(411D) (412D) (413D) (414D) (415D)
Y . . Kanke, M., Matsui, A,, Taianta, 19, 1633 ( 1 972). Yamamoto, Y., Kumamaru, T.. Hayashi, Y., Kanke, M . , Matsui, A,. Jap. Anal. (Bunseki Kagaku), 21, 379 (1972). Yanagisawa, M . , Suzuki, M . , Tokeuchi, T., Mikrochim. Acta ( W e n ) , 1973, 475. Yanagisawa. M . , Tokeuchi, T.. Suzuki, M., Anal. Chim. Acta. 64, 361 (1973). Yoza, N., Ohashi. S., Anal. Lett.. 6, 595 (1973). Yudelevich, I . G., Kustas, V. L., Poleva, G. V.. Zh. Anal. Khim., 26, 1378 (1971); J . Anal. Chem. USSR. 26. 1228 (1971). Yudelevich. I . G., Poleva. G. V., Kustas. V. L., Zh. Anal. Khim., 27, 2432 (1972); J. Anal. Chem. USSR,27, 2209 (1972). ~~
(416D)
.
~~~
I
,
Atomic Fluorescence Spectrometry
(1E) Alger, D . . Anderson, R . G., Maines, I . S., West, T. S..Anal. Chim. Acta, 57, 271 (1971). (2E) Barnett, W. B.. Kahn, H. L., Anal. Chem.. 44, 935 (1972). (3E) Belyaev, Yu. I . , Karyakin, A. V., Pcheiintsev. A. M . , Zh. Anal. Khim., 25, 852 (1970), (4E) Baiyaev, Yu. I., Pchelintsev, A. M . , Zh. Anal. Khim., 25, 2094 (1970); J. Anal. Chem. USSR,25, 1799 (1970). (5E) Balyaev. Yu. I., Pchelintsev, A. M . , Zh. Anal Khim., 25, 2238 (1970); J. Anal. Chem. USSR,25, 1922 (1970). (6E) Black, M . S., Glenn, T. H., Bratzel, M . P., Winefordner, J. D . , Anal. Chem., 43, 1769 (1971).
Browner, R . F., Manning, D. C., ibid., 44, 843 (1972). Dagnall, R. M . , Kirkbright, G. F., West, T. S., Wood, R., ibid.. 43, 1765 (1971). Dagnall, R. M . , Kirkbright, G. F., West, T. S., Wood, R., Analyst (London), 97, 245 (1972). Denton, M. B., Malmstadt, H . V., Anal. Chem., 44, 1813 (1972). Ebdon, L., Kirkbright, G. F., West. T. S., Talanta, 19, 1301 (1972). Fraser. L. M . , Winefordner, J. D., Anal. Chem., 43,1693 (1971). lbid., 44, 1444 (1972) Guzeev, I . D . , Blinova, E. S., Maiorov, I. A,, Nedler, V. V., Zavod. Lab., 39, 165 (1973); lnd. Lab., 39, 231 (1973). Hieftje, G. M . , Bystroff, R. I., Lim. R.. Anal. Chem., 45, 254 (1973). Hobbs, R. S., Kirkbright, G. F.. West, T. S., Talanta, 18, 859 (1971). Human, H. G. C., Spectrochim. Acta, 278, 301 (1972). Jones, M., Kirkbright, G. F . , Ranson, L.. West, T. S., Anal. Chim. Acta, 63, 210 (1973), Kirkbright, G. F., West, T. S., Wilson, P. J., ibld., 66, 130 (1973). Kolihova. D . , Sychra, V., Chem. Listy, 66, 93 (1972). Kolihova, D . , Sychra. V.. Anal. Chim. Acta, 63, 479 (1973). lbid., 59, 477 (1972) Mitchell, Q. G., Johansson, A,, Spectrochim. Acta, 268, 677 (1971). Murugaiyan, P., Natarajan, S., Venkateswarlu, Ch., Anal. Chim. Acta, 64, 132 (1973).
Muscat, V. I . , Vickers, T. J., ibid., 57, 23 (1971). Muscat, V. I., Vickers, T. J., Andren, A,, Anal. Chem., 44, 218 (1972). Norris. J. D . , West, T. S.,Anal. Chim. Acta, 59, 474 (1972). /bid., p 355. Norris, J. D . , West, T. S., Anal. Chem., 45, 226 (1973). Omenetto, N., Hatch, N. N., Fraser, L. M.. Winefordner. J. D . , ibid., p 195. Omenetto, N., Hatch. N. N., Fraser. L. M., Winefordner. J. D.. Spectrochim. Acta, 288, 65 (1973). Patel, 8. M.. Browner, R. F., Winefordner, J . D:, Anal. Chem., 44, 2272 (1972). Patel, B. M., Reeves, R. D . , Browner, 8. F.. Molnar. C. J., Winefordner, J. D.. Appl. Spectrosc.. 27, 171 ( 1 973). Patel, B. M . , Winefordner, J. D . , Anal. Chim. Acta, 64, 135 (1973). Pchelintsev, A. M . , Belyaev, Yu. I., Karyakin, A. V., Koveshnikova, T. A,. Zh. Anal. Khim., 26, 1355 (1971); J. Anal. Chem. USSR,26, 1209 (1971). Robinson, J. W., Araktingi, Y . E., Anal. Chim. Acta, 63, 29 (1973) Shimomura, S.,Hiroto, R., Anal. Lett., 6, 613 (1973). Sievin, P. J., Muscat, V. I . , Vickers, T. J., Appl. Spectrosc., 26, 296 (1972) Thompson, K. C., Reynolds, G. D . , Analyst (London), 96, 771 (1971). Vickers, T. J., Slevin, P. J., Muscat, V. I., Farias, L. T., Anal. Chem., 44, 930 (1972) Warr, P. D.,Talanta, 16, 234 (1971). Weide, J. O., Parsons, M L., Anal. Lett., 5, 363 (1972).
Light Absorption Spectrometry D. F. Boltz Wayne S t a t e University, D e t r o i t , M i c h .
M. G. Mellon P u r d u e University, Lafayette, Ind.
This fifteenth consecutive review of light absorption spectrometry records the progress in this analytical field from November 1971 through November 1973, primarily as documented by Chemical Abstracts, and extends the continuous coverage of the literature on this topic for a 44-year period. The subject matter has been classified under the headings of Chemistry, Physics, and Applications as in previous reviews (107, 452, 453). All abstracts and papers have been evaluated carefully in an attempt to select those developments of most probable interest to analytical chemists. The authors recognize the possibility of errors of judgment in omitting certain references. A number of reviews pertaining to specific constituents or reagents have been published. Methods for the determination of tin in steel have been evaluated with particular attention given to the effect of dispersing reagents on the color forming reagents and the complexes formed (44). Photometric methods for determining low concentrations of silver have been reviewed (416). A review of the application of ternary mixed-ligand complexes to the photometric determination of metal ions emphasizes their selectivity and sensitivity (366). A survey on the use of anabasine azo dyes as reagents in the determination of metals has been published (703). Photometric methods for germanium and their applications have been considered (650). Reviews on the use of l-(Z-pyridylazo)-Z-naphthol, PAN (651) and the formazans, especially dithizone and diphenylcarbazone (344),have been published. In evaluating 25 photometric methods for the determi-
nation of fluoride the zirconium-SPADNS method was recommended in the analysis of air and water samples (612). Another review of colorimetric methods for fluoride was documented (467). A review on spectrophotometric methods for metals and nonmetals using aminotriphenyl methane dyes, thiazine dyes, and xanthene dyes has been compiled (445). The role of spectrophotometry in modern trace analysis has been delineated in respect to many applications in environmental and food investigations (106). Two reviews pertaining to the determination of anions include many spectrophotometric methods (78, 105). Books related to light absorption spectrometry follow: “Practical Manual on Photocolorimetric and Spectrophotometric Methods of Analysis,” 3rd ed., (115);“Use of Organic Reagents in Electrophotometry,” Part 2 (721); Colorimetric Methods of Analysis, Vol. 4AAA, 3rd ed. (673); an English translation of “Photometric Analysis; General Principles and Working Tools” (54), and “Accuracy in Spectrophotometry and Luminescence Measurements” (447). CHEMISTRY Research has resulted in numerous new and improved methods utilizing light absorption spectrometry. However, the use of ion selective electrodes and atomic absorption spectrometry have decreased somewhat the interest in spectrophotometric investigations dealing with certain constituents. High pressure liquid chromatography and gas chromatography are being used more extensively in organic analysis.
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Many of the methods cited in Tables I, KI, and III have mum conditions (154). A ternary complex of aluminum, chromazurol S, and mono(alkylpheny1) ether of polyethylbeen included because of their sensitivity, selectivity, or ene glycol has a molar absorptivity of 1.3 X lo5 (512). 6applicability. In this section of the review, we shall conAcyl-5-hydroxy-1,4-benzodioxan oxime gives a stable color sider some of the new reagents, chemical reactions involvwith titanium(1V) (598). p-Dimethylaminophenylfluorone, ing color formation, and significant developments under antipyrine, tin(IV), and an anion of a mineral acid form a the general categories of metals, nonmetals, organic conTitanium(IV), hydrogen peroxquaternary complex (644). stituents, simultaneous determinations, and kinetic deteride, and 8-quinolinol form a 1:1:2 ternary complex exminations. tractable into chloroform, and this color reaction is the Metals. The color reactions of rezarson with 20 metal basis of a photometric method for titanium (786). Phenoions have been characterized (421). The spectral properthiazine derivatives such as chlorpromazine, methopromaties of the colored systems formed by methylthymol blue zine, and diethazine form ternary complexes with molyband group I1 elements have been determined (35). Comparative spectrophotometric studies of seven reagents for denum(V) and thiocyanate. These complexes are soluble zirconium (727), six reagents for iron (720), and five rein chloroform (714). A number of polyphenols were invesagents for aluminum (723) have been made. Fourteen tigated for the determination of niobium with “Tichrommetal ions give highly colored, extractable complexes with in” being recommended (538). either diacetyl bis[(thiobenzoyl)hydrazone], or 2,3-penSensitive spectrophotometric methods for the determitanedione bis[p-(methoxy)thiobenzoyl)]hydrazone (294). nation of lanthanun, thorium, and iron were developed The colored complexes formed by zinc and four triphenylusing the sodium salts of 2-(2-pyridylazo)-chromotropic methane dyes (xylenol orange, methylthymol blue, pyroacid, 2-(3-pyridylazo)-chromotropicacid, and 2-(2-carcatechol violet, glycinethymol blue) have been studied boxy-3-pyridylazo)-chromotropic acid (430). Zirconium, spectrophotometrically (61). Another spectrophotometric uranium, thorium, and the rare earths were determined sequentially using selective solvent extractions and arseinvestigation was concerned with the complexes formed nazo as the chromogenic agent (520). Calcon carboxylic, by titanium(IV) and six reagents (xylenol orange, glycineeriochrome blue SE, and diamond blue-black E B react cresol blue, chromazurol salicylfluorone, p-dimethylwith uranyl ions to give colored complexes obeying Beer’s aminophenylfluorone, methylthymol blue) (722). law (446). Carboxynitrazo reacts with cerium subgroup The color reactions involving bis(4-substituted) thiosemicarbazones of 1,2- and 1,3-diketones as extractive-phoelements of the rare earths to give colored products (625). Sulfonitrophenol S forms 1:l colored complexes with rare tometric reagents for silver, gold(III), bismuth, cadmium, cobalt, copper, mercury, manganese(II), nickel, lead, palearth metals (17). Arsenazo-p-nitro is a sensitive reagent ladium(II), thallium(I), and zinc have been reported (64). for lanthanum (553).Pyrogallol red was recommended for The potassium salt of 3-methyl-l-phenyl-5-pyrazolone-4- the determination of europium and gadolinium (12). Quiazo-1’,4‘-nitropheny1-2’ sulfonic acid reacts in a waternolylazoaminophenols, quinolylazoaminocresols, and pyriacetone-DMF medium in the presence of Bu4NOH to dedylazoaminophenols have been investigated as reagents velop a color with sodium ions (443).The complex of copfor the photometric determination of gallium and cobalt (176, 280). Palladium(I1) forms a 1:l complex with 5-[pis suitper(1) and l-isonitroso-1,2,3,4-tetrahydrophenazine able for the photometric determination of copper (603). (dimethylamino) benzylidenelrhodanine (196).In studying the complexation of palladium with several 4-(2-thiazoPotassium dodecahydro-1,2-dicarbaundecaborateforms an lylazo) resorcinol derivatives, the best reagent was 4-(5extractable complex with copper in 1-4N KOH solution (482). Copper is extracted with pivaloylacetylmethane in sulfo-2-thiazolylazo)-2-nitroresorcinol (5). Another study benzene with diethyldithiocarbamate replacing the pivaof reagents for rhodium(1) indicated that 5-sulfoallthiox loylacetylmethane prior to measurement (377). In was the most suitable color reagent (178). The formation studying the spectrophotometric properties of nickel comof colored complexes of lead, mercury, and bismuth with the sodium salt of dioxohydrindylidene-dioxohydrindiampounds formed with a variety of organic reagents, xylenol ine, their extractability into chloroform, and use in the orange was found to be satisfactory (73). Acetylated derivatives of 1-hydroxy-2-pyridinethione and l-hydroxy-4- determination of these metals have been investigated (116). Nonmetals. Many anions (Cl-, Br-, CN-, I-, SZ-, methyl-2-pyridinethione have been used as selective reS032-, SCN-, S z 0 3 2 - ) react with mercury(I1) iodate to agents for the determination of copper (211). The color liberate iodate. The reaction of this iodate with iodine to reactions of cadmium(I1) with various thiozolylazonaphform triiodide and the development of the starch-triodide thalenesulfonic acids have been investigated with molar color increases the sensitivity for the anion being deterabsorptivities as high as lo4 and conformity to Beer’s law being observed for several of the colored systems (39). In a mined (298). An indirect method for perchlorate is based on the exstudy of pyridylazo compounds as reagents for zinc, 5-(2pyridy1azo)-p-cresol and 2-(5-bromo-2-pyridylazo)-5-di- traction of a 1:l:l complex of copper(I), G-methylpicolinaldehyde azine, and perchlorate into chloroform or ethylaminophenol were found to be sensitive and suitable methel isobutyl ketone (757). I-Ephedrine was found to be (284). The thiocyanate or halide complexes of mercury(I1) a satisfactory substitute for pyridine in the silver diethylare extractable by organic solutions of xanthene dyes (pydithiocarbamate reagent used for the spectrophotometric ronine Zh, rhodamine 6 Zh, rhodamine S) (557). The use of a medium containing about 20% by volume sulfolane determination of arsenic (369). enhances the absorbance of the thiocyanato-cobalt comBorosalicylic acid and ethyl violet form a 1:l complex plex and permits extraction from nickel into nitrobenzene extractable into benzene (65).In studying various azo dye (228). Copper(1) forms a 1:l complex with bis(6-methyl- systems for the determination of nitrite, the naphthionic 2-pyridyl) glyoxal dihydrazone (756). Solochrome violet acid-chromotropic acid-nitrite reaction is applicable over Rs gives colored 1:2 complexes with zinc and cadmium a wider concentration range but is not as sensitive as the ions (168). The spectrophotometric study of azo comGriess reaction (249). pounds of 2-naphthylhydrazine derivatives as reagents for Tellurium(1V) bromide reacts with diphenylthiourea to zinc showed that a hydroxyl group in the benzene ring was form a 1:2:6 Te:DPTU:Br ion associate (451). The optimum conditions for determining tellurium as iodide comessential for color formation (337). plexes with methyl violet, brilliant green, blue basic turThe color reaction of N-glycylcomenamic acid with ironauoise. rhodamine Zh. and malachite ereen have been de( I n ) to give a red 1:l complex with an absorbance maxilineated (597). mum at 500 nm and a molar absorptivity of 9.60 x 102 ThioDvrine and two of its derivatives. l-~henvl-2.3-dihas been reported (50). 3,6-Pyridazinediol has been suggested as a specific reagent for iron(II1) (291). 2-Hydroxymethyl’-~-bromo-3-pyrazolin-5-thione and l-phenyi-2,3dimethyl-4-nitro-3-pyrazolin-5-thione, form colored com5-methylpropiophenone oxime reacts with iron(II1) to form a 3:l complex which is extractable into chloroform (582). plexes with selenium(1V)(709). 2-Mercapto-5-anilino-1,3,4-thiadiazole redcts with bisOrganic Constituents. A new spectrophotometric muth(II1) to give a yellow precipitate which is extractable method for the determination of pyruvic acid uses the into chloroform (147). Stilbazo forms a blue 1:2 complex color reaction of pyruvic acid with p-dimethylaminobenwith bismuth(II1) a t pH 2-2.3 and a red 1:l complex a t zaldehyde in dimethyl sulfoxide in the presence of a pH 6.5-7.2 (726). The color reaction of scandium(II1) with strong base (335).A formaldehyde catalyzed oxidation of rn-cresolphthalexon has been studied to delineate optip-phenylenediamine with hydrogen peroxide to form
s,
-
228R
A N A L Y T I C A L C H E M I S T R Y , VOL. 46, N O . 5, A P R I L 1974
David F. Boltz, professor of chemistry at Wayne State University, is also a science advisor for the Detroit District Laboratory of the Food and Drug Administration. He graduated from the University of Wisconsin in 1938, received an MS from the University of Missouri-Rolla in 1940, and a PhD in analytical chemistry from Purdue University in 1946. His particular fields of research include ultraviolet and light absorption spectrometry, analytical separation methods, heteropoly chemistry, and atomic absorption spectroscopy. He has been the author of 70 research papers, 15 chapters in books, and 14 reviews. In 1971 Dr. Boltz received the first Anachem Fellow Award from the Association of Analytical Chemists and the Faculty Research Award from the Sigmi Xi Chapter at Wayne State University. He is a member of the Advisory Board of Analytical Chemistry and also serves on the Editorial Board of Analytical Letters. Professor Boltz is a member of ACS, SAS, Association of Analytical Chemists, Sigma Xi, Alpha Chi Sigma, and Phi Kappa Phi.
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.
bis(2',5-diaminophenyl) benzoquinone diimine is the basis of a new method for the determination of formaldehyde (63). The charge-transfer complexes formed by primary, secondary, and tertiary aromatic amines with 1,3,5-trinitrobenzene distinguish the different amines and serve as the basis for their quantitation (646). Antipyrine, after nitrosation, reacts with 1-naphthylamine to develop a characteristic color (232).
Simultaneous Spectrophotometric Determinations. The difference in the decomposition rates of molybdotitanophosphate and molybdovanadophosphate is the basis of a simultaneous method for vanadium and titanium. Stoppin the decomposition after 1 minute by reduction with tinfiI) chloride gives the total amount of titanium and vanadium. The decomposition of the heteropoly acids in another aliquot is teminated in 20 minutes; the more stable
Table I. Spectrophotometric M e t h o d s for Metals Constituent
Ac Ag
Material
...
...
... Cyanide solns Ores Uranium A1
...
NaI-KI Rocks Steel Soils Steel
Am
...
Au
...
... ... ...
... ...
...
Method or reagent [Wavelength; molar absorptivity]
References
Arsenazo I11 [660; 3 . 8 X 1041 p - (Dimethylamino)benzylidene rhodamine [460; 3.09 x 1041 Rubeanic acid 1,lO-Phenanthroline, rose bengal A 3-Methyl-5-phenyl-2,6-dimercapto-4H-thiopyran-4-one Decolorization of copper (11) diethyl dithiocarbamate in PhMe 1,lO-Phenanthroline, pyrogallol red Aminobenzylidine rhodanine 4-(2-Thiazolylazo) pyrocatechol [510; 4 , 9 X 1041 Xylenol orange Solochrome violet R S [560, 1 . 7 X 1041 Chromazurols, OP-10 Chromotrope 2R Aluminon, gelatin Alizarine red S, 1,3-diphenylguanidinium (isoBuCOMe) [525; 2.90 X lo4] Arsenzo I11 [600; 1 . 9 8 X 1041 Methylthymol blue Solochrome azurine BS [560; 8.88 x 1061 Automatic; eriochrome cyanine R 8-Quinolinol (C6Hs) Hematoxylin Eriochrome cyanine R Phthalexon S [530; 3 . 3 3 X 1041 9- (5-Bromohydroxyphenyl)-2,3,7-trihydroxy-6-tluorone ~540;7 . 5 x 1041 Arsenazo 111, K2S208 Dithizone (CC14) 4-(Dimethylamino)phenyl-4-methylbenzylaminophenylantipyrylcarbinol Rhodamine 6 Zh (C&) Astrazon pink FG-AuCla -(CC14-C2H4C12) Chromopyrazole I (PhMe) Colloidal: 8-quinolinol o-Phenylenediamine Diantipyrylpropylmethane (C6H6) Pyronine G (C&) [528;9 . 7 X lo4] p-Dimethylaminobenzylidenerhodanine(PhN02) [535; 2 . 9 x 1 0 4 1 Methylthymol blue [500;1 . 3 X 1041 Aluminon Rhodamine B, benzoic acid (PhMe) Thorin A N A L Y T I C A L C H E M I S T R Y , VOL. 46,
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Table I (Continued) Material
Constituent
... ...
Method or reagent [Wavelength; molar absorptivity]
Cyclopentanone-2-carboxanilide(MIBK) Benzohydroxamic acid (cyclohexanone) ; Beryllon I1 2'-hydroxy chalcone
A1 alloys, steels Bi
... ...
... ...
...
Ores Lead Ca
...
Alkali metals A1 alloys Fe alloys Iron Zirconium Cd
...
Cyanide solns Ce co
.
.
I
I
.
.
...
...
Pb alloys Steel Steel
... ... Steel Reagents
...
Steel
...
Alloys
... ...
Steel ... ... Alloys Nickel salts
... ... ... 230R
Chromazurol S, zephiramine [610; 1 . 0 9 X los] 2-Mercapto-5-anilino-l,3,4-thiazole (CHCL) Differential, thiourea 2-Mercaptobenzimidazole (isopentanol) Bromocomplex, tri-n-octylamine Zinc dibenzyldithiocarbamate (ccl4) [370; 1 . 2 X 10‘1 Astrazon red F G (CsHrMe2CO) Thiothenoyltrifluoroacetone (CCln) [460; 5 . 6 X lo3] 9- (2-Hydroxyphenyl)-2,3,7-trihydroxy-6-fluorene [520; 2.57 X l o 4 ] 2-Mercaptopyridine Methylthymol blue [584; 6.99 X lo3] 2-Mercapto- A2-1,3,4-thiadiazoline-5-thione 1,lO-Phenanthroline, ascorbic acid, iodide (cyclohexane) Iodide, 3-(p-diethylaminophenylazo)-1,4-dimethyl-l,2,4triazolinium chloride (CeHsPhNO,) Xylenol orange Oxine; diazonaphthoic acid Anthrapurpurin complexon Rhodizonate Kinetic: ligand substitution of Cu(I1)-EGTA with PAR Glyoxal bis(2-hydroxyanil) Glyoxal bis (2-hydroxyanil) Chlorophosphonazo I11 Chlorophosphonazo I11 Methylthymol blue Murexide 6-Bromobenzothiazole-(2’-azo-2)-4-methylphenol (CHCl,) ~610;4.92 x 1041 Solochrome violet R S Methylthymol blue [610; 8 . 9 X 1031 1-[ (5-Chloro-2-pyridyl) azo 1-2-naphthol (CHC13) [566; 6 . 6 X l o 4 ] Dithizone (CHCL) Solochrome azurine BS [505; 1 . 1 X 1041 Beryllon I1 [610; 2.15 X l o 4 ] Sulfosalicylic acid a-Benzil monoxime (CHCla) [390; 2.25 X lo4] Na p - (2-Hydroxy-1-naphthylazo) benzene sulfonate [357; 2.68 X l o 4 ] o-Mercaptobenzoic acid [570;1.65 X 1041 Sulfosalicylic acid 4-(2-Pyridylazo)resorcinol[510; 5 . 6 X lo4] Triphenyltetrazolium thiocyanate (CHC13) 4-(2-Pyridylazo) resorcinol,. zephiramine (cHc13) [536; 6 . 2 x i o 4 1 2-Nitroso-5-dimethylaminophenol (1,2-dichloethane) [456; 6 . 0 x 1041 2- (2-Thiazolyazo) -5-diethylamino-rn-phenol p80; 6 . 4 x 1041 2,4,6-Tris(2-pyridyl)-s-triazine[485; 2 . 8 X l o 3 ] 1-(2-Quinolylazo)-2-phenanthrol [550; 5.12 X l o 4 ] N-Hydroxy -N-phenyl-N’-p-naphthylthiourea Bromopyrogallol red [620; 1 . 6 X 1041 Quinoxaline-2,3-dithiol [540; 5.15 X lo4] 2-Nitroso-5-dimethylaminophenol (1,2-dichloroethane) [456; 6 . 0 x 1041 1-(2-Pyridylazo)-2-phenanthrol Thiovioluric acid [413; 6 . 4 X l o 4 ] N-Methylanabazine-a’-azo-p-cresol[565; 1 . 9 0 X 10‘1 Disodium ethyl bis (1H-tetrazol-5-ylazo) acetate Nitroso-R-salt, diphenylguanidine (CHClI) Thiothenoyltrifluoroacetone (CCl,) [490; 8.96 X lo3] EDTA 2-Pyridyl-2-thienylketoxime(CHC13) Methylthymol blue [610; 1 . 2 X lo6] Quinolineazo R 2-Nitroso-5-dimethylaminophenol (1,2-dichloroethane) 6 . 0 x 1041 N,N’-Bis(thiosalicy1idone)ethylenediamine (CHCla) Isonitrosoacetophenone (CHC13) [390; 2.82 X l o 4 ] Nioxime (amyl a1c.-CHClr) [470; 9.84 X l o 3 ]
ANALYTICAL CHEMISTRY, VOL. 46, NO. 5, APRIL 1974
Table I (Continued) Constituent
Material
... Cr
cs cu
... Steel
...
... ... ... .. Alloys Steel ... Aluminum ... Bismuth
Alloys ... Steel Alloys Al, Zn Alloys ...
... Electrographic deposits ... CSCl Eu Fe
... ...
...
...
Method or reagent [Wavelength; molar absorptivity]
PAR, zephiramine (CHC13) [520; 5 . 8 X 1041 Violuric acid [390; 3 . 2 X 1041 l , l ,1-Trifluoro-4 - (2-thienyl)-4-mercaptobut-3-ene-2-one (cyclohexane) [480; 5.5 X 1031 3-Thianaphthenoyltrifluoroacetone[460; 1 . 3 X 1031 Triethylenetetraminehexaaceticacid Indirect: pptn. with NaBPh4; 1,l‘-dianthrimide [620; 1.65 x 1041 2- [5-(3-Carboxy-1H-1,2,4-triazolyl)azo ]-1,8-dihydroxy-3,6naphthalenedisulfonic acid [640; 2.24 X 1041 Picolinaldehyde thiosemicarbazone [360; 2 . 0 X lo4] 1-Pyrrolidine carbodithoate (CHC13) [435; 1 . 3 5 X l o 4 ] 3-Thianaphthenoyltrifluoroacetone [410; 9 . 3 X lo2] 8-(p-Ethylbenzenesulfonamide)quinoline (CHCL) ~380;1.58 x 1041 4-Isonitroso-l-phenyl-3-methylpyrazolin-5-one (CHC13) [395; 6 . 9 9 X 1031 1-(2-Quinolylazo)-2-phenanthrol(CHC13) [590; 3.84 X l o 4 ] 3,5-Diphenylpyrazolidithiocarbamatedisulfide (CHCl,) 2,2’-Biquinoline 4,4’-Bis (p-carbethoxyanilino)-2,2’-diquinolyl (BuOH) 1556; 1 . 7 X 10‘1 Automated Ligand exchange, Cu oxinate-dithizone (CHC13) 2- (0-Hydroxyphenyl) benzoxazole [370; 2.5 x 1041 2-Thioxo-5-mercapto-1,3,4-thiadiazolidine Diethyldithiocarbamate (C&) Isoamyl 2-(2-quinolyl)cinchoninate[566; 8 . 6 1 X 1031 2- (3-Carboxy-5-triazolylazo)-2-hydroxy-S-amino-3,6naphthalene disulfonic acid [610; 1 . 6 6 X 1041 Sulfarazen [500;4 . 0 X 1041 Acetoacetanilide (CHCl,) [340; 1 X 10x1 Antimony dibenzyldithiocarbamate(CC14) 8-Hydroxyquinoline-5-sulfonic acid, zephiramine (CHC13) [4io; 9 . 4 5 x 1031 2- [ (3,5-Dibromo-2-pyridyl)azo]-5(diethylamino) phenol [560; 5 . 6 5 X l o 4 ] 2- (8-Pyridylazo)-1-naphthol 5 - (3,5-Dibromo-2-pyridylazo) -2-ethylamino-p-cresol ~545;4 . 8 5 x 1041 Potassium dodecahydro-1,2-dicarbaundecaborate (Bu3POa-MeCOEt) [490, 2 . 8 x 1 0 4 1 Copper(1)-2,2‘-biquinolyl(Bu0H) Rubeanic acid Catalytic oxidn. of amidol Pivaloylacetylmethane; diethyldithiocarbamate (C&) 2-(5-Nitro-2-pyridylazo)-naphthol (CHC13) [598;8 . 6 X l o 4 ] Kinetic; amidol, hydrogen peroxide Triethylenetetraminehexaacetic acid Chrome azurol S PAR, zephiramine (CHCl,) [522; 4 , 5 X l o 4 ] Sodium N-(sulfobenzoyl)-N-phenylhydroxylamine [450; 4.1 x 1031 Exchange reaction; zinc acetylacetonate (dioxane) [440; 3.84 X l o 3 ] 2,2’-Dipyridyl-cu-glyoxime1534; 1 , 3 3 X 1041 Benzoylacetanilide Pyrocatechol violet [610; 6.24 X 1041 Quinoxaline 2,3-dithiol (450; 1 . 0 X 1051 4- (6-Methoxy-3-methylbenzothiazolylazo)-N-methyl diphenylamine-FeC1:- Ic6H,-PhNo2) [643; 7 . 8 X 104) Gallein, cetylpyridinium chloride 2,3,5-Triphenyltetrazoliniumchloride PAR [500; 5 . 6 X 1041 Bipyridylglyoxal dithiosemicarbazone
Aluminum
N,N’-Dimethylthiolatidinarnide 2-Carbethoxy-5-hydroxy-l(4-tolyl) -4-pyridinone (CHCI,)
Water
Pyrrolidinecarbodithioic acid [600; 3 . 7 X 1041 Thiothenoyltrifluoroacetone [490; 2 . 4 5 X l o 4 ]
[432; 7.45 x 103)
Steel ... ...
Acetylacetone, pyridine, benzene 2-Benzoyl-3’-nitroacetanilide[530; 2.05 X Pivaloylacetylmethane (CsH,) [435; 4 . 3 x
lo3] 1031
A N A L Y T I C A L C H E M I S T R Y , VOL. 46, N O . 5, A P R I L 1974
231 R
Table I (Continued) Constituent
Material
Method or reagent [Wavelength; molar absorptivity]
Pyrocatechol violet
water Water ...
Ga
...
...
Alumino-silicates ...
... ...
Bauxite ... ...
Gd Ge
...
... ... Hf-V alloys
Hf
Mo alloys Hg
...
...
...
Copper ... ...
In
...
... ... ...
Ir
Americium
K Lanthanides La
Lu Mg
... .. ... ,
,..
Aluminum 232 R
2,2'-Dipyridyl-p-glyoxime(CHC13) [558; 1 . 9 X 1041 2-Hydroxy-6-methylpyridine-3-carboxylic acid ~410;5 x 1031 2,6-Diamino-5-nitroso-4-pyrimidinol [653; 2 . 0 x 1041 Hydroxyiminoacetylacetone [600; 2.85 x 1041 7-Nitro-8-quinolinol-5-sulfonic acid [550; 4 . 9 X 1031 Phthalexon S [530; 2.75 X 1041 Bathophenanthroline (BuOH) [533; 2.03 x 1 0 3 1 Morin, antipyrine, perchlorate (CHCIS Pyronine Pyrocatechol violet, cetylpyridinium bromide (BuOH) 1600; 8 . 7 x 1041 Chromotrope 2R [580; 1 . 7 X 1 0 4 1 1-(2-Thiazolylazo)-2-naphthol-3,6-disulfonic acid Magneson (BuOH) Janus green-GaClr-iC6H6-Me*co) [640; 8 . 7 5 X l o 4 ] Pyridylazoaminophenol Astrazon blue 5 GL (C6H6-MeCOEt) Alizarin red S,1,3-diphenylguanidine (BuOH-C6H6) ~525;2 . 9 x 1041 Methylthymol blue [600; 1 . 7 X 1041 Pyrocatechol violet, diphenylguanidine (CHCI,) ~600;1 . 0 8 x 1051 Sulfonitrophenol azurin Solochrome violet RS [565; 5 X 1041 Astrazone rose FG (C6H6-MeCOEt) Methylxylenol blue [553; 2.02 x 1 0 4 1 Toluylene blue (C6H,-Me&O) Diphenyltetralylmethane 4-(2-Pyridylazo) resorcinol [516; 8 . 8 9 X l o 4 ] Gallein, cetylpyridinium chloride Alizarin red S Molybdogermanic acid, rhodamine C (560; 3 . 6 8 X 1051 3,5-Dinitropyrocatechol, brilliant green (CCL) [625; 1 . 4 1 X lo5] Alizarin red S 12-Molybdovanadohafnium heteropoly blue [ n o ; 3 . 4 x 1031 Arsenazo Brilliant green, iodide jC6H6) [640; 1 . 0 X lo5] Thiothenoyltrifluoroacetone (CCl,) Halide complex, brilliant green [640; 1 . 2 X 1051 Chlorocomplex, methyl green (PhMe) [640;1 . 3 1 X lo5] Iodocomplex, victoria blue B (C6H6) [634; 7 , 8 X lo4] Bromide, 4- (6-methoxy-3-methyl-benzothiazolium-2ylazo) -N-methyl-diphenylamine chloride (PhMecyclohexanone) Phthalexon S [570; 1 . 6 2 X l o 4 ] Bromide, victoria blue B (C6H6-EtOAc) 4-(2-Pyridylazo) resorcinol Crystal violet (PhMe) Xylenol orange, tri-n-octylamine (CHCl,) Xylenol orange, diphenylguanidine (CHC13-isoamyl alc.) [MO; 1 . 2 x 104 1 Diantipyrylmethane, .S-quinolinol (CHC13) 1-(2-Thiazolylazo)-2-naphthol-3,6-disulfonic acid N-Methylanabasine-a'-azoazotolXA [CHCl,] [mo; 3 . 3 x 1041 Thiothenoyltrifluoroacetone [480; 6 . 7 X l o 3 ] Xylenol orange [570; 3 . 3 X l o 4 ] Astrazon blue 5GL (C6Hs-MeCOEt) [640; 1.1 X lo4] Oxidn. of N,N'-di (2-naphthyl)-p-phenylenediamine by I r (IV) Tin(I1) chloride Indirect: pptn. with NaBPh4, 1,l'-dianthrimide Methylxylenol blue, cetyltrimethylammonium bromide Antipyrine S [735; 1 X 165] Arsenazo-p-nitro [665; 6 . 2 X l o 4 ] Cresolphthalexon, cetylpyridinium bromide [607, 6.5-7 X l o 4 ] Sulfoalizarine B, ammonia 1BuOH) [530; 3 . 2 X lo4] 8-Quinolinol, pyridine (ClCH&H2C1) Methylthymol blue [610; 1 . 5 X l o 4 ] 7- [ a-Co-Methyoxycarbonylanilino)benzyl 1-8hydroxyquinoline [400; 8 X lo3]
A N A L Y T I C A L C H E M I S T R Y , V O L . 46, N O . 5, A P R I L 1974
References
Table I (Continued) Constituent
Material
Beryllium oxide Cast iron Iron Mn
...
Titanium dioxide Mo
.
I
.
... Ores Steel Steel Alloys Steel ... ...
... ...
Ferromoly bdenum Steel Steel Na
...
Nb
,..
Method or reagent [Wavelength; molar absorptivity]
References
8-Quinolinol (CHCl,) Sodium 5- (3-nitrophenylazo) salicylate Titan yellow 5,7-Dichloro-8-hydroxyquinoline, rhodamine 6G (CsH,) N-Methylanabasine-a‘-azoazotolOA (CHC13) [NO; 5 . 2 x 1041 Dithizone, pyridine (cc14) 1-(2-Pyridylazo)-2-naphthol (CHC13) -4-hydroxybenzene3- (3-Methyl-l-phenyl-5-py1azolon-4-yl) sulfonate 1530, 4 . 2 X l o 3 ] Thiocyanate, crystal violet (PhMe) Thiocyante [470; 1 . 5 6 X lo4] Pyrocatechol, butyltriphenylphosphonium cation (CHCl3-CH,Clz) Mo(V)-8-quinolinol, pyridine [405, 4 . 4 X l o 3 ] Solochrome dark blue G Chloropromazine, thiocyanate (CHClJ Tiron, zephiramine (CHCl3) Indoferron, diphenylguanidine (CHC13) [555;1 X 1041 1,lO-Phenanthroline, thiocyanate 3,5-Diphenylpyrazolinedithiocarbamate
Unithiol Thiocyanate, N-benzylaniline (CHC13-isoamylalc.) Chrome black special Thiolactic acid Disodium cis-1,2-dicyanoethylene-1,2-dithiolate [665; 5 . 0 5 X l o 3 ] p(Dimethy1amino)phenylfluorone [540;2 . 0 x 1041 Carminic acid [565; 1 . 4 X 1041 Crystal violet, thiocyanate Gallobenzophenone Dimedrol, pyrocatechol (CHCl,) Differential; redn. with hydrazine sulfate Pyrocatechol violet (PhMe) [545; 2.02 X 1041 Sulfonitrazo Potassium 3-methyl-l-phenyl-5-pyrazolone-4-azo-l’,4’nitrophenyl-2’-sulfonate
...
Alloys Alloys Ores Ores Steel Steel Nd Ni
...
... ... ...
Magneson [540; 1 . 6 X l o 4 ] Pyrocatechol, thiocyanate, l-phenyl-3-methyl-4benzoyl-5-pyrazolone [414, 7 . 8 x 1031 Pyrocatechol, thenoyltrifluoroacetone (CHC13) [4i4; 7 . 7 x 1031 Chloranilic acid Pyrogallol red Benzenesulfohydroxamic acid (CHC13) [320; 1 . 0 8 X Alizarin red S 4-(2-Pyridylazo)resorcinol [540; 1 . 7 X l o 4 ] 5- (2-Thiazol ylazo) -2- (ethylamino)-p-cresol Rezarson [510; 1 . 9 4 X 1041 Sulfochlorophenol S 1-(2-Pyridylazo)-2-naphthol 4- (2-Pyridylazo)resorcinol Bromopyrogallol red, or pyrogallol red 2-Amino-5- (2-hydroxynaphthylazo)-1,3,4-thiadiazole [570; 1 . 6 5 X l o 4 ] Bromopyrogallol red [620; 2 . 9 X 1041 Dimethylglyoxime(naphtha1ene) (CHC13) 1375; 3 . 0 1 x 1031 Diethylaminoethanethiol hydrochloride Methylthymol blue, zephiramine [625; 2 . 9 X 1041
1041
3-Nitroso-4-hydroxy-5,6-benzocoumarin
... NP
...
OS
Pb
[395; 2 . 4 8 x 1041 4- (5-Sulfo-2-thiazolylazo)-2-nitroresorcinol [510;6.51 X 1041 Picolinaldehyde thiosemicarbazone [385; 1 . 9 X 1041 Thiothenoyltrifluoroacetone (CCI,) Thionaphthenic acid (CCl,) Hydrogen peroxide [430; 5 . 0 X l o 3 ] Arsenazo M [664; 1.18 X l o j ] Oxidn. to Np(VI1) with K2S208 2-Amino-8-naphthol-3,6-disulfonic acid Bismuthiol I1 (EtOAc)
...
3-Hydroxy-5-mercapto-6-hexyl-1,2,4-triazine
...
2- (0-Hydroxyphenyl) benzothiazoline (PhMe) Bromopyrogallol red [630; 5 X l o 3 ]
...
A N A L Y T I C A L C H E M I S T R Y , VOL. 46, NO. 5, A P R I L 1974
233R
Table I (Continued) Constituent
Steel ...
Pd
,..
... ...
... Catalysts
... Organo-Pd Compds.
...
...
...
... ...
Pt
... Americium ... Fuel solns.
Pu Rare earths
Method or reagent [Wavelength; molar absorptivity]
Material
... ...
Semiconductors
...
Rb Re
... ... Alloys Cu ores Ni-Mo alloys Rh
References
Glycinecresol red Oxalyl dihydrazide l,l,l-Trifluoro-4- (2-thienyl)-4-mercaptobut-3-en-%one (CC14) Iodide Zincon, urotropine [595; 2 . 6 X lo4] 2-Mercaptopyridine Diacetyl monoxime-2-benzo-thiazolylhydrazone(CHCl,) 1-(5-Bromo-2-thiazolylazo)-2-naphthol (CHCI,) 1690; 1 . 4 x 1041 2,2’-Diquinolyl ketoxime (C&) [478; 1 . 3 X 10‘1 p-Dimethylaminobenzylidenerhodanine (FhNO,) 1535; 4 x 1041 1-Phenyltetrazoline-5-thione(CH.Cl3) 2,6-Diamino-3,2’-azopyridine1620; 1 . 4 X l o 4 ] Azide, methylene blue (CHCl,) 1653; 5 . 8 X l o 4 ] Pontachrome azure blue B [605; 4.79 X l o 4 ] Palladiazo N-Methylanabasine-a-azoguaiacol,[600; 215 X 1041 or pyridylazoguaiacol [6.0; 2 . 3 X lo‘] 5- [p-Dimethylamino)benzylidonelrhodanine [515; 4 . 8 8 X l o 4 ] Methylthymol blue 1530; 2 . 1 X l o 4 ] Thiooxine (CHC13) 4- (5-Sulfo-2-thiozolylazo)-2-nitroresorcinol Eriochrome cyanine R , tetradecyldimethylbenzylammonium bromide Nicotinaldehyde thiosemicarbazone 1-Benzoyl-4-R-thiosemicarbazides Xylenol orange or methylthymol blue 1590; 1 . 7 X 1041 1620; 1 . 5 X l o 4 ] Phthalic acid monothioureide Tropolone (CHCI,) [395; 1 . 8 9 X 1041 Bromide complex Cadion (CHC13) 1473; 4.22 X 10‘1 1-Benzoyl-4-thiosemicarbazide o-Phenylenediamine [703; 9 . 8 3 X l o 4 ] Rubeanic acid, gelatin Acenaphthenequinone monoxime [390; 9 . 0 X 1031 Thiosalicylamide (CHC13) 1430; 1 . 2 3 X l o 3 ] Rhodanine- (5-azo-1)-2-hydroxy-3-sulfo-5-chlorobenzene Tin(I1) chloride Arsenazo I11 Arsenazo I11 Arsenazokhimdu Beryllon I1 Eriochrome cyanine R, 1,lO-phenanthroline Methylthymol blue, diphenylguanidine (isoamyl alc.) [610; (27-40) X l o 3 ] Differential; stilazokhimdu 2-Phenylquinoline-4-carboxylic acid, rhodamine B (C6H6) Indirect; pptn. with NaBPhd, 1,l’-dianthrimide [620; 1 . 6 5 x 1041 Diantipyrylpropylmethane, diphenylcarbazide (CHCl,) Methylene blue perrhenate (1,2-dichloroethane) [658; 1 . 0 X lo6] Morpholinium morpholine-N-dithiocarbamate [344; 4 . 6 X l o 3 ] Antipyrine, thiocyanate (CHC1,) Thioglycolic acid i450; 1 . 5 X l o 3 ] Thioglycolic acid, antipyrine (isoamyl alc.-CHC13) a,a’-Dinaphthylthiourea, tin(I1) chloride fCHC13) Thioglycolic acid, diantipyrylmethane [460; 1 . 7 X l o 4 ] Thiourea, tin(I1) chloride 8-Alkylthioquinoline, ascorbic acid [400; 7 X l o 3 ] 4-Amino-5,7-disulfo-2,1,3-benzothiadiazole 5-Sulfoallthiox [430; 7.0 X lo3] 1-(P-Thiazolylazo)-2-naphthol(CHCl~)[630; 1 , 1 9 X
Ru
... ... ...
234R
Diphenylcarbazone [530; 1 . 6 2 X l o 3 ] Diphenylthiovioluric acid Thiovioluric acid [540; 2 . 2 X lo‘] o-Hydroxythiobenzhydrazide [540; 1 . 3 8 X Kinetic: oxidn. of anisidine with Mn(II1)
A N A L Y T I C A L C H E M I S T R Y , V O L . 46, NO.
5,
A P R I L 1974
lo4]
lo4]
Table I (Continued) Constituent
... Sb
... ...
...
Lead Rocks Steel Steel sc
.
I
.
...
... Sm Sn
... ... ...
Rocks Steel Steel Ta
Zircaloy ...
... Th
Ti
... ...
iiioYs Mg alloys ...
... ...
...
...
T1
Method or reagent [Wavelength; molar absorptivity]
Material
Bitumen A1 alloys Soils Steel Ores ... ...
o-Tolidine Ruthenate [465; 1.88 X Brilliant green (PhMe)
lo3]
l-(2-Quinolylazo)-2-naphthol (CHCI,) Basic turquoise-chlorostibate (C&) [648; 3 X l o 4 ] Dimethylthionine (Dichloroethane-trichloroethylene) [640; 4 . 9 x 1041 or Trimethylthionine [655; 8 . 1 X 1041 1-(2-Pyridylazo)-2-naphthol (CHCL) N-Methylanabasine-0’-azodiethylaminophenol [GOO;3 . 0 x 1041 4- (N-Methyl-2-anabasineazo)-resorcinol [540; 1 . 0 6 X 1041 Janus green S b C k (CaHs) [600; 1 18 X 10’1 Propylfluorone [540; 5 . 7 2 X l o 4 ] Pyrogallol red [420; 4 . 5 X l o 3 ] Phen ylfluorone Rhodamine B Methylfluorone Methylene blue (CHCl,) Azophosphon [415; 1.36 X 1041 Diantipyrylmethane, sodium 2- (4-sulfophenylazo)1,8-dihydroxy-3,6-naphthalenedisulfonic acid [BO; 2.13 x 1041 Methylxylenol blue 2-Phenylquinoline-4-carboxylic acid rhodamine S (C&) Beryllon I1 [635; 2.0 X 1041 2-(o-Hydroxyphenyl)benzothiazoline r PhMe) [415; 1 . 7 X 10’1 3,5-Dinitropyrocatechol, brilliant green (CHC13-C6H6) 1630; 1.75 x 1051 Phenylfluorone, oxalic acid, cetylpyridinium chloride Pyrocatechol violet Trihydroxyfluorones, antipyrine (CHCI,) Phenylfluorone Phenylfluorone Catechol violet, cetyltrimethylammonium bromide ~662;9.2 x 1041 Phenylfluorone Acridine orange NO-TaF6 - (C2H4Cl,-CHC13) [ ~ o o4; . 3 x 1041 Ethyl violet (C&) Pyrogallol red, complexon I11 Arsenazokhimdu [582; 8 . 0 X 1031 Bromophthalexon, or p-xylenolphthalexon S Carminic acid, trichloroacetic acid (BuOH) Chlorophosphonazo I11 (3-Me-1-butanol) [670; 1 . 2 x 1051 Nitroso-4-hydroxycoumarin [419; 1 . 0 3 X lo2] Purpurin (BuOH) Phenylthiazolylazochromotropic acid [630; 3 . 0 X 1041 2-(2-Pyridylazo)-l-naphthol[582; 1.74 X 1041 Molybdotitanophosphoric acid Quercetinsulfonic acid Hydrogen peroxide, 8-quinolinol (CHC13) Hydrazo 11, diphenylguanidine (CHCI,) [530; 5.26 x 1041 Eriochrome cyanine, or gallocyanin N-Benzoyl-N-p-tolylhydroxylamineICHCl,) Redn., titanomolybdophosphoric acid [820; 6 . 0 X 1031 Pyrocatechol, pachycarpine (CHCl,) [390; 1 . 0 3 X 1041 Tiron - ._ Tribromopyrogallol, antipyrine 1CHCl3-isoamyl alc.) [400; 1 . 1 7 X l o 4 ] TGon (BuOH) [3851 1 . 4 X l o 4 ] Ti (IV), tetrabromopyrogallol, antipyrine [400; 1.44 X l o 4 ] Eriochrome B Diantipyrylmethane 2-Hydroxy-5-carboxyphenylfluorone [465; 6 . 9 6 X 1041 Diantipyrylmethane [390; 1 . 4 X 1041 Pyrogallolsulfonic acid, diphenylguanidine, or antipyrine 2-Methylisonicotinic acid salicylalhydrazide Brilliant green (PhMe) Crystal violet (CsH6) Tetraline areen-T1Br - I 1C6Ho-MeCOEt) . . [620; 4.-31 X l o 4 ] Astrazon pink F G (C6H6-MeCOEt) [620; 4.31 X l o 4 ] ~
~~
~
A N A L Y T I C A L C H E M I S T R Y , V O L . 46, NO.
5.
A P R I L 1974
235R
Table I (Continued) Constituent
... ...
U
P b Alloys Zn Alloys ...
... R. E. elements Minerals
...
... ... V
...
... Alloys Silicates Steel ... ...
... Ores
...
... Steel ... ... Bauxite
...
Slag ...
...
Ilmenite ...
Copper ores ...
... Steel Soils ... 236R
Method or reagent [Wavelength; molar absorptivity]
Material
Copper(I1) diethyldithiocarbamate fCC1,) [436; 1.96 x 1041 Neutral red-T1Br4- (CsHs-MeCOEt) [540; 6 X l o 4 ] Pyronine G-TlBr4- (C&) [520; 8 . 1 7 X l o 4 ] Thiocyanate, pyridine 1-(2-Thiazolylazo)-2-naphthol-3-carboxylic acid [598; 2.35 X l o 4 ] 2-(4-Antipyrylazo)-5-diethyl-m-aminophenol (CHC13) Triphenyltetrazolin chloride, crystal violet (C6H.6) Rhodamine B Chlorophosphonazo 111, (3-Me-1-butanol) [673; 1 . 2 X 1051 Pyrocatechol, aniline (CCl,) Arsenazo 111, dodecyloctylmethylbenzyl ammonium chloride (CHCl,) Arsenazo I11 Glycinecresol red [470; 8 . 6 X lo3] p-Nitrophenylfluorone 2- (5-Bromo-2-pyridylazo)-5-diethylaminophenol 7-Chloro-8-hydroxyquinoline-5-sulfonic acid [355; 6 . 6 X l o 3 ] Gallacetophenone [380;6 X l o 3 ] Chromazurol S, cetylpyridinium bromide [625; 9 . 9 x 1041 Solochrome azurine BS [600; 2.25 X l o 4 ] Thiothenoyltrifluoroacetone (CC14-BuOAc) p-Nitrophenylfluorone [530; 2 . 2 X 1041 Chlorophosphonazo (BuOH-PhCH20H) 3-Thianaphthenoyltrifluoroacetone (C6H6-EtOH) [408; 1 . 7 x 1041 Brilliant green, benzoic acid (PhMe) [640; 9.34 X l o 4 ] Eriochrome cyanine R , cetyltrimethylammonium bromide (CHC13) Decolorization of metanil yellow by U(II1) Potassium iron(II1) cyanide Phenylacrylic acid, rhodamine S (C&) 2- (5-Bromo-2-pyridylazo)-5-diethy laminophenol (tri-n-octyl-phosphine oxide-cyclohexane) 4-Phenyl-7,8-dihydroxycoumarin [600; 8 . 8 X 1103] Stilbazo [510; 5 . 4 X l o 4 ] N- (0-Sulfobenzoyl sodium salt-N-phenylhydroxylamine [450; 2.62 X lo3] PAR or PAN Eriochrome B Methvlthvmol blue 1560: 1 . 8 6 X 1041 . 3-Pyridylhorone [569; i . 3 x lo5] Sulfonitrazo 1-(2-Pyridylazo) azotol OT(CHC13) 2-Hydroxy-3-naphthohydroxamicacid (octyl alc.) Thiocyanate (BuOH-EtOAc) 5- (4-Antipyrinylazo)-2 (ethylamine) p-cresol [520; 2.25 X l o 4 ]or 2-(4-antipyrinylazo)-5 (diethylamine) phenol [530; 2.85 X lo4] Phthalocyaninetetrasulfonic acid Benzohydroxamic acid Bis (6-methyl-2-pyridyl)glyoxal dihydrazone (PhN02) [440; 8 . 7 x 1031 Veratrole [500; 1.1 X l o 3 ] Sulfonitrazo [582; 2 . 1 X l o 4 ] N-m-Tolyl-o-methoxybenzohydroxamicacid (CHC1,) Thiosalicylamide or thiosalicylic acid [390; 6 . 3 3 X l o 3 ] [400; 8 . 6 7 X l o 3 ] 1,lO-Phenanthroline [645; 8 . 0 X lo3] 8-Quinolinol-5-sulfonic acid, zephiramine (CHCL) Tungstovanadophosphoric acid Eriochrome cyanine, or gallocyanine 8-Quinolinol, azide (C&) [415; 8 . 6 5 X l o 3 ] N-Acet ylsalicyloyl-N-phenylhydroxylamine Eriochrome green B [595; 2 , 1 7 X l o 4 ] 4-(2-Pyridylazo)resorcinol[545; 3 . 4 X l o 4 ] 4- (2-Pyridylazo)resorcinol, tetraphenyl phosphonium chloride (CHC13-Me2CO) 4- (2-Pyridylazo)resorcinol Pyrocatechol, pyridine N-oxide (C2H:CL) Tungstovanadophosphoric acid (isoamyl alc.) 3,5,7,4'-Tetrahydroxyflavone[425; 1 . 3 8 X l o 4 ]
A N A L Y T I C A L CHEMISTRY, VOL. 46, NO.
5 , A P R I L 1974
Table I (Continued) Constituent
TiC14
W
... ...
Niobium
Y
...
Yb
... ...
Zn
,..
...
Zr
Method or reagent [Wavelength; molar absorptivity]
Material
A1 ‘Alloys A1 Alloys Mg Alloys Silicates Steel Tellurium Zinc oxide ...
... ...
Mo alloys
...
... ... T i Materials Ni alloys Steel
...
... Steel Ores Steel
References
4- (2-Pyridylazo) resorcinol Redn. of molybdovanadophosphoric acid (MIBK) [ ~ o o2; . 3 x 1041 Pthalexon S [540; 2 . 1 X l o 4 ] Quinalizarin [530; 7 . 9 X lo3] Sulfonitrophenol M [650; 3 , 0 8 X lo4] Zinc dithiol (CHCl,) [645; 2 . 8 X 1041 Pyrocatechol violet Disodium cis-1,2-dicyanoethylenedithiolate [570; 5 . 5 2 X loa] Dithiol (AmylOAc) Arsenazo I [560; 4.38 X l o 4 ] Arsenazo M [645; 6 . 7 5 X lo4] Borodisulfophenylfluorone [550;4.25 X lo4] Glycinecresol red [540; 1.88 X lo4] Methylxylenol blue Xylenol orange diphenylguanidine (CHClr-isoamyl alc.) [582; 6 . 2 5 X 1041 Chromotrope 2R [570; 2 . 5 X 1041 Borosulfoalizarin, ethylenediamine [510;4 . 1 1 X l o 4 ] Solochrome violet R S 2- (5-Bromo-2-pyridylazo) -5-diethylaminophenol (CC1,) [MO; 8.5 x 1041 Xylenol orange [570; 3 . 1 X lo4] 2- (Salicylideneamino) thiophenol (CHC13) [415;1 . 0 7 X l o 4 ] Dithizone (PhMe) Sulfarsazen Malachite green, thiocyanate (C6Ho) 8-Mercaptoquinoline (PhMe) [565; 2.62 X 1041 2- (N-Methylanabasine-a’-azo)-p-cresol Methylthymol blue [584;1.38 X lo4] Dithizone (PhMe) Indirect; 1,10-phenanthroline Benzoic acid, rhodamine B (C&) [551;4 . 9 X l o 3 ] 3,5,7,3’,4’-Pentahydroxyflavone-6’-sulfonic acid Phthalexon S [530; 1 . 7 3 X 1041 Bromopyrogallol, cetylpyridinium bromide Methylxylenol blue [573; 4.06 X l o 4 ] Methylxylenol blue, zephiramine [627; 4 . 3 X lo6] Arsenazo 2-Hydroxy-5-nitrobenzeneazo-2-naphthol
Stilbazo [585;5 . 6 X 1041 Arsenazo Magneson IREA (BuOH) [570; 8.46 X lo3] Gallocyanin MB Arsenazo 2’-Quinolylfluorone [539; 1.65 X lo5] Arsenazo Acid chrome violet K [560; 5 . 5 X 1031 Solochrome azurine BS [545; 1 . 0 9 X 1041 Arsenazo I11 1,8-Dihydroxy-2-[2- (4-phenylthiazolyl)azo]-3,6naphthalenedisulfonic acid (620; 2.20 X 10‘1 Picramine-e Pyrocatecholsulfonthalein [655; 3.75 X lo4]
molybdovanadophosphate gives the color. Titanium is calculated on the basis of the difference in absorbance values (484). Molybdenum (VI) is reduced by thioglycolic acid, complexed with thiocyanate, and extracted into butylacetate. The tungsten(V1) is then reduced with titanium(II1) chloride, complexed with thiocyanate, and extracted, thus permitting the determination of molybdenum and tungsten in one sample (736). Cobalt and nickel are determined by a simultaneous spectrophotometric method based on the formation of EDTA complexes. When the amount of nickel is much larger than the cobalt, the cooalt(II1)-EDTA is formed instead of the cobalt(II)-EDTA complex (767). A simultaneous method for the determination of palladium(II), rhodium(III), and platinum(I1) based on pH and temperature control and using 1-(2-pyridylaz0)-2-naphthol in dimethylformamide solution has been developed (225).
The fact that palladium readily forms an extractable complex with 1-(2-pyridylazo)-2 naphthol while platinum requires heating to form an extractable complex with PAN serves as the basis of a method of analysis for such binary systems (319). Another simultaneous method for palladium and platinum utilizes chlorofurthizone with measurement of the absorbance a t 390 nm and 450 nm (350). Nickel(II), copper(II), and palladium(I1) ions are determined in the presence of each other by using 1-(0carboxyphenyl)-3-hydroxy-3-phenyltriazeneas the chromogenic reagent. After measurement of the absorbance a t 410 nm due to the palladium and copper, oxalate is added to eliminate the absorbance due to copper. In the presence of thiosulfate the absorbance of the nickel complex is measured a t 420 nm (431). Molybdenum and tungsten can be determined simultaneously using o-xylene 4,5-dithiol (303). The simultaneous determination of barium and
A N A L Y T I C A L C H E M I S T R Y , V O L . 46,
NO. 5, A P R I L 1974
237R
Table 11. Spectrophotometric M e t h o d s for N o n m e t a l s Material
Constituenl
As
...
B
Antimony Gallium or antimony chlorides Steel Steel Zinc ...
...
A1 'alloys Geological Mineral acids Steel Steel Br Alkali halides ...
Br03c102 -
...
c10, Biological fluids Potassium chlorate ...
CN -
co
FHz0
Ro'cks Acetone Organic solvents ... ...
KO2 I-
... ... ...
Water ...
I03 -
I04 N "3()
Organic Si Compds. Steel Steel
NO2 ~
(
~
... 0
~
3
-
1
Alloys Furnace gas Nitrates Solns. contg. NTA, EDTA Iron Steel Steel p30io3-
SI-
... Tin plate
SO? (SO32 -1
...
so,= ...
...
238 R
Method or reagent [wavelength; molar absorptivity]
Molybdoarsenate, crystal violet Silver diethyldithiocarbamate, pyridine Redn. of molybdoarsenate by H&O Heteropoly blue Heteropoly blue Heteropoly blue (hexanol-3-methylbutanol) Silver diethyldithiocarbamate, pyridine Heteropoly blue (iso-BuOH) Borosalicylic acid, ethyl violet (CsH6) Curcumin (CHICII) [555; 1.32 X lo5] 4,8-Diaminoanthrarufin 4-Nitropyrocatechol Curcumin [555; 1 . 4 5 X lo5] Curcumin, propionic anhydride, oxalyl chloride Methylene blue-BF4 Methylene blue Automatic Indirect: HgBrn (isoquino1ine)z ICHC13); dithizone Rosaniline Redn. to Br2; fuchsine Iodide, malachite green (CeHe) Iodide, acid violet S Antimony (111)-trihydroxyfluorone-antipyrine (CHCla) 1550; 8 . 7 X 1041 Copper(I), 6-methylpicolinaldehyde azine (CHCL) [480; 3 . 2 5 X 1031 Indirect: perchlorato-bis(2,9-dimethyl-l,10-phenanthroline)-coppe~(I) iEtOAc) Brilliant green (CEHE)[640; 9 . 4 X lo4] l-Phenyl-3-methyl-5-pyrazolone, isonicotinic acid, DMF Mercury (11)-p-dimethylamino-benzylidonerhodanine [452; 2.60 X 1041 M e r c u y (11), disodium ethyl bis(5-tetrazolylazo) acetate Indirect: Pd(I1): Fe(I1); 1,lO-phenanthroline Ti-chromotropic acid Dithizone 1-Methyl-4 [ ~4-oxocyclohexa-2,5-dienylidene)ethylidene]-1,4dihy dropyridine Copper (11)-p-toluidine Peroxyvanadate Antimony (III)-trihydroxyfluorone-antipyrine(CHC1~)[550; 8 . 7 X l o 4 ] Oxidn. by chloramine B, crystal violet (CsHe) [625; 6 . 1 5 X lo4] 4-Bromo-N,N'- bis (0-hydroxy propyl) -0-phenylenediamine N,N'-bis(p-hydroxypropyl)-o-phenylenediamine[525; 5.14 X l o 4 ] Oxidn. by H20,; o-tolidine 4-Bromo-N,N'-bis (0-hydroxypropyl)-0-phenylenediamine N ,N'-Bis (p-hydroxypiopyl)-0-phenylenediamine 4-Bromo-NJV'- bis (p-hydioxypropyl)-0-phenylenediamine Indophznol blue
Indophenol blue (BuOH) Copper(II), chromotropic acid 2-Mercaptoethanol Indirect; molybdophosphoric acid, carminic acid Heteropoly blue iiso-BuOAc) Heteropoly blue Heteropoly blue Heteropoly blue Molybdophosphoric acid, crystal violet (BuOAc-MeCOEt) Molybdovanadophosphoric acid Bis(4-dimethylaminophenyl)antipyrilcarbinol molybdophosphate Hydrolysis; molybdovanadophosphoric acid Crystal violet, iodide, chloramine B (C&) Methylene blue Sodium nitroprusside, Zn(OAc)z,pyridine Redn. of iron(II1); ferrozine Mercury(I1) thiocyanate, iron(II1) [470; 7 . 7 X lo3] FeSOJ Indirect; 2-aminoperimidine HC1 Indirect; barium iodate, starch-iodine [585; 3 . 1 X l o 4 ] Redn. to HzS, tris (1,lO-phenanthroline) iron(I1) GeMSAEC: turbidimetric, CAD Redn. to HzS, chloramine B, iodide, crystal violet
A N A L Y T I C A L C H E M I S T R Y , V O L . 46, NO. 5, A P R I L 1974
Table I1 ( C o n t i n u e d )
sod2-
&os2SCN -
Se Si
References
Cr plating baths
Redn; lead sulfide
(507)
... ... ... ... ... ...
Cyanolysis; methylene b l u e S C N (ClCH2CHzCl) Rhodamine 6G, or crystal violet (CJ&-PhN02) Mercury (11)methylthymol blue, zephiramine (CHCla) [646; 1.02 X lo6] Antimony (111)-trihydroxyfluorone-antipyrine (CHC13) [550, 8 . 7 X 1041 Rhodamine (C6H6) Indirect; silver(I), copper(I1)-diethyldithiocarbamate (cc14) [438; 3 . 8 x 1041 Naphthylbjsmuthol (CCl4) (334; 3 . 7 X lo4] Thioacetamide (CHCL) [400;5 X 1081 4-Methyl-0-phenylenediamine (PhMe) Molybdosilicate, chromopyrazole Molybdosilicate, crystal violet Molybdosilicate, rhodamine B Indirect: molybdosilicate, Mo-2-amino-4-chlorobenzenethiol (CHCl,) Molybdosilicic acid Janus green, TeBro2- (C6H6-MezCO) Naphthylbismutho (C6H6) [330; 2 . 2 7 X lo3] Diethyldithiocarbamate ICHCl,) Colloidal T e [420; 5 . 4 9 X lo3] Diphenylthiourea (C&) [480; 5.85 X lo3]
(367) (272)
... ... Steel ... I
.
.
... ... Te
Method or reagent [Wavelength; molar absorptivity]
Material
Conatituent
Electrolytes ... ... Silver Steel Steel
strontium is possible by measuring the differential absorbance of the sulfonazo complexes a t 640 nm using a EGTA buffer solution at pH 6.1 and a CDTA buffer solution a t pH 5.8 (349). Measurement of the absorbance of the ethyl acetate extract of cobalt and nickel xanthates, and then measurement of the absorbance of the cobalt xanthate after decolorization of the nickel complex with perchloric acid, is the basis of a simultaneous method for cobalt and nickel (600). Selenium(N) and tellurium(1V) can be determined in the presence of each other by measuring the selenium(1V) naphthylbismuthol extracted into chloroform from an aqueous solution pH 1.8 and then extracted the corresponding tellurium complex into benzene from the solution adjusted to pH 4.8 (122). Chlorine and bromine have been determined simultaneously by their characteristic reactions with methyl orange (400).A simultaneous method for phosphorus and silicon in cast iron takes advantage of the different stabilities of the corresponding molybdoheteropoly blues a t two selected acidities (700). Glycerol in binary mixtures with either sorbitol or xylitol can be determined by the formation of blue complexes of copper(11)at two different alkali concentrations (704). Kinetic Spectrophotometric Determinations. A method for determining very small amounts of molybdenum is based on its catalytic effect on the reduction of methylene blue by hydrazine sulfate (784). Trace amounts of chromium have been determined by a kinetic method in which the catalytic effect of chromium on the oxidation of o-dianisidine with hydrogen peroxide in the presence of y-picoline is the fundamental reaction (200). A kinetic method for the determination of osmium depends on the catalytic action of osmium(VII1) on the oxidation of arsenic(II1) by bromate (28). Morcury can be determined by its catalytic effect on the substitution of cyanide in potassium ferrocyanide by 2,2’-bipyridine (460). Copper(I1) has been determined by its catalytic effect on the oxidation of amidol by hydrogen peroxide (384). The catalytic effect of vanadium(V) on the oxidation of 1,5-diphenyl-3-aminopyrazoline by bromate is the basis of a kinetic method for the determination of vanadium in alkali metal halides (540). The catalytic effect of thiosulfate on the azide-iodine reaction has been utilized in the photometric determination of ultramicro amounts of thiosulfate (754). A kinetic method for estimating phosphate is based on the rate of formation of molybdovanadophosphoric acid (202). Ketones are determined by measuring the rate of reaction with Ehrlich reagent (701).
PHYSICS Topics related to fundamental principles of measuring radiant energy and instrumentation are included in this
(505)
(498) (275) (488) (122) (243) (345) (796) (53) (259) ( 738) (223) (278)
(122)
(274) 1364) (451)
section of the review. Optimum conditions for differential spectrophotometry have been discussed from a theoretical viewpoint (370) and the accuracies of the absolute, differential, and trace spectrophotometric technics were compared (371). The trace technique is no more accurate than the absolute technique when the contribution of the multiplicative component to the instrumental error predominates. Errors due to multiple path reflections in the absorption cell have been examined critically and an error of 1-2 ppt is indicated as probable in measuring the absorbance of aqueous solutions (117). A method for reducing errors due to a perturbing component in polycomponent systems by the introduction of a perturbation function, as a second order polynomial which is dependent on the wavelength has been proposed (418). Dual wave spectrophotometric measurements have been discussed in respect to obtaining first derivative spectra (652, 664), instrumentation, and analytical applications (579, 581). The theory and applications of internal reflection spectrometry have been treated from a practical viewpoint (778). The quantitative reflectometric determination of nickel has been investigated using test-strips which develop a color when an aqueous nickel(I1) solution is added (346). The determination of the optimum working concentration range from calibration plots obtained with a colorimetric AutoAnalyzer has been studied (774). Other studies include a method for calculating equilibrium concentrations and molar absorptivities of complexes by using absorption spectra intercepts of isosbestic points (436), a method for determining the number of absorbing species in solution (113), computerized continuous variations method for spectrophotometric determination of extraction and formation constants (414), and a computerized approach in determining formation constants by the spectrophotometric method of corresponding solutions (268). A review on rapid scanning spectrometry indicated experimental aspects of this technique and its analytical applications (614). The features and advantages of photon counting systems in spectrophotometry have been presented (434). A single beam spectrophotometer with automatic control of dynode supply voltage so that the sample and reference are measured a t the same photomultiplier sensitivity has been designed (238). A photometer has been described with which the relative radiant fluxes of sample and standard solutions are recorded so that different calibration plots automatically correspond to output (551). Attention is directed to a collection of papers entitled, “Instrumentation in Analytical Chemistry” edited by Senzel (638). Papers entitled “Instrumentation of a Spectrophotometric System Designed for Kinetic Methods of Analysis” ( 772) “Radiation Sources for Optical Spectros-
ANALYTICAL CHEMISTRY, VOL. 46,
NO. 5, APRIL 1974
239R
Table 111. Spectrophotometric Methods for Organic Compounds
Acetophenone Acid halides Acridine derivatives Aldehydes Aldehydes Aliphatic amines Alkylbenznne sulfonate Amines, pi,im., sec Amino acilis Aniline Anisidines Aromatic amines Aromatic carboxylic acids Aromatic nitro compds. Benzidine Bisthiosemicarbazones Carbazole Catechol 0-Chlorobenzylidene malonic acid Chloral hydrate Chloroaminopicolines C hlorophenols Cyclohexylamine Diantipyridyl methane Dimethylsulfoxide Diphenylmethan-4,4’diisocyanate Fatty acids Formaldehyde Furfural Gallic acid Glycolic acid Guanidine p-Haloaniline 21-Halocorticosteroids Homatropine 4-Hydroxy-1,3benzene disulfonic acid Hydroxy carboxylic acids Hydroxylipids Hvdroxtriazenes Hydroxyurea Indoxyl acetate a-Ketoaldehydes Laurylhydroxamic acid L-Lysine Maleic acid Malic acid Mannitol Methionine 2-Methyl-3-aryl-4quinazolones 2-Methylbenzimidazole 1,4-NaphthoquinoneOxalate Nicotinic acid Nitrophenols Phenanthrenequinone Phenol-2,4disulfonic acid Phenols P henoxyacetic acid derivatives Picric acid
240R
Method or reagent
Material
Constituent
... ...
... ... Organic compds.
...
Kinetic, Ehrlich reagent Isoquinolinium carbethoxymethylide, Et3N Chromium (111) thiocyanate Molybdophosphoric acid Fuchsine
... ...
Amion (CHC13) Crystal violet Coupling with azo dye 2,4-Dinitro-l-fluorobenzene (MeN0,) Chloranil Amidopyrine Quinoneimine Extrn; diazotization, a-naphthol Diazotization, urea Astraphloxin FF extra (CeH6)
...
Redn. with LiAIH4 in T H F
... ...
Hypochlorous acid (CHC1,) Copper (11) complexes Xanthydrol Triethanolamine, iron(II1) [595;1 . 8 3 X 1031 p-Nitrophenyldiazonium hydrochloride 1,2-Naphthoquinone
...
... ...
...
...
...
...
Anthracene ... ...
...
... ... ...
2-Thiobarbituric acid Pyridine, NaOH 4-Aminoantipyrine, K3Fe(CN)6 2,4-Dinitrofluorobenzene (isoamyl. acetate) Zr-xylenol orange IroniIII) alum p-Me2NC6H:CH0
...
Rhodamine 6 Zh (CsH6)
... ...
... Urea o-Haloniline ... ... ...
2-Hydrazinobenzothiazole, ferricyanide Aniline Sodium cobaltinitrite ,?-Naphthol Nitroprusside, ferricyanide Chloranil Conv. to quaternary pyridinium salt, MeaNOH Tetrabromophenolphthalein ethyl ester (ClCH,CH,Cl) Iron (111)
...
Decolorization, molybdosilicic acid
...
Sulfation; methylene blue (CHCI,) 1-Naphthylamine 8-Quinolinol Conv. t o indigo Diphenylamine Vanadate [575; 3 X l o 3 ] Formaldehyde, 2,4-dinitrofluorobenzene Tris (1,lO-phenanthroline) iron(I1) (PhNO,) Pyrogallol 4-Aminoantipyrine, ferricyanide Sodium nitroprusside Cobalt (111) thiocyanate iCHC13)
...
... ... ...
...
... I . .
... ... ...
... ... ... ... ... ... ... ... ... ... ...
Cobalt (11) complex Indene (C6Hs) Indirect; U(1V)-PAR 4,4’-Diaminostilbene-2,2’-disulfonic acid Diazotized sulfanilic acid, Na2C03 2,4-Dinitrophenylhydrazone
Phenol
Iron (111)
... ... ...
4-Aminoantipyrine hydrochloride, K3Fe(CN)6 Diazotized amine Nitration (BuOH)
Terephthalic acid
NHEt?iPhMe)
,..
A N A L Y T I C A L C H E M I S T R Y , V O L . 46, N O .
5.
A P R I L 1974
Table I11 (Continued) Constituent
Pyrocatechol Resorcinol Salicylanilide Salsoline Sorbitol Sugars, non-reducing Thiuram disulfide o-Tolidine Triethyllead ion Trifluoroacetic acid Triphenylmethanol Xanthates
Material
... ...
Fibrous materials ... ...
...
... ... ... ... , . .
...
Method or reagent
IronOII) [510; 1 . 6 X lo3] p-Nitrophenyldiazonium chloride Iron(II1) salicylate Titanium (IV), pyrocatechol HIO, oxidn.; 3-methylbenzothiazolin-2-one hydrazone Blue tetrazolinium, or Neotetrazolinium Copper (11) dithiophosphate Hypochlorite (CHC1,) 1-Hydroxy-4(p-nitrophenylazo)-2-naphthoic acid (CHC13) Tris(1,lO-phenanthroline)iron 01) (PhN02) Sulfuric acid. Dimethylphenylenediamine, oxidant
:opy” (295), “Double-Wavelength Spectroscopy (58U), Photon Counting for Spectrophotometry” (435), and a “Commentary” by the late Ralph H. Muller (473) are especially recommended. Spectrophotometers. The number of new spectrophotometers and new models appearing on the market must attest to the widespread popularity and utility of this method of measurement. The new Coleman Model 54 spectrophotometer features all solid state electronics, a 330- to 835-nm wavelength range, and a digital readout in concentration or transmittance (160).Zeiss has introduced their PMQ 3 photometer system with many optional attachments and optical systems. A spectral range of 1852500 nm is available with a single prism monochromator (137). The new MS 2 UV-Visible spectrophotometer introduced by Micromedic Systems, Inc. is a grating instrument which features twin 17-p1 cuvets having a 10-mm optical path length, a 4-digit display or printer, and an operational monitor (455). The new Cary 118 spectrophotometer series has three basic models, a manual spectrophotometer, a ratio recording spectrophotometer, and a ratio recording-scanning spectrophotometer. All models have a double prism monochromator operating in the 185- to 800-nm region and computer compatibility (139). Perkin-Elmer has introduced the Hitachi Perkin-Elmer Model 323 UV-VIS-NIR recording spectrophotometer having a single prism monochromator, a double-beam photometric system and optional accessories, including integrating spheres, and a turbidity measuring attachment. A Model 156 digital double wavelength spectrophotometer is also available from Perkin-Elmer (554). Sargent-Welch has marketed two basic models of a single beam spectrophotometer operating in the 325- to 625nm region, or to 925 nm provided a red sensitive phototube is used. One model has a mirrored meter readout and the other model has a digital readout (617). The new Beckman Model 25 double beam spectrophotometer provides five absorbance ranges, two scan speeds, and either digital readout or a recorder. A Model 24 instrument is similar in design but can be used only in the visible region. Beckman’s new Acta M series of spectrophotometers has two models IV and VII, with a wavelength range of 190-3000 nm. Several models, VI and VII, feature double monochromators (76). The Bausch and Lomb new Spectronic 700 has a 2-nm bandwidth throughout the 200- to 950-nm range and a mirrored scale readout (75). The Hitachi Model 102 spectrophotometer features digital readout, a 10-nm bandwidth and a 220- to SUO-nm range. The Model 191 is also digital indicating but has a 2-nm bandwidth and a 195- to 900-nm range (300). The new Leitz photometer Model 340-800 uses a selenium barrier layer detector whose output is fed to a solid-state operational amplifier. A series of narrow bandpass filters mounted in a turret assembly facilitates selection of the most appropriate wavelength (214). Another photoelectric filter photometer, designed primarily for field analysis of water pollutants, combines an interference filter and glass filters to provide the equivalent of 16 color filters (399). Gilford (258) has an adapter which permits the use of its accessories to convert a Beckman DU monochromator into a
References
(81) (550) 1699) (
209)
(549)
‘737) (679) ‘230) 1309) ( 77) 1619’1 (793)
more versatile spectrophotometer with digital or recorder capability, improved resolution, and an extended absorbance range. Automated Instruments. An automated spectrophotometer which sequentially analyzes 76 samples with a subsequent print-out of results has been described (645). Another spectrophotometer features programmed sample selection and automated wavelength scanning (138). A photometer has been designed to analyze automatically liquid droplets on a transparent band (6). A programmable monochromator for the rapid, automatic sequential isolation of wavelengths (165) and an automatic multiplesample photometric analyzer (492) have been described. Special Application Instruments and Accessories. A photometric analyzer which initially measures the NO2 at 436 nm and then the NO, after its conversion to NO2, is applicable to the determination of NO and NO2 in automotive exhaust gases (779). A disposable liquid sampling device containing a chromogenic agent, and utilizing plastic sheets to form cavities, has been patented (174). The performance of a spectrophotometer, especially suitable for measuring turbid solutions, and capable of operating in dual wavelength and derivative modes has been discussed (635). It is feasible to modify an atomic absorption spectrometer for the measurement of the absorbance of solutions (427). A simple modification of the Cary 14 spectrophotometer to permit photometric titrations (401) and a flow-through cell which is suitable for h i g h l o w rates in spectrophotometric titrations (48) have been described. A patent has also been issued for a concentration difference cell consisting of two chambers with variable optical paths (25‘*?). A He-Ne laser has been used as the radiant energy source in a special photoelectric colorimeter (302). The Brinkmann UDC-1A Six-Channel Colorimeter has been designed to use a single central light source with the maximum of six separate interference filter-type photometric systems being used simultaneously. Flow-through cells make this instrument especially suitable for use with AutoAnalyzer systems and in clinical analysis. The Brinkmann Probe Colorimeter utilizes a fiber optics light guide which eliminates the need of absorption cells. The probe is inserted into the test solution. Six filters provide a choice of wavelengths in the visible region (111). The Hach DR 2 spectrophotometer is a single beam instrument wit a circular variable interference filter and is available as a carrying case model or a laboratory model. This instrument is intended primarily for use in water analysis as test-set chemicals and direct reading meter scales are available for over 50 colorimetric determinations (287). The versatile Tektronix digital photometer/radiometer has five rapid interchangeable precalibrated probes for measuring illuminance, irradiance. luminance, light-emitting-diode output, and relative intensity (728). Hunter has introduced the D25D-2 colorimeter featuring digital display for color specification in either terms of the CIE X, Y, Z values, or the Hunter L, a, b, values. This colorimeter has numerous special attachments and is adaptable to monitoring the color of most industrial products (305). Leitz (217) manufactures microscope photometers which
L
A N A L Y T I C A L C H E M I S T R Y , VOL. 46, N O . 5. A P R I L 1974
241 R
can be used to measure the absorbance and, hence, the quantity of a stained constituent in a portion of a cell, or to determine electrophoresis profiles. A spectrophotometer has been designed to measure simultaneously and continuously the absorbance of two solutions a t different wavelengths. This instrument is especially applicable as a detector in liquid chromatography (771). A process stream spectrophotometer has been used to determine ppb amounts of iodine and iodide in acetic acid utilizing the catalyzed arsenic(II1)-cerium(1V) reaction (665).
given in the Tables does not include the unique preliminary chemical treatments, tolerances to diverse constituents, and special features of a particular reagent or method. Color Specification. The determination of the color of food by the Munsell and C.I.E. system and the interconversion of measured values (66) and the Kubelka-Munk theory as used in the specification of the color of turbid or translucent food materials (159) have been discussed. The spectrophotometric measurement of color in solutions of commercial sugars has also been examined critically (9). A computer program was devised to select the d es and the amounts of each required to obtain a desirecr textile color (466). Spectrophotometry was used to measure color deviations of dyeing and colorings and maintaining them within a specified tolerance (55) and to measure the color of spin-dyed synthetic fibers (235). The color differences of semitransparent polyethylene films were calculated by C.I.E., Adams, Hunter, and Cube Root methods (693). Other papers have dealt with color measurement of dyed cloth (352), oils (166),and dyed leather ( 7 ) .
APPLICATIONS
Methods of Analysis. The chemical literature is replete with spectrophotometric methodology and data. In the Chemistry and Physics sections of this review, a representative sampling of recent developments in methodology has been given. In this section, an extensive summary of spectrophotometric methods used to determine specific constituents either in real or synthetic samples is compiled in Tables I, 11, 111. In many cases the information LITERATURE CITED Abasov, G. A., Gasanov. D. G., Uch. Zap., Azerb. Univ.. Ser. Khim. Nauk. 3, 30 (1971), Abdisheva. A. V., Nauch. Tr. Tashkent. Univ., 379, 177 (1970). Abromaityte, D.. Ramonaite, S., Kiskyte, M.. Lief. TSR Aukst. Mokyklu Mokslo Darb.. Chem. Chem. Techno/., 13, 5 (1971). Adamovich, L. P., Gershuns. A. L., Oleinik. A. A,, Degtyar'ova, L. I., Visn. Kharkiv. Univ.. Khim.. 84, 66 (1972). Adamovich, L. P., Gershuns, A. L., Oleinik, A. A,. Nguyen, T. 2.. Zh. Anal. Khim.. 28, 715 (1973). Adler, S. L., Ger. Offen. 2,255,471(Cl G O l n ) . 24 May 1973; U.S. Appl. 200,545, 19 Nov 1971, 19 pp. Afonskaya, N. S . , Shesternina, G. P.. Belen'kii. L. I., Borisova, L. E., lzv. Vyssh. Ucheh. Zavod. Tekhnoi. Legk. Prom., 1, 60 (1972). Agarwala, 6 . V . . Ghose, A. K., Talanta. 20, 1929 (1973). Agrawal, S. K. D., Misra, 0 . S., Int. Sugar J., 74, 195, 235 (1972). Agrawal, Y . K.. Anai. Lett., 5, 863 (1972) Akatsuka. K.. Bunseki Kagaku, 21, 1372 (1972). Akhrnedli, M. K., Ayubova, A. M., Babaeva, T. R., Azerb. Khim. Zh., 4, 121 (1972). Akhmedli, M. K.. Basargin, N. N., Islamov, S. J.. Uch. Zap., Azerb. Univ., Ser Khim. Nauk. 1. 14 (1972). Akhmedli, M. K., Chan, H. T.,ibid., 2, 17 (1971). Akhrnedli, M. K.. Glushchenko. E. L., Gasanova, 2. L., Zh. Anal. Khim.. 26, 1947 (1971). Akhmedli, M. K., Glushchenko, E. L., Kyazirnova, A. K., Azerb. Khim. Zh., 1, 138 (1972). Akhmedli. M. K.. Granovskaya, P. 6.. Neirnatova, R. A,, ibid.. 5-6, 116 (1971). Akhmedli. M. K.. Granovskaya, P. 6 . . Neimatova, R. A,, Uch. Zap., Azerb. Univ., Ser. Khim. Nauk. 3, 15 (1972). Akirnov, V. K., Busev, A. I., Kliot, L. Y., Zh. Anai. Khim.. 28, 1014 (1973). Akimov. V. K., Busev. A. i., Shubashvili, L. V., Shvedova, N. V., Zavod. Lab., 38, 146 (1972). Akimov. V . K.. Busev, A. I., Zhgenti, K. A,. Zh. Anal. Khim , 27, 1941 (1972). Akimov, V. K.. Kliot,, L. Y., Busev. A. I., ibid., 28, 118 (1973). Akki, S. B., Khopkar, S. M.. Bull. Chem SOC.Jap.. 45, 167 (1972). Alekperova, A. A.. Alekperova, R. A.. i ssied. Obi. Neorg. Fiz Khim , 1970, 59. Aleksandrov, A,. Mikrochim. Acta. 1972, 664. Aleksandrov, A,, Dimitrov. A,, ibid., p 680. Aleksandrov, A,, Dirnitrov, A,. Nauch. Tr.. Plovdivski Univ.. M a t , F i z . . Khim.. Bioi.. 10, 93 (1972).
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Mass Spectrometry A. L. Burlingame and Robert E. Cox Space Sciences Laboratory University of California Berkeley Caiif 94 720
Peter J. Derrick' Deparfmenf of Chem,stry, University College University of London London W C l H OAJ Engiand
Mass spectrometry has a Janus-like quality in embracing and pursuing both the roles of chemical reactor and analytical instrument. Mass spectrometry in its guise of chemical reactor is probing a t ever deeper levels the nature of the chemical reactivity of (radical-)ions. As one of the most sensitive of analytical techniques. mass spectrometry is a t the forefront of applied science seekW r i t t e n d u r i n g a v i s i t t o t h e Space Sciences L a b o r a t o r y , University of California, Berkeley.
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ing to rationalize the phenomenological universe a t the atomic and molecular level. We have organized the present review according to this duality. Following our initial section discussing techniques, instruments. and computers, we make sharp distinction between the chemistry of organic (radical-)ions and analytical applications in bioorganic chemistry and medicine. The sheer enormity of the number of publications in mass spectrometry, which exceeds 20,000 in the two years 1972 and 1973. demands that we restrict the scope of this review. We choose to
A N A L Y T I C A L C H E M I S T R Y , V O L . 4 6 , NO. 5, A P R I L 1 9 7 4
