of micelle-forming reagents is attributed to a bathochromic shift (506). Errors in absorbance measurements due to the use of nonmonochromatic radiant energy has again been thoroughly examined (11, 12). Factors affecting the precision of measuring absorbances have been delineated (453). The importance of cell positioning, maintaining clean optical surfaces, selection of spectral band width, and selection of amplifier gain were stressed. 218R
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ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
The theory and applications of diffuse reflectance spectrometry in color measurement have been reviewed (111). The precision of direct reflectance measurement of (TLC) test-strips for the determination of nickel has been ascertained with a relative precision of 3.2 to 4.6% for the 10-100 ppm concentration range being achievable (263). The principles and applications of dual-wavelength spectrometry (481 ) and derivative spectrometry (207,507) have been discussed. In evaluating the precision of differential spectrophotometry, an equation was developed for the transmittance ratio method that includes factors for the instability and sensitivity of the spectrophotometer (281). Differential spectrophotometric measurements are recommended not only in determining highly concentrated solutions but also when the color forms slowly or is subject to fading so that errors are minimized (70). A rapid scanning spectrophotometer employing wavelength modulation and a new optical system has been used in derivative spectrophotometry (507).
The applicability of TV-type multichannel detectors (522) and silicon target vidicon tubes as detectors (344, 345) in light absorption spectrometry have been discussed.
The hardware and apparatus associated with the use of an on-line digital computer for the acquisition of microsecond scan spectra and the application of the real-time system of the determination of spectral and kinetic data of a photochromic compound have been described (346). The KBr disk technique has been used in determining the visible spectra of transition metal complexes with good correlation with reflectance spectra for complexes containing no water and for undehydrated hydrates (435). Dyesensitized continuous photochemical analysis in which a substrate compound is oxidized by a photo-excited dye has been discussed in respect to experimental parameters (580).
Spectrophotometric methods for the determination of formation constants by the equimolar molar method (81) and by using a computer program (304) have been discussed. The formation constants of metal complexes and acids (317); of zinc complexes with semi-xylenol orange (595); and the complexes of cobalt(II), nickel(II), copper(11),and zinc(I1) with semi-methylthymol blue (594) and methylthymol blue (593) have been determined spectrophotometrically. Spectrophotometers. Innovative modifications in spectrophotometer design continue to be made with many new and up-dated commercial instruments having become available in this past biennium. Spectrophotometers featuring automatic compensation for dark current or background (579), a rapidly pulsed broad spectrum, flash tube facilitating use of either small samples or very dilute solutions (228); a memory device for storing calibration information and automatically correcting base line (583); and alternating beams which pass through three channels (one transparent, one of known absorbance, one of unknown absorbance in order to minimize source, detector, and other instrumental errors (129) have been described. Bausch and Lomb have introduced the Spectronic 2 1 series of low cost visible and UV-visible spectrophotometers featuring 10-nm spectral band width, solid state electronics, and a 200- to 1000-nm range (53). Hitachi has added the 100 series of single beam spectrophotometers offering spectral band widths of 7.5 nm, or 2 nm, a range of about 200 to 900 nm and a variety of accessories (218). A new Zeiss spectrophotometer, PM6, has a grating double monochromator with a spectral band width of less than 2 nm. Several modified models of this instrument are available that are especially applicable to kinetic, substrate, and repetitive measurements (220). The Zeiss P M 2 series are less expensive UV-visible spectrophotometers with numerous options and accessories (94). The Gilford Model 250 with automatic cuvette positioning and 0-3 absorbance range is especially applicable to enzyme kinetic studies (181). The Unicam SP series of spectrophotometers also offer a variety of optional features (438). The new Varian Cary 17 D model features a 5-digit readout, computer capability, and expanded recorder capabilities (566). Beckman has added a Model 26 UV-VIS model with an extended (190-900 nm) wavelength range (54). The GCA/McPherson 707 D spectrophotometer features modular construction, signal aver-
Table I. Spectrophotometric Methods for Metals Constituent
Materia 1
Method or reagent [wavelength; molar absorptivity, o r concentration range]
Ref.
Ag
... ... ... ... ...
Catalytic oxidn. of bromopyrogallol red by S,OS2- 1,lO-phenanthroline (activator) [500; 0.2-20 nglml] Thiodibenzoylmethane (C,H,) [420; 1.07 x 10'1 Indirect; tris(2,Z'-bipyridine)iron(II) tetraphenylborate [ 552; 5-50 ppm] 4-(2-Pyridylazo)resorcinol [ 510; 2.0 X l o 4 ] Ferron, cetyltrimethylammonium chloride Xylenol orange Pyrocatechol violet, ethyltridodecylammonium bromide (BuOAc) [597; 8.4 X 10'1 SPADNS [590; 0.05-0.6 ppm] Chromazurol S, zephiramine [620; 1.15 X 10'1 8-Quinolinol (CHC1,) Quercetin, antipyrine [419; 4.92 X l o 4 ] Catechol violet [580; 6.3 X l o 4 ] Rhodanine, pyridine [515; 3.8 X l o 4 ] Maxilion blue GRL-AuC1,- (C,H,) Victoria pure blue BO-AuG1,- (C,H,) [635; 0.2-2 ppm] p-Dimethylaminobenzylidene rhodanine (PhNO,) Pinacyanol (C,H,) [610; 8.7 x 10'1 Astrazon FG(C,H,) [530; 7.2 X 10'1 Dithiodiantipyrylmethane [370; 3.5 X l o 4 ] Sodium azide, methylene blue (CHCl,) [653; 1 X l o 5 ] Rhodamine B (PhMe) [568; 9.06 x 10'1 Arsenazo I11 [650; 3.65 x 10'1 Chromazurol S, hexadecyltrimethylammonium I1 salt (BuOH) [596; 5.85 x l o 4 ] Methylxylenol blue Benzoylacetone (CHCl, ); Ti(IV), fluoride, H,O, Bi14-, Bu,PO,(C,H,) [370; 5.4 x l o 4 ] Pyronine G, iodide (C,H,-MeCOEt) [530; 3 x l o 4 ] 5-Mercapto-3(2-pyridyl)-1,3,4-thiadiazole-2-thione (CHCl,) [ 340; 2.9 x l o 4 ] Dinitrohydroxyazo I11 [630; 1.7 x l o 4 ] Papaverine-Bi1,- (CHCl,) [490; 1.07 X l o 4 ] Dithiopyrylmethane [535; 1.26 X l o 4 ] 3-Mercapto-4-phenyl-5-anilino-l,2,4-triazole (CHC1, ) Quinoxaline-2,3-dithiol [490; 3.73 x l o 4 ] Arsenazo I11 [650; 4.40 x l o 4 ] 2,3,4-Trihydroxyacetophenone [ 540; 3.55 x l o 3 ] 2-(2-Hydroxy-l-naphthylazo)2'-hydroxy-5'-methylazoxybenzene (CCl,) Glyoxal bis( 2-hydroxyanil) Antipyrylazo I11 [605; 2.15 X l o 4 ] Arsenazo I1 [ 575; 0.2-2 ppm j l-Benzoxazolyl-3,5-diphenyl formazan [ 610; 4.67 x l o 4 ] 2-(6-Bromo-2-benzothiazolylazo)-5-diethylaminophenol (CHCl,) r570: 8.38 X 1041 Thiodibenzoylmethane [400; 3 X l o 4 ] Arsenazo 111, iodide, allyl alc. [600; 3.85 X l o 4 ] 6-(Benzothiazol-2-ylazo)-2,4-dichlorophenol [ 550; 3.88 X l o 4 ] 4-Dimethylaminoazobenzene-4'-arsonic acid [490; 10-450 ppm] Tetramethyl-0-tolidine [470; 2.8 X l o 4 ] Arsenazo I11 1-(Z-Pyridylazo)-Z-naphthol, Triton X-100, sodium dodecylbenzene sulfonate ~ 6 2 01.90 ; x io4] 2-Nitroso-5-dimethylaminophenol [ 530; 3.1 X l o 4 ] Monothiobenzoic acid (CHCl,) Bis(thiosalicy1idene)ethylediamine [ 470; 6.09 X l o 3 ] 0-Dithionaphtholic acid [535; 5.5 x l o 4 ] 5-Chloro-7-iodo-8-quinolinol [ 430; 9.35 x l o 3 ] Picraminazo-4-cyclohexylresorcinol (CHC1,) [ 555; 2.8 x l o 4 ] 1-Napthamide oxime (Me,CHCH,OH) [581;4.4 x l o 3 ] 2-Amino-3-quinoxalinethiol [ 428; 3.78 X l o 4 ] Ferrozine [550; 4.64 X l o 3 ] Sulfosalicylic acid [325; 2.67 X l o 3 ] 3-Hydroxypicolinealdehyde azine [ 545; 3.04 x l o 4 ] Thiocyanate, malachite green (CC1,-cyclohexanone) [ 630; 8.6 x l o 4 ] 7-Nitroso-8-hydroxyquinoline-5-sulfonic acid [ 525; 1.15 x l o 4 ] -5-(diethy1amino)phenol[ 580; l o 5] 2-[ (5-Chloro-2-pyridyl)azo] Di-2-pyridylketone-2-pyridylhydrazone [ 480 ; 3.2 X lo43 2,2'-Dipyridylketoxime (CHC1,) 4-Nitroso-5-hydroxy-2,1,3-benzothiadiazol 5-(3,5-Dichloro-2-pyridylazo)-2,4-diaminotoluene [ 590; 1.38 x l o 5] 4-(2-Pyridylazo)-rn-phenylenediamine[ 555; 8.6 x l o 4 ] Thiovioluric acid [ 580; 0.05-0.5 ppm] 4-(5-Bromo-2-pyridylazo)-1,3-diaminebenzene 2-Nitroso-5-dimethylaminophenol 2-Nitroso-5-dimethylaminophenol [456; 6.0 x lo']
360
A1
*.. *.. ...
... Alloys Glass Water Au
Ba Be
... ... *.. ... ... ... ... ... Tellurium ...
...
*..
Alloys
... ... ...
... ... Lead alloy' Steel
'
... ...
Ca
...
... ... ... ...
Cd
..
*
...
...
Ce
co
Steel Steel
... ... ...
... ...
... ... ... ... ... ... Pharmaceuticals Steel Steels Nickel Rocks, meteorites Uranium salts Steel
-
ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
361 339 155 191 541 487 43 378 209 106 140 308 117 116 76 39 415 137 297 292 342 233 561 337 187 409 89 235 520 138 101 107 342 125 582
484 82
240 266 205
465 343 31
148 232 85 57 7 359 16 459 189 393 98 357 392 295 227 127 29 1 237 202
567 221
145 483 323 154 275 358 545 219R
Table I (continued) Constituent
Material
Method or reagent (wavelength; molar absorptivity, or concentration range]
cr
...
1,2-Diaminocyclohexanetetraaceticacid, trioctylmethylammonium chloride (CHC1, 1 Diphenylcarbazide, trioctylmethylammonium chloride (CHC1, ) Glycine thymol blue [570; 2.2 x l o 3 ] 1,2-Propylenediaminetetraaceticacid PAR, tetradecyldimethylbenzylammonium base [ 540; 4.7 x l o 4 ] Catalytic oxidn., hydrogen peroxide, o-dianisidine Arsenazo I11 r610; 2.6 X l o 4 ) O(III)-EDTA 6-Phenyl-2,3-dihydro-as-triazine-3-thione (CHCl,) [ 500; 4.98 x IO3] LIX 64N (CCl,) 1-(2-Pyridylazo)-2-phenanthrol [ 560; 3.0 x l o 4 ] 1,2-Propylenediaminetetraaceticacid N-Methylaminothioformyl-N‘-phenylhydroxylamine [ 430; 2.46 X l o 4 ] 2-Thiophenealdehyde 2-benzothiazolylhydrazone (C,H,) [422; 4.4 X l o 4 ] 1-Naphthaldehyde-2-benzothiozolylhydrazone(C,H, ) [422; 4.8 x l o 4 ] a,P,y,fi-Tetraphenylporphinetrisulfonate [ 434; 5.0 X l o 5] Bis(2-aminoethy1)dithiocarbamicacid [437; 1.32 x l o 4 ] Ferrozine [470; 4.32 X l o 3 ] Pb bis(4-sulfobenzy1)dithiocarbamate[433; 1.58 x l o 4 ] Phenylpyruvic acid 2-quinolylhydrazone [450; 3.15 X l o 4 ] Lead diethyldithiocarbamate (CHC1, ) 2,2’-Biquinolyl, bromophenol blue (3-Me-1-BuOH) [ 605; 2.5 x l o 4 ] Gallein, N-benzoylphenylhydroxylamine (BuOH) 1,lO-Phenanthroline, methyl orange [420; 4.83 x l o 4 ] Biacetyl oxime thiosemicarbazone 1507: 6.25 x 1031 6-Hydroxy-5-nitroso-1,3-dimethyl-i, 2,3;4-tetrahydr&2,4-pyrimidinedione 1615: 1.55 X 1041 D{Z-pyridyl ketone 2-pyridylhydrazone [ 538; 1.5 x l o 4 ] 7-Nitroso-8-hydroxyquinoline-5-sulfonic acid [ 704; 1.84 X l o 4 ] N-Methylanabasine-0’-azo-p-cresol [ 510; 1.94 X l o 4 ] 2,2’-Bipyridine, automated 2-Nitroso-4-ch1oropheno1, rhodamine B (toluene) [ 558; 9.0 x l o 4 ] 2-Nitroso-5-dimethylaminophenol[ 750; 3.95 X l o 4 ] 7-Nitroso-8-quinolinol-5-sodium sulfonate [ 710; 1.9 X l o 4 ] Di-2-pyridyl ketone azine [460; 9.3 X l o 3 ] 2-Hydroxy-5-methylacetophenone thiosemicarbazone [ 645; 0.5-8 ppm] Glycinecresol red [520;2.42 x l o 4 ] Chrome green BLN [598; 2.96 X l o 4 ] Chromeazurol S, cetyltrimethylammonium bromide [ 640; 1.14 x l o 5 ] o-Hydroxybenzaldehyde isonicotinoyl hydrazane (1-pentanol) [ 390; 3.40 x l o 4 ] Rhodamine B (BuCOMe-C,H,) Sulfonitrazo E Alumocreson [ 505; 3.56 X l o 4 ] Extrn; bis(2-ethylhexyl)phosphate,methyl red (C,H,,) [ 550; 2-20 ppm] Diphenylguanidine (isoamyl OH) [540; 6.4 X l o 3 ] Catechol violet: 1.10-Dhenanthroline 1640: 0.16-1.6 m m l 1,2,4-TrihydroXyanthraquinone“purpurin;’, diphenyiiuan’idine (CHCl,) r545: 1.85 x 1041 PAR (isoamyl OH)-[510; 3.75 X l o 4 ] Alizarin red S Hematein [520; 5.8 X l o 4 ] Eriochrome cyanine 6-Phenyl-2,3-dihydro-as-triazine-3-thione (CHCl,) [ 430; 6.09 x lo3] Xylenol orange, hexamine [ 590; 2.2 X l o 5 ] 6-(4-Nitropheny1azo)pyridoxine 1,lO-Phenanthroline, rose bengal B Janus green (C,H,-C,H,Cl,) [625; 0.8-20 ppm] Cu(II)-bis(4-sulfobenzyl)dithiocarbamate[ 433 ; 1.59 x lo43 Thiodibenzoylmethane Dithizone (CHCl,) Direct absorbance measurement at 2 wavelengths of TLC plate spots 6,7-Dihydroxy-2,4-diphenylbenzopyryliumchloride [ 550; 4.57 x l o 4 ] Chromeazurol S, cetyltrimethylammonium bromide [ 630; 1.23 x lo5] Victoria blue-InBr,- (C,H,) [625; 1.2 X 10’1 o-Hydroxybenzaldehyde isonicotinoyl hydrazone (1-pentanol) [ 380; 3.20 X l o 4 ] Malachite green-In1,- (C,H,-CHC1, ) 3-Nitroso-4-hydroxy-5,6-benzocoumarin [ 520; 1.28 x l o 4 ] Acenaphthenequinone monoxime Methylthymol blue, diphenylguanidine [ BuOH] 5,7-Diodo-8-quinolinol, rhodamine S (CHCl,) Boropyrocatechol Acid chrome black K [550; 1.3 x l o 3 ] Xylidyl blue Eriochrome black T Thiothenoyltrifluoroacetone (CC1,) [450; 3.8 X l o 3 ]
... *.. Atmospheric Steel Steel
... ...
cu
... ... ... ... Alloys Foods Ni alloys DY Fe
... ... ... *.. .. ... ...
Silicate rocks Sea water Water Pharmaceuticals
... ...
A1 alloys Ga
...
...
... ... ... ...
Ge
... Hf
...
Hg
... ,..
...
*.. ... *..
...
Foods Hg, inorg. and org.
... ... ...
In
Alloys
Ir La Lu
Mg
... ... ... ... ...
Silicates Tobacco leaves Mn 220 R
...
ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
Ref.
4 3
503 572 596 27 7 537 353 321 283
451 572 336 389 390 238 511 295 527 260 364 468 429 226 564 557 17 23 293 581 284 546 149 563 406 400 309 158 568 231 560 310 307 18 171 372 509 325 131 282
322 91 41 529 40 528 562 364 223 395 158 114
568 274 279 488 59 348 470 28 7 592 495 497
Table I (continued) Constituent
Material
Steel Mo
. . ,I
.
I
.
.,.
... ... ... ... ... ...
Soils Steel Steel Steel Steel Plants Steel Nb alloys Biological, steel Steel Steel Steel Nb
Steel
...
...
Ferrous alloys Zr alloys Rocks Steel Alloys Nd Ni
... ... ... ... ... ... ...
Steel Steel NP
os
... ... ... *.. ... ...
Pd
...
... ... ...
... ... , . .
.
..
,,
..
Method or reagent [wavelength; molar absorptivity, or concentration range]
PAR [496; 8.65 X 10‘1 Ferrocene redn.; thiocyanate, Me,CO or MeCN [465; (1.37-1.65) X l o 4 ] Quinoline, thiocyanate (PhNO,) [470; 1.80 X l o 4 ] 2-Hydroxy-5-nitrobenzene-1,l’-azo-(3-naphthol,Me,CO Dithiooxamide [600; 2.2 X lo’] 1-Pyrrolidinecarbodithioate (CHCI,) [385; 4.5 x l o 3 ] Thiosulfate (isoamyl OH) [475; 3-30 ppm] Toluene-3,4~dithiol[705; 1.84 X l o 4 ] Gallein [620; 5.2 x l o 4 ] 3,4,5,3’,4’-Pentahydroxybenzophenone [ 4 10 ; 1.58 X 1O4 ] Unithiol [364; 0.3-3 ppm] 4-Galloylpyrogallol [420; 1.4 X l o 4 ] Redn., hydrazine sulfate (isoamyl OAc) 4-(2-Thiazolylazo) resorcinol, hydroxylamine [ 530; 2.94 X l o 4 ] Mo(V)-oxypentathiocyanate-rhodamine B [ 600; 0.004-0.4 ppm] Benzylaminopyridine, thiocyanate (CHCI,O) [465; 2.0 x l o 4 ] p-Nitrophenylfluorone (Bu,PO,-C,H,) [ 530; 4.5 x l o 4 ] Thiocyanate, tetraphenylarsonium chloride, quinol (CHCl,) [ 470; 1.74 X l o 4 ] Thiocyanate, ethylxanthate (acetophenone) [ 380 or 470 ; 2.5-10 ppm] Catalytic, iodide, hydrogen peroxide; automated Bromopyrogallol red, zephiramine [629; 5.56 x l o 4 ] Ferrocene, thiocyanate [465; 1.45 X l o “ ] Dithiol Stilbazo, zephiramine [535; 6.3 X l o 4 ] Phenylfluorone (amyl OAc) [520; 1.04 x l o 4 ] 2-Mercaptobenzo-y-thiopyrone,thiocyanate, tin( 11) chloride(acetophenone) [470; 0.8-8.5 ppm] Tannin, thioglycolic acid [420; 1-10 ppm] Sulfonitrophenol M Pyrocatechol violet, cetylpyridinium bromide [ 565; 5.3 X l o 4 ] Thiocyanate, tetraphenylarsonium chloride (CHCI,) [ 390; 3.2 x l o 4 ] Thiocyanate PAR o-Nitrophenylfluorone (CHCl,) [530; 1.38 x l o 5 ] Gallic acid, aniline (amyl OH-C,H,CI,) [320; 7 x l o 3 ] Thiocyanate; 1,lO-phenanthroline (Bu,PO,-C,H,) [400; 4 X l o 4 ] 2-(2-Thiazolylazo)-5-dimethylaminophenol, triethanolamine [ 605; 4.8 x lo4J Heteropoly blue of molybdoniobate Gallein, cetyltrimethylammonium ion 4-Sulfo-1,2-naphthoquinone dioxime, zephiramine [480; 2.03 x l o 4 ] o-Chlorobenzoic’acidhydrazide Acetamidoxime [620; 4.5 X lo3] Dimethylglyoxime, test papers, reflectance Dimethylglyoxime, diphenylguanidinium chloride (CHC1,-isoamyl OH) Chromotropic acid [545; 3.0 X l o 3 ] Thiovioluric acid [375; 2.33 X lo4] N-Methylaminothioformyl-N’-formyl-N’-phenylhydroxylamine [ 440; 2.72 x l o 4 ] 2-Amino-3-quinoxalinethiol [495; 2.4 x l o 4 ] Hydroxyrubwnic acid [640; 1.44 X l o 4 ] Nitroxaminazo [585; 2.5 x l o 4 ] Complexon 111, HNO, Arsenazo M 1-Pyrrolidinecarbodithioate, Triton X-100 Dithiobenzoic acid (CHCI,) [490; 1-60 ppm] P-Benzoyl-a(ethano1)thiourea [410; 6-18 ppm J fl-Benzoyl-a(o-tolyl)thiourea[400; 6.8 x l o 3 ] Rubeanic acid [490; 6-18 ppm] 2,3-Quinoxalinedithiol [560; 1.73 X l o 4 ] Acenaphthenquinone monoxime Benzylselenide (C,H,) [342; 0.6-3 ppm] Bismuthiol I1 (Bu,PO,) [450; 4.6 X l o 3 ] 2-Hydroxy-4-methyl-thiazole [ 385; 10-25 ppm] Crystal violet, thiocyanate Sodium-3-formyl-4-hydroxyazobenzene-4-sulfonate [ 490; 8.1 x l o 3J Thioridazine hydrochloride [ 490; 3.68 x l o 3 ] Diacetylmonoxime (CHCI,) [320; 4.8 x l o 3 ] p-Dimethylaminobenzylidene rhodanine (PhNO,) Phenothiazine [600; 7.13 x l o 3 ] K butyl xanthate (CHC1,) Chromotrope I1 [610; 1-11 ppm] Promazine hydrochloride [ 540; 8.8 X l o 3 ] 1,8-NapthalenedithioI,gum arabic [ 450; 0.2-7 ppm] Chlorpromazine hydrochloride [ 565; 1.89 x l o 4 ] Methythymol blue [530; 2.1 x l o 4 ] Phenylthiourea [400; 3.04 x l o 3 ] 1,3-Bis(2’-pyridyl)-1,2-diaza-2-propene (C,H,) [ 573; 1.8 x l o 4 ] ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
Ref.
380 499 446 431 584 302 591 126 456 433 56 432 590 516 20 6 420 42 164 33 78 122 498 439 399 58 462 144 178 369 180 578 494 376 20 31 1 558 597 428 29 8 434 333 289 599 225 102 335 392 15 120
350 384 21 3 185 69 68 67 245 489 422 547 25 2 418 251
193 403 76 192 402 264 437 512 303 502 407 467 221 R
Table I (continued) Constituent
Material
Method or reagent [wavelength; molar absorptivity, or concentration range]
... ...
1-(2-Pyridylazo)-2-phenanthrol (CHCl,) [670; 8.4 x 10'1 o-Hydroxythiobenzhydrazide (CHC1,) [690; 2.78 x l o 4 ] Chlorophosphonazo I11 [690; 3.7 x 10'1 Pu Rare earths ... Chlorophosphonazo I11 (n-butanol) Glycinecresol red, cetyltrimethylammonium base ... ... acid 2-4(Sulfophenylazo)-1,8-dihydroxynaphthalene-3,6-disulfonic Re 4-Phenylthiosemicarbazide [395; 9.1 X l o 3 ] ... ... Rhodamine B (C,H,) o-Hydroxythiobenzhydrazide [ 565; 9.62 x l o 3 ] ... Acridine yellow (1,2-dichloroethane-Me~CO) [455; 3.5 x lo'] *.. Acriflavine-ReO4-(l,2-dichloroethane-Me,C0 [465; 4.2 X lo'] *.. Alloys 1-Phenylthiosemicarbazide [ 365; 1.5 X lo'] Rh 5-Sulfoallthiox [430; 7.4 X l o 3 ] ... Sulfochlorophenolazorhodanine, H,SO,-HOAc [ 510; 6.5 X l o 4 ] o-Tolylurea (C,H,Cl,) [400; 1.47 x l o 4 ] ... Nitroso-R salt [480; 1.2 X 10'1 ... Acenaphthenequinone monoxime Arsenazo I [ 580; 1-7 ppm] Ru ... P-Dithionaphthoic acid (CHCl,) [490; 2.36 X lo'] ... ... 3-Nitroso-4-hydroxy-5,6-benzocoumarin (BuOH) [ 520; 1.04 x l o 4 ] Glycine ... 4,5-Diamino-6-hydroxypyrimidine: sulfate [ 530; 6.5 x l o 3 ] ... Pyronine G [530; 6 X l o 4 ] Sb ... Methyl green (C,H,-PhNO,) Cadmium Methylene green (CHC1,) [655; 7.6 x 10'1 N-Methylanabasinyl-cy-azo-n-heptylresorcinol Ores Safranine o-SbC1,- (C,H,) Steel sc Glycine cresol red [525; 2.75 X l o 4 ] ... Xylenol orange, ethyltridecylammonium bromide (C,H,) [ 520; 2.,7 X lo4] ... Methylthymol blue, diphenylguanidine (BuOH) ... 1-(2-Pyridylazo)-2-naphthol (C,H,) [580; 1.9 x l o 4 ] Sn .. . 2,2'-Diquinoxaline [675; 2.06 X l o 4 ] ... Cationic pink 2S, tin(I1) chloride (C,H,) [540; 4.1 X l o 4 ] Ores, alloys Gallein Ores Phenylfluorone Organotin compounds Tin( IV)-chloride-8-quinolinol (CHCl, ) Catechol violet, cetyltrimethylammonium bromide Steel Thioglycolic acid, Na laurylsulfate Silicates Gallein or dihydroxyfluorescein (cyclohexone) .. 3,5,7,4'-Tetrahydroxyflavone[430; 4.12 X l o 4 ] Rocks 3,5-Dinitropyrocatechol,brilliant green (CCl,) Arsenazo I11 [650; 4.00 x l o 4 ] Sr Pyrocatechol violet, cetylpyridinium bromide [ 605 ; 0.2-1.8 ppm] Ta ... 8-Hydroxquinoline-5-sulfonic acid ... Crystal violet (BuOAc) [590; 8.5 X 10'1 Capri blue-TaF,- (CHCl,) [660; 1.07 X l o 5 ] ... Pyrocatechol, aniline [isoamyl OH] Janus green-TaF,- (C,H,-Me,CO) [650; 1.32 X l o 5 ] Niobium Zr alloy Victoria blue B Sulfochlorophenol S [640; 3.3 X 10'1 Th Chromeazurol S, cetyltrimethylammonium bromide [ 635; 1.46 X l o 5 ] ... Chlorophosphonazo I11 [685; 3.59 X l o 4 ] *.. Hydrazo T (CHC1,) [525; 0.08-0.8 ppm] Ti ... Salicyltrihydroxy fluorone, thiocyanate (iso-BuOH-CHC1,) [530; 1.44 X lo5] 2-Carboxyphenylazopyrogallol [ 490; 0.5-1.8 ppm] ... Diantipyrylmethane, thiocyanate (CHCl,) [360; 7 X l o 4 ] ... 6-(2-Pyridylazo)-4-cyclohexylresorcinol (CHC1, )-isoamyl OH .. * Benzoylphenylhydroxylamine, phenylfluorone (CHCl,) [ 550; 7.5 X l o 4 ] ... Diantipyrylmethane, tin(I1) chloride (CHCl,) [395; 6.8 X l o 4 ] Alloys PAR, pyrocatechol [510; 4.2 x l o 4 ] Ferroniobium 1-( 2-Hydroxy-4-sulfo-6-nitro-l-naphthylazo)-2-naphthol [420; 1.9 X l o 4 ] Steels Dibromotichromin, diphenylguanidinium chloride (BuOH) [480;1.03 X l o 4 ] Steel Tl Naphthalene green-TlBr,- (C,H,-MeCOEt) [630; 8.4 X lo'] ... Methyl red, bis( 2-ethyl hexy1)phosphate (heptane) ... Astrazon blue P (C,H,) [630; 1.1 X l o 5 ] ... Benzothiazolyl (2'-azo-6)-4-methylphenol *.. Brilliant green-TIC1,- (di-isopropyl ether) [630; 1.06 X l o 5 ] Indium 6 4 2-Quinolylazo )-3,4-dimethylphenol ... Furfurol green-T1Br4- (C,H,-MeCOEt) [627; 2.6 X l o 4 ] o-Nitral green (C,H,) [635; 1.10 X l o 5 ] .. U Benzoate, malachite green (C,H,-CHCl,) [630; 1.3 X l o 5 ] .. Quinalizarin 1-[(5-Methyl-2-pyridyl)azo]-2-naphthol (CHCI,) [ 560; 2.1 X l o 4 ] p-Tolylbenzohydroxamic acid (CHC1,) [ 515 ; 5-20 ppm] 2-Mercaptopyridine-1-oxide[ 490; 1-30 ppm U O Z z f ] *. 1-Phenyl-3-@-sulfophenyl)-1,3-propanedione sodium [ 398; 1.93 X l o 4 ] Pt
222R
ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
Ref.
66 173 586 519 270 598 38 515 174 534 533 74 121 436 44 3 331 490 265 188 280 84 570 408 273 532 1 86 14 486 59 441 46 88
139 573 332 35
124 2 175 375 342 370 476 328 151
19 200 259 236 157 314 135 30 169 571 99 419 430 219 286 50
112 29 469 204 330 442 113 115 505
444 482 9 146 552
Table I (continued) Constituent
Material
... Alloys V Steel Slags Steel
Fuel oils
... ... ...
... ...
... ... .. , ..,
Silicates Steel TiC1, W
..
,I
..,
...
Steel Steel Steel Y
Zn
Mg alloy Zr
... *.. ... ... ... *.. ... ... ... ...
Copper alloys Steel
...
Method or reagent [wavelength; molar absorptivity, or concentration range]
Bromopyrogallol red, cetyltrimethylammonium bromide Rhodamine B-uranyl benzoate (MIBK) [555; 9.0 X lo'] 5-(4-Antipyrylazo)-2-monoethylamine-p-cresol (CHCl,) [ 515; 0.3-16 ppm] 1,5-Bis(2-hydroxy-5-sulfophenyl)-3-cyanoformazan [ 635; 1.63 X 10'3 N-rn-Tolyl-o-methoxybenzohydroxamic acid (CHCI,) [ 510; 0.3-20 ppm J Glycinethymol blue, cetyltrimethylammonium base [ 560 ; 0.1-6 ppm J l-(2-Pyridylazo)resorcinol, hydroxylamine [ 550; 3.0 x 10'1 44 2-Thiazolylazo )resorcinol, tributylamine (CHCl,) [ 550; 2.5 X lo' J N-Cinnamoyl-N-phenylhydroxylamine(CHC1,) [ 535; 1-10 ppm J 2-Carbethoxy-5-hydroxyl-l-(4-tolyl)-4-pyridinone [ 615; 5.10 X l o 3J N-Phenyl-2-naphthohydroxamicacid (CHCI,) [ 545; 7.1 X l o 3 ] Tunstovanadophosphoric acid 24 2-Thiazolylazo )-5-dimethylaminophenol (CHCl, ) 1,2,3-Phenyloxyamidine (CHCl,) [560; 4.21 X 10'1 Disodium maleonitrile dithiolate [ 580; 4.89 X l o 3J Molybdovanadophosphoric acid, malachite green N-p-Tolyl-2-furohydroxamic acid (CHCl,) [ 540; 3.0 X l o 3J Thiothenoyltrifluoroacetone (CCl,, n-butanol) [ 450; 3.5 X l o 3 ] Tannic acid-thioglycolic acid [ 600; 0.5-5 ppm J Anthranilic acid acetonehydrazide [ 525; 5.1 X l o 3J 2-( 3,5-Dibromo-4-methyl-2-pyridylazo)-5-diethylaminophenol, H,O, [615; 5.43 X 10'1 o-Phenylenediamine [400; 0.5-10 ppm] 44 2-Pyridylazo) resorcinol Tribenzylamine-V(V)-thiocyanate :CHCI,) Solochrome violet RS [550; 3.5 X l o 3 ] Eriochrome black T, or solochrome 6BN 3,5-Dinitropyrocatechol, brilliant green (CHC1,) Molybdate, ascorbic acid [825; 0.01-0.1 ppm] Quercetin [413; 1.4 X lo'] Pyrocatechol, dimedrol (CHC1,) [310; 4 X l o 3 ] Hydroquinone Xylenol orange, ethyltridodecylammonium bromide [ 604; 7.6 x 10' J Methylthymol blue, diphenylguanidine (BuOH) acid 2-(8-Quinolinazo)-l-naphthylamine-3,6-disulfonic 1-Picolylideneamino-2-naphthol (CHC1,) [ 520; 4.5 x 10'1 PAR, "GeMSAEC Fast Analyzer" 1-(2-Pyridylazo)-2-naphthol, Triton X-100 [ 555; 5.6 x 10'1 5 4 2-Quinolylazo)-2-monoethylamino-p-cresol [ 530; 9.6 x lo'] Arsenazo 111, iodide, allyl alc. [590; 4.28 X 10'1 Rutin [410; 1 . 2 x 10'1 Arsenazo I11 [ 686; 0.8-4 ppm J PAR [540; 6.75 X l o 3 ] Phthalexon S Sodium 2-bromo-4,5-dihydroxyazobenzene-4'-~sulfonate [ 520; 2 x 10'1 Arsenazo I11
aging, and computer compatibility (177). The PerkinElmer Model 575 UV-visible spectrophotometer features dark cycle stepping, a photometric system that measures the ratio of sample and reference absorbances a t identical wavelen ths. This instrument includes automatic zeroing of absorEance, and BCD output (412)
Special Application Instruments and Accessories. Photometers for detectors in liquid chromatography continue to be extensively used. The LDC Spectro Monitor I is a double beam instrument designed to make differential or direct absorbance measurements in the 200- to 700-nm range on HPLC streams. The dual flow cell has a 10-mm optical path and a 10-111 cell volume (299). The Dual Channel Absorbance Monitor by Glenco (182) uses interference filters and is especially applicable to measuring the absorbance of effluents from a chromatographic column. A digital photometer for monitoring liquid chromatographic streams and routine photometric measurements has been described (224). A multichannel photometer employing fiber optics is applicable to continuous flow systems (51) and a fiber optics accessory permits spectrophotometric measurements outside of the cell compartment (457). Automation of routine spectrophotometric determinations is becoming more extensively adopted. An automatic spectrophotometric analyzer with a program-timer has been utilized to determine acid soluble aluminum in steel (396). A new UV-VIS spectrophotometer for use with the
Ref.
269 143 201 471 10 268 327 197 199 521 7 47 559 461 100 93 8
496 45 136 276 44 427 589 4 24 363 373 326 556 477 382 493 59 508
398 184 570 203 343 176 103 365 104 49 239
Technicon AutoAnalyzer I1 continuous flow system has a 200- to 900-nm range (538). A sample ,cell with a stirrer to prevent bubbles and whirlpools (414), and a two-chamber cuvette with a movable window between chambers so that the path length of the first chamber can be increased to compensate for the decrease in the absorbance of the solution in the second chamber (28) have been designed. The Tektronix 7S20 rapid-scan spectrometer system has a 250- to 1100-nm spectral range. When coupled with a digital processing oscilloscope, it permits use of a minicomputer to calculate rapidly the CIE color coordinate values (539). The Zeiss TLC spectrophotometer permits reflectance, transmittance, fluorescence, and fluorescence quenching measurements (94). An instrument which enables optical rotatory dispersion, circular dichroism, and absorbance to be measured in a single scan has been described (24). A two-cavity micro flow-through cuvette has been patented (458). Special cells have been designated to minimize formation of gas bubbles (161, 414). Rotors having separate sample and transfer channels have been developed for centrifugal photoanalyzers in order to prevent premature moving (87).
APPLICATIONS Methods of Analysis. Spectrophotometric methods are used extensively in many scientific disciplines so that nuANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
* 223R
Table 11. Spectrophotometric Methods for Nonmetals Constituent
As
... ... e
.
.
Antimony Alloys Cu-plating baths Lung tissue Plants B
*.. Silicon Soils, plants
...
co c1-
...
Polymers
... ...
c10,CN-
*.. ... ...
Cyanide complexes Sodium F-
... 1
.
.
...
Apatites Inorganic, organic compds. Fe(CN),NO,HzO, 1-
NO,~
0
~
3
-
Method or reagent [wavelength; molar absorptivity or concentration range]
Material
Heteropoly blue 354 Redn. of molybdoarsenic acid with SnC,O,; aq. [ 830; 1.8 x 10.3 ; aq.-Me,CO 355 r720; 2.1 x 1 0 4 1 Methylene blue-fluorarsenate (C,H4C1,) 60 Heteropoly blue (iso-BuOH) 366 Heteropoly blue 186 Heteropoly blue 600 Kinetic; catalytic redn. of Os(V1II) to Os(II1); formation of thiourea complex Copptn.; heteropoly blue Azomethine, automated Methyl green Carminic acid Methylene blue-BF,- (ClC,H,Cl) Azomethine [420; 0.5-8 ppm] Bis(1,lO-phenanthroline)palladium chloride Catalytic; conv. of NO,- to NO,-; chromotropic acid [505; 1-100 ppm] Mercury(11) diphenylcarbazone (C,H, ) Turbidimetric; silver chloride Decolorization; acid chrome violet K Monosulfonated diphenylcarbazone, copper(11) Copper(I1); oxidn. of phenolphthalein Nitrobenzene contg. sulfur; tris( 1,lo-phenanthroline)iron(II)thiocyanate Indirect; kinetic; dicyanoferroin (CHCI,); acid chrome black ET, H,O, Prussian blue spot; densitometric Conv. to thiocyanate; iron(II1)
449 52 401 198 301 249 478 6 24 2 160 34 246 166 21 6 194 229 544
Pyridine-barbituric acid Sulfonated alizarin fluorine blue, La(II1) Decolorization; Zr-eriochrome cyanine R Zirconium(IV), rufigallic acid [ 560; 1-7 ppm] Indirect; Th(IO,),, redn., linear starch [625; 0.2-6 ppm] iron(111) Indirect; N,N'-bis(0-hydroxpropy1)-o-phenylenediamine, Alizarin complexone Alizarin complexone, lanthanum( 111)
41 0 306 105 92 217 405 347 272
...
Ferroin (MeNO,) [510; 2.75 x l o 4 ] Iodide, butylrhodamine p (C6H6.) Bis(neocupr0ine)-copper(1)-triiodide (PhCl) ... Milk 4,4' -Tetramethyldiaminodiphenylmethane Plant nutrients Catalytic; arsenic(III), cerium( IV); semi-automated Rocks Butylrhodamine C(C,H,) Salt 2,4,6-Triphenylpyrylium iodide (CHCl,) [545; 6.46 X 10' ] Water Catalytic; arsenic(III), cerium(1V);automated Dairy products Kjeldahl, indophenol, automated Metals Hypochlorite, thymol Oxidn. t o "0,; Griess reaction peri-Naphthindan-2,3,4-trion hydrate [ 460; 3.6 X l o ' ] ... Diazotization, coupling with guayazulene [ 520; 4.1 X lo4J ... 4,4'-Bis(dimethy1amino)thiobenzophenone Mercaptoacetic acid (isoamyl OH) ... Rutin Soil, water Redn. t o NO,-; orange I Water Methyl orange; UV irradiation Tris(4,7-dihydroxy-l,lO-phenanthroline)iron(II) [ 520; 1-20 ppm J Gallium Heteropoly blue Halosilanes Indirect; molybdophosphoric acid (CHC1,-n-BuOH), thiocyanate Plant nutrients, Molybdophosphoric acid (EtOAc);heteropoly blue soil Water Reduced molvbdoantirnonylphosuhoric acid (acetophenone-CHC1, ) -- [820; 2 x l o 4J Hydrolysis, heteropoly blue [882; 4.6 X lo4] Nitroprusside Palladium monothioacetylacetonate Indirect; pptn. CuS; diethyldithiocarbamate (CCl,) [438; 1.25 x 10'1 Metals Methylene blue Modified methylene blue ... He or H, gas Methylene blue Ba-chlorophosphonazo I11 ... Pptn.; octamine-pamido-phydroxydicobalt(II1) chloride [ 500; 10' ] Plants Oxygen flask; turbidimetric, BaSO, Soils Fusion, NaNO,/KNO,; turbidimetric, BaSO, Water Methylthymol blue, barium(I1); automated Alk. cyanolysis, copper(I1); iron(II1) thiocyanate ... 1
.
.
" I
P,o,~8-
H,S
s0,z-
e
s,o,'224R
.
Ref.
.
ANALYTICAL CHEMISTRY, VOL. 48,
NO. 5,
APRIL 1976
535
83 514 587 248 565 425 95 555 463 21 0 255 21 2 32 141 447 267 214 134 426 190 130 247 183
142 550 262 368 460 334 349 31 3 41 7 96 320 5 381
Table I1 (continued) Constituent
... ... ... *..
s 0 =-
s:o:z-, s,o,z-, s,o,~SCNSe Si
Method or reagent [wavelength; molar absorptivity or concentration range]
Material
Alk. cyanolysis; iron(II1) thiocyanate Cyanalysis; iodimetric Indirect ; bis( thiocyanato )bis(quinoline)mercury(11) Diaminochrysazine Heteropoly blue Kinetic, catalytic; iodide, molybdate Heteropoly blue, automated 9,9'-Methylene bis(6-hydroxy-rn-phenylene)J bis[ 2,3,7-trihydroxy-6fluorone J Rhodamine 6G [525; 1.7 X l o 4 ]
A1 alloys Steel
...
Te Steel
Ref.
381 278 147 80 491 356 397 374 485
Table 111. Spectrophotometric Methods for Organic Compounds Constituent
Material
*..
Acetic anhydride Acetone Alcohols Alcohols, C,-C,, Alcohol prim. and sec. Aldehydes, Aldehydes, aromatic
Phthalic esters Mixtures
... ...
...
Alkylbenzenesulfonate Amides Amines, prim. Amines, prim. Amines prim. and sec. Amines, prim., sec., and tert. Amines, aliphatic Amines, p-aromatic Aminophenol isomers p -Aminophenol p-Aminophenoxyacetic aci d Amprolium Antazoline Anthraquinone N-Arylhydroxylamines Ascorbic acid Azide, organic Benzaldehyde Benzidine Benzophenone Bilirubin Biuret n-Butylmercaptan Carboxylic acids Carbohydrates Carbohydrate carbon Carbazole Carbonyl compds. Catechol Cephalosporins Chloropromazine Cyclohexylphenyl ketone Cysteine Deoxyribonucleic acid o-Dianisidine 3,5-Dinitro-o-toluamide Diphenylamine Dipyrone Disulfides, thiuram, dixanthates Ergocalcifer 1 Flavanols Folic acid Formaldehyde Glycoaldehyde
...
... ... .. Food dyes
... ...
Feed stuffs Pharmaceuticals Anthracene
...
Pharmaceuticals Pharmaceuticals
... ... ...
... ... Blood ...
Hydrocarbons
**.
...
Sediments Anthracene
... ...
Pharmaceuticals
...
... ... Feedstuffs ...
Tissue
Pharmaceuticals
... ... ... Pharmaceuticals ...
Method or reagent [wavelength; molar absorptivity or concentration range]
Ref.
N - (Carbethoxymethy1)isoquinolinium bromide, Et,N(CHCl, ) [440; 4.0 X 10,J 2,4-Dinitrophenylhydrazine 3,5-Dinitrobenzoyl chloride Vanadium-8-quinolinol (C,H,), or 3,5-dinitrobenzoyl chloride (pyridine) Nitration, simultaneous Propionaldehyde( 3-phenyl-2-quinoxaliny1)hydrazone Antipyrine Thiosemicarbazide; 2,3-dichloro-l,4-naphthoquinone (CH,Cl, ) 2,2,5,5-Tetrakis(carboxymethylthio)-p-dithiane Crystal violet, plasticized polyvinyl sheet [ 596; 0.2-10 ppm] Neutral red (PhNO,) Oxidn., triiodide-starch complex Salicylaldehyde, copper( 11) (amyl OH) Fluorescamine Fluorescamine; simultaneous Acetylchloride, iron(II1)
54 3 518 55 3 48 29 6 525 526 466 290 548 549 448
Bromophenol blue (CHC1,) 4-Dimethylaminocinnamaldehyde Copper(II), ammonia [BuOH] Indophenol Diazotization; 1-naphthol Naphthalene-2,7-diol, hexacyanoferrate(III), cyanide Nitrite [410; 20-120 ppm] Sodium hydroxide, sodium hydrosulfite 9-Chloroacridine Phenylhydrazinium chloride [ 395; 25-100 ppm] Dimethoxydiquinone [ 510; 10-80 ppm] Iron(II1) azide 2,4-Dinitrophenylhydrazine; KOH Dichromate oxidn. Sodium hypochlorite 2,4-Dinitrophenylhydrazine; KOH Automated; Michaelsson method Kinetic; phenol, hypochlorite Cobalt naphthenate Hydroxylamine, dicyclohexylcarbodiimide [ 525; 0.25-2.5 x Hydroxylamine, dicyclohexylcarbodiimide, iron( 111) 2,2,5,5-Tetrakis(carboxymethylthio)-p-dithiane Phenol, concd H,SO, Xanthydrol 2,4-Dinitrophenylhydrazine Iron(III), EDTA, Aliquat 336 (PhCl) [480; 8.8 x l o 3 ] Hydroxylamine, nickel(I1) Picric acid (C,H,) [405; 9.8 X l o 3 ] 2,4-Dinitrophenylhydrazine; KOH Crystal violet-SbC1,- (C,H, ) Hydrolysis ;p-nitrophen ylhydrazine Dichromate oxidn. Acetone, NaOH Oxidn.; cerium(1V) sulfate [570; 4.5 x l o 4 ] Neotetrazolium chloride Dithiof luor escein
289 133 455 450 450 473 26 24 1 170 574 150 79 601 162 163 601 244 257 37 1 258 41 3 296 319 168 391 57 338 530 601 479 119 162 472 172 569 423
l o 6M J
Trifluoroacetic acid, hydroquinone [490; 2-6 ppm J Antimony(II1) Redn.; 1,2-naphthoquinone-4-sulfonic acid [485; 12-58 ppm J 2,3-Dimethyl-2,3-bis(hydroxyamino)butane, sodium periodate, pyridine Ethylene glycol 3-Methyl-2(3H)-benzothiazolone hydrazone (CCl,); 2,4-dinitrophenylhydrazine, DMF [616; 7.1 X l o 4 ] ANALYTICAL CHEMISTRY, VOL. 48, NO. 5, APRIL 1976
51 3 13 38 5 208
179 65 25 6 362 501 225R
Table I11 (continued) Constituent
Glyoxal Hexoses Isoxazole amines GI-Ketoglutaricacid Malic acid Mer captans Methanol Organic per acids Nitric esters Nitroaromat ics
Material
Method or reagent [wavelength: molar absorptivity or concentration range]
*..
2,4-Dinitrophenylhydrazine ... Os(VII1) oxidn.; diperiodatocuprate(II1) ... Sodium naphthoquinone-4-sulfonate ... Diazobenzenesulfonic acid ... KMnO, oxidn. ; 2,4-dinitrophenyl hydrazine, KOH, MeiCO Janovsky reaction *.. Oxidn., KMnO,, H,SO, ; acetaldehyde, ammonia; chromotropic acid ... o-Tolidine Kinetic; alkaline hydrolysis .*. Redn. ; formamidinesulfinic acid ;p-dimethylaminobenzaldehyde ... PhNEt, (CHCl,) Nitrobenzene Aqueous -solns. Redn., chromium(I1); amidopyrine [540; 1.3 x 10‘1 Nitrophenols ... Redn.; formamidinesulfinic acid; @-) indophenol reaction; (0-) periodate oxidn.; ( m - by ) difference N-Nitrosamines Heating KOH-CuS0,-N,H, ;N-naphthylethylenediamine, sulfanilic acid Pharmaceuticals Alk. hydrolysis; p-aminoacetophenone, concd HCl Nystatin ... Paracetanol Hydrolysis; indophenol formation Pentaerythritol tetranitrate Waste water Phenoldisulfonic acid p-Phenetidine ... Diazotization; coupling, 1-naphthol Phenols *.. Oxidative coupling Cerium(IV), hydroxylamine p-Phenylenediamines ... Oxidative coupling Phenylpyrazolone derivs. ... Dragendorff reagent Picric acid *.. Propericiazine (C,H, ) Pyruvic acid p-Diethylaminocinnamaldehyde Retinal *.. 2-Diphenylacetyl-l,3-indandione-l -hydrazone Robenidine Poultry feed NaOH, DMF [464; 0.3-3 ppm] P-Sitosterol Vanillaldehyde, HOAc-H,SO, Steroid oximes Azo dye formation Surfactants (LAS, ... Inhibition of enzymatic reaction ABS, SDS) Sulfanilamide Indophenol reaction [ 625; 2.59 x 10‘1 Tetraphenyl arsonium Vanadium(V), PAR (CHC1,) *.. Drugs 2,3-Dichloro-1,4-naphthoquinone [ 540; 20-80 ppm] Thiambutosine Vitamin Thiamine Bromothymol blue, automated (CHC1,) preparations Benzene Thiophene Isatin, sulfuric acid, iron( 111) o-Tolidine Dichromate oxidn. ... Toluene diisocyanate ... Iodate Toluidine, 0 - , or m ... Bromophenol blue (CHCl,) Triphen ylphosphine Org. solvents Dioxobis(diethyldithiocarbamato)molybdenum(VI) Tryptophan Nitration, alkali; simultaneous Tyrosine Cerium(IV), hydroxylamine ... Vitamin A .. Trichloroacetic acid, MgCl, Vitamin D Pharmaceuticals Anisaldehyde, H,SO, Xanthates Nickel(II), Me,CO ... Xylose Blood Phloroglucinol [554; 3.3 x lo‘] merous specific and specialized methods are found throughout the chemical literature. There is some indication that spectrophotometric methods are being more widely used for the determination of metals, which are not very amenable to atomic absorption spectrometry, and for the determination of nonmetals, which are not easily determined by ion-selective electrode potentiometry. However, the reproducibility and permanence of calibration graphs fosters the adoption of spectrophotometric methods for many applications. Automated spectrophotometric methods are being developed and used for highly repetitive types of samples such as those encountered in clinical, environmental, and pharmaceutical analyses. The results of an extensive sampling of recent developments on specific
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226R
22 2 454 329 351 90 386 230 75 588 388 474 352 387 452 25 152 383 450 118 108 118 110 531 234 97 73 294 165 524 153 49 2 128 404 21 5 162 123 288 318 21 1 108 196 27 445 551
methods and applications are summarized in Tables I, 11, and 111. Color Specification. T h e attention of color scientists is directed to the book, “The Perception of Color” (156),to “Color Essays” by MacAdam (316),and papers on uniform color scales (253, 315, 377, 585). A new two-parameter phase function has been proposed for colorant characterization (22). Tristimulus values when calculated with larger than 5-nm wavelength intervals have been found to be subject to extreme errors as the interval is increased to 10 or 20 nm (394). Computation of tristimulus values by the method of Gaussian quadratures is much faster for certain color matching problems (575). Equations necessary in computer color matching have been discussed (21).
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__
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Mossbauer Spectroscopy John G. Stevens, Department of Chemistty, University of North Carolina at Asheville, Asheville, N.C. 28804
Lawrence H. Bowen Department of Chemistty, North Carolina State University, Raleigh, N.C. 27607
This review is the sixth in a series on Mossbauer spectroscopy published in Analytical Chemistry. As before, the coverage largely includes the literature of the previous two years (1974-1975). The size of this review, however, has been reduced by eliminating most of the tables and narrowing the selection of references (from 839 references in the previous review (S42) to only 424 in the current one). The smaller size reflects the growing difficulty of adequately covering the ever-increasing number of Mossbauer papers being published. There has been a 10% increase in volume over the 1972-1973 period. Many more papers are being devoted to applications of Mossbauer spectroscopy and fewer with the refinement of theories relevant to the Mossbauer effect. Applications have become more and more diverse, moving from the original ones in physics and chemistry, into such fields as mineralogy, biology, metallurgy, and archaeology. Mossbauer spectroscopy is also being used for detailed studies of phase transitions, surfaces, pottery, soils, air samples, catalysts, chemical reactions, the radiation damage process, impurities, biological structures, and colloids, among others. T o the one hundred Mossbauer transitions reported by 1973, only one new one has been added to the literature: Muller et al. ( M 2 4 ) observed the 159-keV transition in l17Sn. The difficulty of observing this transition and its similarity, except for nuclear properties, to the already widely used 23.9-keV transition in l19Sn will probably make its application minimal. Although observation of the Mossbauer effect in the 13.3-keV transition of 73Ge had been previously reported, the results are highly questionable. Careful studies of this transition by a group at Bell Telephone Laboratories, (PIO, R2),therefore, come as welcome information. The extremely narrow linewidths observed (some as small as 0.014 mm/s) make this transition particularly interesting and useful for future studies of systems containing germanium. Observations of the Mossbauer effect in two other transitions have been reported at a conference, although the written results are not yet published. The nuclear physics group a t Darmstadt, Germany, headed by Kankeleit, reported on the 158-keV transition in lQ9Hg at “Fruling232R
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schule-Mossbauerspektroskopie und ihre Anwendungen.” At the same meeting, Gerdau of the University of Hamburg reported the observation of a weak and broadened absorption line for the 10-keV transition in the radioactive isotope of ‘37La. A trend worth noting is the increase in studies of isotopes other than the popular 57Feand l19Sn during the ast two years. The most frequently used have been l5 Eu, 121Sb, and 125Te.In addition, more than ten publications each were written on lg7Au 161Dy 155Gd,1291,lg31r, 237Np, 9 9 R ~and , 170Ybduring 1974-1975.’ Three general books on Mossbauer spectroscopy have been published since the last review. By G. M. Bancroft (B6),“Mossbauer Spectroscopy, An Introduction for Chemists and Geochemists” is an excellent book, especially for the two groups mentioned in the subtitle. Much of the discussion in the inorganic chapters centers around the concepts of partial quadrupole splitting5 and partial chemical shifts. Problems at the end of each chapter make it quite suitable as a textbook. U. Gonser (G19) edited the second book: “Mossbauer Spectroscopy”, issued as Vol. 5 in the “Topics in Applied Physics” series. The emphasis as stated by the editor is to “address those persons interested in learning about what has been done and what can be done with the tool”. After an introductory chapter by Gonser, the other chapters, written by long-time experts in their fields, cover chemistr (P. Gutlich), magnetism (R. W. Grant), biology (C. E. Johnson), lunar geology and mineralogy (S. S. Hafner), and metallurgy (F. E. Fujita). The third book, written in German by D. Christov, Z. Bontschev, and Z. Busova ( C S ) ,is titled “Mossbauer Spectroscopy as a Research Method in Applied Organic Chemistry-Present State and Prospects”. Four Mossbauer conferences and symposia were held during the last two years: 1) “Conference on the Applications of the Mossbauer Effect”, Bendor, France (September 1974), papers of which are published as a supplement to Volume 35 (C6)of Journal de Physique (Paris); 2) “Fruhlingschule-Mossbauerspektroskopie und ihre Anwendungen”, Hunfeld, West Germany, (March 1975; 3) “International Conference on Mossbauer Spectroscopy”,
P
