Light absorption spectrometry - ACS Publications

Vest. Mosk. &OS. Unw., Ser. Khim., 6, 96 (1968). (35 Al&va, I. I., Smirnova, I. B., Jataimirskii, K. B., Zh. Anal. Khim., 25, 539 (1970): (36) Jasinskiene, E., Kalesnikaite, S., w..D 87. (37 F(dokva, T. I., Shvedova, L. V., datsimirskii K, B. W . p 307. (38) Kukuahkh p. k., Vhova, R. A., Zh. Prikl. Kham.. Lmmw., - , 41.. 2293 (1968). (39) Alekseeva, I. I., Ignatova, .N. K., Uchen. Zap. Mosk. Zmt. Tonkoa Kham. Tekhnql., 1, 59 (1970). (40)K a h m a , V. E., Yatsimifskii, K. B., Zunma. T. S.. Zh. Anal. Kh%m..24. 1178

(63) Tamarchenko, L. M., Zh. Anal. Khim., 25, 567 (1970). (64) Yateimirskii K., Rmolovskii, S., ~ r i e sE. E., a&,, p 324. (65) Rdsolowski, S., Chim. A d . (Warm ~ )15, , 157 (1970). (66) Babko, A. K. Markova, L. V., Maksimenko, T. Zh. Anal. Khim., 23, 1268 (1968). (67) Suteu, A., Crisan, I. A,, Mhdrutiu, E., Rev. R a m . Chim., 15, 1187 (1970). (68) Alexander P. W., Orth, G. L., J . Ehroanal. dhha., 31, A p. 3+ (1971). (69) Buckley, J. P., Anaf Chzm. Ada, 52, 379 (1970). (70) Hojman, J., Stefanovic, A., Stankovic. B.. Zuman. P.. J . Eledroanul. Chem:, 30, 469 (1971).’ (71) Ezereka a, N. A., Kiseleva, I. N., Zh. Anal. ghim., 24, 1684 (1969). (72) Sinyakova, S. I., Stepanova, I. K., W.,23, 1405 (1968). (73) Milyavskii, Y., Sinyakova, S., ibid., D r 1183. (74) Tur’ an, Y., Saksin, E., W., 25, 998 (19?0). (75) Skobets, E. M., Chernyi, V. A., Drutstsa, P. I., Tr. Nikolaev. Korabbstrod Inst., (36), 167 (1970). (76) Mottola, H., Talanta, 16, 1267 flg69). (77j-M6ttolaI H., ANAL.CHEM.,42, 630 (1970). (78) Ingle, J. D., Jr., Crouch, S. R., ANAL. CHEM.43, 697 (1971). (79) Zbid.. D 7. (80j TikhGova, V. I., Zh. Anal. Khim., 23, 1720 (1968). (81) Rodziewicz, W., Kwiatkowska, I., Kmatkowski. E.. Chem. Anal. (War.saw), 13, 1067 (1968). (82) Zbid., p 1305. (83) Ibid., 14, 55 (1969). (84) Cordos, E., Cirlig, E., Stud. Univ. Babes-Bolyai, Ser. Chem., 15, 13 (1970). (85) Hargis, L. G., ANAL.CHEM.,42,1494 (1970). (86) Ibid., D 1497. (87) Ha&, L. G., Anal. Chim. Acta., 52, 1 (1970). (88) Greinke, R. A,, Mark, H. B., Jr., ANAL.CHEM.,39, 1577 (1967). (89) Willeboordse, F., J . Phys. Chem., 74, 601 (1970). - -,(gojwillis, G. B., Woodruff, W. H., Frysinger, J. R., Margerum, D. W., Pardue, H. L., ANAL.CHEM.,42, 1350 (1970). (91).Worthington, J. B., Pardue, H. L., zbzd., p 1157.

d.,

\ - -

,-”--,.

(61) Zoledziowska, Z., Chem. Anal. (Warsaw), 15, 1037 (1970). (62) Bognar, J., Nagy, L., Mikrochim. Acta, 1969, 108.

(92) Deming, 8. N.,ibid. 43,1726 (1971). (93) Greinke, R. A. dark, H. B., Jr., W . 39,1572 (196t). (94) Shreate, I. L., Das, M. N., A d . Chim. Ada, 50, 135 (1970). (95) Zaia, P., Peruzzo, V , Lazzogna, G., W , ,51, 317 (1970). (96) Brook, A., Munday, K., Analyst (London),94,909 (1969). (97) Schwartz M., Delduce, A., J . Phurm. Sci., 58, 113b (1969). (98) Dela orte, N., Laval-Martin, D., Anal. d i m . Ada. 55, 425 (1971). (99) Yatsimirskii, k. Budarin, L. I., Khachatryan, A., bokl. A M . Nauk SSSR, 195, 898 (1970). (100) Sand, J. R., Huber, C. O., ANAL. CHEM.,42, 238 (1970). (101) Ingle, J. D., Jr., Crouch, S. R., Bittikofer, J., Pardue, H., M a r g e m D., ibid., p 1340. (103) Deming, i., Pardue, H., aid., p 1466. (104) Varley, J. A., Baker, K. F., Analyst (London),96, 734 (1971). (105) D a m n , J., Fisher, G., Annan, W., ibid., p 380. (106) Husbands, A. P., Spectrovhion, (23). 13 (1970). (107)’Lalo< G. C., Lab. Pract., 19, 607 (1970). (108) Hexter, R. M., Hand, C. W., Appl. Opt. 7, 2161. (1968). (109) keene, J. P., Black, E. D., Hayon, E., Rm. Sei. Znstrum., 40, 1199 (1969). (110) Toropova, V., Zabbarova, R., Zh. Anal. Khim., 25, 1059 (1970). (111) Bonchev P. R., Aleksiev, A. A., Dimitrova. f.. Mikrochim. Acta. 1970. 1104. (112) Kreuger, R., Vas, S., Jmehkis, B., Talanta, 18, 116 (1971). (113) Alekseeva, I., Nemzer, I., Zh. Anal. Khim., 25, 1118 (1970). (114) Masalovich, V. M., Agasyan, P. K., N. Kolaeva, E. R., Tr. Ural. NauchIssbd. K h m . Znst., 19, 173 (1970). (115) Fleet, B., Rechnitz, G., ANAL. CHEM.,42, 690 (1970). (116) Hicks, G. P., Eggert, A. A., Toren, E. C., Jr., ibid., (117) Toren, E. E gert, A. A., Sherrv. A . E.. kicks. P.. Clin. Chem:.’16. 215 i1970). ’ (118) Eggert, A. A., Hicks, G. P., Davis, J. E., ANAL.CHEM.,43,736 (1970). (119) Demina. -, S. N., Pardue, H. L.. ibid.. . p i92. (120) Mottola, H. A,, Harrison, C. R., Takanta, 18, 683 (1971). \-_.

I

,

a’?:,

8

8.

I - - -

Light Absorption Spectrometry D. F. Bok, Wayne State University, Detroit, Mid. M. G. Mellon, Purdue University, La fayetfe, Ind.

T

HE APPLICABILITY OF SPECTROPHOTOME-Y to the determination of

traces of metals, nonmetals, and organic substances is one of the main reasons for the continued widespread utilization of this opticometric method of analysis. Reliable low cost instrumentation, speed, satisfactory accuracy and precision, and suitability for automation are additional factors contributing to the popularity of spectrophotometric 300R

analysis. This review records the sigiiificant developments in analytical, light absorption spectrometry for the period from November 1969 through November 1971, as documented by Chemical Abstracts. The subject matter has been classified under the topics of Chemistry, Physics, and Applications, aa in the previous reviews (103, 494, 496)* The extensive literature cited in this

ANALYTICAL CHEMISTRY, VOL. 44, NO. 5, APRIL 1972

review attests to the large number of relevant publications which have appeared in this biennium. It has been necessary to evaluate carefully all papers and abstracts and to cite only those references of most probable significance to analytical chemists. Although hundreds of papers of scientific merit have not been mentioned because they were judged to be either of limited applicability or repetitious, this review

undoubtedly does include mme references belonging to one of theae ate gories. The authors also acknowledge the probability of errors of judgment in omitting certain references. Attention is directed to several reviews and books relevant to analytical light absorption spectrometry. A comprehensive review on absorptiometry including the basic theory, instrumentation, and a variety of applications has been published (169). The procedure for the spectrophotometric determination of 25 metals and 9 nonmetals have been reviewed (266). A book on the “Colorimetric Determination of Elements” has been published in Polish (470). “Spectrophotometric Analysis of Alloys” is the title of a book published in Russian (87‘4). A timely book “Extraction-Photometric Methods of Analysis with the Use of Basic Dyes” has also been published in Russian (99). Books devoted to the photometric analysis of organic compounds (404,844) are also available. A supple mentary volume to the Snell and Snell treatise, “Colorimetric Methods of Analysis, Including Photometric Methods, Vol. UA,” (708) is in English. Chapters on “Ultraviolet and Visible Absorption Spectrophotometry” (IO$?), “Spectrophotometry and Spectrofluorand ‘Colorimetry” (664) imetry” (SI$?), streas fundamentals and specific applications.

Table 1. Constituent

-

...

ElectrolyG

Om

red

Tellurium

AI

1,lO-Phenenthrolinebromopyrogallol

red Anthrawchrome [~Qo;2.9 x 1041 %Bromo-4,5+ihydroxy-4’-azobenzene sulfonic acid [455; 2.7 x 1041 Enochrome cyamne R [MO; 3.1 x 1041 l-(l-Hydroxy4methyl-2- henylazo>2... naphthol-rl-sulfonicacid? Phenoxydinaphthofuchsonedicarboxylic ... acid Rutin Stilbazo, zephiramine [540; 1.08 x loci] Sulfochrome ... 1560; 3 . 8 . ~1041 Phenoxydmaphthofuchsonedicarboxylic Alkali halides acid S-Quinolinol (CC?) Alloys Carbon tetrachloride Eriochrome cvamne Pyrocatechol “violet silicatea Semiautomatic: dihydroxytartaric acidSodium aluminate 2,4-dinitrophenyl osazone j=Ne solns luconate uinolinol (CHClr) Steel Chrome azurol S Steel, low-alloy [620; 7.34 X lo4] Eriochrome cyanine Steel Xylenol orange Ta-electrolytes S-Quinolinol (CHCla) Thorium compds SQuinolinol (CHCb) Tungsten Butylrhodamine S ... (4Dimethylamipophenyl) (4-benzyl.. methylaminophenyl) antipyrylcarbinol “ Chromopyrazole-I’ (PhMe) [580; 6.08 X lo4] 2,2‘-Di yridyl-a-glyoxime ... 5-(pE&oxyanilino >5,6-dihydrouracil ... [520; 1.3 X 10’1 Hydrogen tetrabromobis(p ridine-N.. oxide) aurate(II1) (CH281r) Isonicotinic acid hydrazide ... [520; 3.88 X 107 3-Methyl4vadlylidene-5-isoxazolone Meth leneblue bromoaurate (CgH&lC*J*CL) [Ssd; 9.0‘X lo4] Rhodarmne B (CsHs4so-PrtO) ... Thioca rolactam-tetraodioaurate(II1) ... (CHh) [MO; 3 . 7 x .lo’] Bromaunc acid (EtOAc) 4Dimethylaminopheny1-4’-met hylbenzylamhophenyl antipyrylcarbinol IPbMe)

*.

. I .

d

Au

CHEMISTRY

Progress continues in the development of new and improved light absorptive chemical systems for metals and nonmetals baaed on the use of a wide variety of chelating agents and/or dyes to form ternary complexes which are extractable and have high molar absorptivities. The ingenuity of analytical chemists in controlling homogeneous and heterogeneous equilibria and adjusting solution variables in order to obtain specificity and to contend with many potential interfering substances present in real samples is especially note worthy. Some of the methods cited in Tables I, 11, and I1 have been included only because of the effective means developed to cope with interferences. In this section of the review, we shall consider primarily new reagents, chemical reactions and structures, and critical evaluations of methods under the general categories of metals, nonmetals, organic constituents, simultaneous determinations, and kinetic determinations. Metals. More t h a n 30 metal ions give colored products with 1,2,7trihydroxyanthraquinone 3 - methylamine-N,N-diacetic acid depending upon the p H of the aqueous solution (144). Methods involving the use of antipyrine and its derivatives have

MBterial

Ag

Photometric Methods for Metals Method or re ent [Wavelength; molar %orptivity] picolinaldehyde thioeemicarbazone Dithiwne 1,lO-Phenanthroline 1,lO-Phenanthrolinebromopyrogallol

Be

Be

~

Copper, nickel Waste

... ...

...

... ...

...

Carboxyazo 1685; 4.46 x 1041 Carboxysulfonazo [645; 4.04 x 1041 Sulfonazo 1650; 4 . 8 x 1041 Arsenazo I11 [5m; 1.s x 1041 Chrome azurol S, zephiramine Chrome blue G [6!0; 3.1 X lot] Enochrome bnlhant violet B 5.95 x 10‘1 Enochrome cyanme R Methylthymol blue [m;1.32 x 1041

[e;

(UO)

(676, 716)

(Continued)


301 R

Table 1.

Photometric Methods for Metals (Continued) Method or Reagent Conetituent Material [Wavelength; molar absorptivity] Solochrome azurine BS Be [MO;4.6 X 10'1 Bronze Eriochrome cvanine Bi Chromeammi [520; 7.1 X 10'1 Indirect; starch-iodine [590. 3 x l(r] I o d e , tnbenzylamine (CHCL) ... Indirect : antipyrineklithiocarboxylic acid (CHC4) nickel(I1) nitrate Diphenylthiourea [450; 8.4 X 10'1 7- [a-(o-Methoxycarbonylalino )beneyl] ... quinolinol [400;7.2 X 10'1 Meth 1 green-iodobismuthate (CaHc PhXOd 1650: 4.3 4 . 3 X 10'1 [650; *.. Methyl xyienol xylenol hbluee [570; 8.9 X 1081 ... Methylth mol blue (BuOH) 1-Pvmdnecarbodithioate Thibcyanate [470; 6.2 X lo*] ... 3,4,5,6-Tetrachloro-3 ',4',5',6 '-tetrahydrox uran ; 1,3diphenylquanidine (isam ?OH) 1,2 3,4~etrahydr&mercaptoquinoline (CHCl.) Ni alloys eTolylt66urea (C2H4Cl2) [455; 9.4 x 10'1 Ores Io&de Iodide Steel Ca 2 7-Bisazo deriv. of chromotropic acid d l oxal bis(2-hydroxyanil), (l-octanolLctanol) [545; 9.3 x 10'1 Methylt hymol blue ... [610; 1.83 X 10': Methylxylenol blue [610; 8.3.X 10'1 Boron compds Glyoxal bls(2hydroxyanil) ROCkS Glyoxal bis(2-hydroxyanil) Zirconium, titanium Murexide Cd 2,2 '-Bibenzoxazoline (CHC&-CsHsN) p o ; 1.2 x 1041 Diphenylcarbazone (Bu,POd) 1530;.4 x 1041 ... Cadrmum(II), 1 10-phenanthroline, brornopyrogadol red 1610; 1.o x 10.41 Iron(II1)-cadrmum(I1)-tartrate ... P(2Pyridylazo)resorcinol [495;, 8.4 X lo'] Zircaloy-2 Dithzone Ce ... o-Aminophenol 1470; 2 . 5 X !Os]. Glutanrmde d i o m e Chromotrom 2R [550; 6.65-X 10'1 ... Methylene blue (847) ... 3-Thianaphthenoyltrifluoroacetone (30-9 (CsHs) [424; 5.51 X lop] o(wTo1uenesulfonamidoh i l i n e o3olidine N-Benzoyl-N-pheny lhydroxylamine co Benzamidoxiiie 542; 4 x 10'1 ... enzil mono-(2pyridyl)hydrazons ... Bianthrazochrome r 6 w 8 . 8 x 1081 Chromazurol S N,N '-Bis(msulfobenzy1 )dithiooxamide N,N-Bis [2]bis(carboxymethy1)amino ethyl lycine "DTPA" ... P[ oro-2-pyridyl)azo]-1,3-di-

...

... ...

... ...

-

...

B

(5x8

...

... (Continued)

302R


been reviewed (98). Thionaphthenic acid has been found to be an extraction reagent for silver, antimony(III), bismuth, cobalt, and nickel with each extract having a characteristic hue (96). Substitution of chlorine or sulfonic acid in the ortho position of 3',3'-dimethyibenzaurin-5',5'dicarboxylic acids inc m e s the molar absorptivity of metal complexes of this reagent (338). 1-

(2-Carboxy4sulfophenyl)-3-hydroxy-3phenyltriazene has been reported to be a highly eatisfactory reagent for the determination of iron(III), molybdenum(VI), and vanadiumw) (461). A new chromogenic reagent for the determination of metals is 1-[ (5chloro2-pyridyl)azo]-2-naphthol (678). Factors involved in the spectrophotometric analysis of ternary solute systems have been discussed and a list of 78 applications of spectrophotometry to the analysis of binary and tertiary organic and inorganic systems has been included (666). A comprehensive spectrophotometric study of 17 hydroxyl-containing triphenylmethane re agents in respect to the effect of halogen substitution, protonation, pH, and ionization on the absorption spectra has been reported (976). 6'- [ (1-Hydroxy5sulfo-2-naphthyl)azoI-l-methylanabasine has been investigated as a reagent for the spectrophotometric determination of copper, nickel, cobalt, palladium, zinc, cadmium, and manganese (671). N-Hydroxysuccinamic acid has been found to be a suitable reagent for the photometric determination of vanadium, titanium, manganese, and iron (91). Reviews on photometric methods for magnesium (798) and thorium (229) have been published. 2,3-Dihydroxynaphthalene has been proposed as a new reagent for the photometric determination of traces of iron, vanadium, titanium, and molybdenum. The colored complexes are extractable into chloroform (668). A review of certain extraction-photometric methods for bismuth, iron, titanium, molybdenum, vanadium, zinc, nickel, and manganese (also selenium and tellurium) has been published (667). An interesting reaction of sodium ions, in an aqueous-dimethylformamideacetone solution, reacting with nitroanthranilazo [4-(2-carboxy-4-nitrophenyl) - 3-methyl-1-phenyl-2-pprazolinSone] to form a complex exhibiting a molar absorptivity of 1.1 x IO4 has been reported (477). A comparative study of reagents for the determinatian of calcium showed glyoxal bis-hydroxyanil and calcion to be the best although azoazoxy BN has certain advantages if an extraction is utilized (266). -4 review of organic reagents for the photometric determination of copper has been published (690). Two new ferroin-type reagents, 6-methyl-2-pyridylhydrazidine and 3-

(6-methyl-Zp yridyl)-5,6-diphenyl-l,2,4triazine, have been indicated as being specific for copper (731). 4[ (5Chloro-2-pyridyl)azo]-1,3-diaminobenzene is a new highly sensitive and selective reagent for the determination of cobalt (677). M e t h y l t h p o l blue, xylenol orange, 4-(2pyridylazo)-resorcinol and 9-salicylfluorone have been studied as reagents for manganese(I1) with PAR being the most selective (783). Several organic reagents including dithizone, xylenol orange, magneson XV, and chrompyrazole I were compared as chromogenic agents. Dithuone and sulfarsazene gave very reproducible results in the photometric determination of zinc in aluminum alloys (368). A procedure involving a preliminary partial partitioning of traces of copper, mercury, cadmium, and thallium ultimately used sequential photometric methods for each metal. Copper was determined by the diethyldithiocarbamate method; cadmium and mercury by the dithizone method; and thallium by the rhodamine B method (4). The tris(1,lO-phenanthroline) iron(I1) cation reacts with two singly charged anions of the dye, 1amino4 - (0-toluidine)anthraquinone- 2sulfonic acid, to give an ion associate extractable with chloroform. Conformity to Beer’s law was observed for 0.1 to 1 ppm of iron (396). Nickel forms a 1:2 complex in acidic solution and a 1:3 complex in basic solution with p-hydroxydithiobenzoic acid (644). A critical review of photometric methods for aluminum has been written (797). A study of five reagents which react with chromium(II1) showed that xylenol orange and glycinecreaol blue were the most sensitive (781). An evaluation of reagents for the determination of cerium indicated that leucobase malachite green, arsenazo 111, and xylenol orange were the most satisfactory (914). A study of organic reagents for the spectrophotometric determination of germanium indicated that the o-diydroxyphenolic and 0hydroxyquinone groups were the most reactive and that stilbazo and hematoxylin were the best reagents ($6). A new reagent “Tipyrogin” or [4,4’(methylimino)dimethyleneIdipyrogallol has been proposed for the determination of niobium (70). The extraction of the SbCL- species with methylene green and other dyes was studied spectrophotometrically. The effect of acidity and the nature of the solvent, and the resultant distribution coefficients were examined (679). Reactions of antimony(II1) in a benzene extract with 5-(2-pyridylazo)-Z(ethylamino)-p-cresol “PAAK”, 4,4’-bis(dimethylamino) - 3 - nitrodiphenylantipyrylcarbinol“ 3-MFPK,” and 2,2’,4’trihydroxy-3-arsono-5-chloroaaobemene “rezarson”

have

been

Table I.

Constituent

Photometric Methods for Metals (Continued)

Material

...

co

...

...

Method or Reagent [Wavelength; molar absorptivity] References 5-(2-Hydroxy-l-naphthylazo)pyrazole+ carboxylic acid 2- [ (2-Hydroxy-5-nitrophenyl)azo]-4,s diphenylirmdazole monoacetic acid Mercaptothiadiazolylazonanhthol [680* 1.J8 X lo4] C(1-byndylazo) resorcinol 2-Pyridinecarboxaldehyde t,hiosemicarbazone [425; 7.25 x io*] 1356; 1.4 x 1041 Potawium benzenesulfonyl&thocarhamate --

2,2-Quinolylketo&e (Cas) [365; 5.5 x 1041 Oximidobenzotetronic acid (CflH.) .[430; 1.82 x 1041 Reduction of molybdophos horic acid N-Methylanabmine-a -azo!iethylaminophenol [440; 7 . 8 X 1041 4(2-Thazolvlazo ) reeorcinol [570; 2 . 5 $? lo4] l-(2-Thiszolylazo)naphthol 3.7 x 1041 Thiovioluric acid (425; 5.8 x 1041 Trioctylmethylammoniium chloride, nitroso-R+t (CHClr) pToluamidoxune 1-Phenyl4 henylazo-1,2,Ctriasolinium chloride &H4Cli) 3-Merca to-p-propionophenetidide (CH&) 1-( -Sulfophen lrtzo>2-hydroxy-3,6&ulfonaphtKalene Nitroso-Rsalt Azorubine Diphenylcarbazide Cr(V1)-trioctylamine (CHCls) Indirect; copper(II>-chrome azurol S, re hiramine 4-&Y ridylazo ) resorcinol Xylenol orange Xyleno! orange [MO;1.0 x 1041. Eriochrome c amne Octylamine (6HCls) Pyrocatechol violet Diphenylcarbazide Tns(1 10- henanthroline iron(l1) (Hdr041, (PhNOd Diphenylcarbrtzide Diphenylcarbazide 2,3-Bis(salicylideneaminobenzofuran -I

... ...

...

Auoys

... ...

Soils Sulfide minerals Steel

Cr

... ... ... ...

... Alloys

..*

Auoys Alloys Anodic powders Resistor alloy films Steel Tin Vanadium compds cu

...

... .. ...

... ...

... ... ...

wo;

(C&)

[5iO; i.‘m x 1041 Bls(pentamethy1ene)thiocarbamoyldisulfide Chrome azurol S 1582; 1.7 x 1041 Chrome azurol S [m;3.9 x 1041 Chrome azurol S, zephiramine 1530; 4.76 X lo4] 1-(2-Carboxy-Psulfonatophenyl-3hydroxy-3-phenyltriazene 7-(2-Hydroxy-3,5-dinitrophenylazo)8hydyx 1,6-naphthalinedisulfonic acid d k n i n e C” 3-Hydroxy-l,3diphenyltriazene ( C a s ) [395; 1.91 x 104) 2- [2-Hydroxy-5-nitrophenyl)azo]4,5diphenylimidazole monoacetic acid (isoamyl OH) Isatin-Zoxime

(ContinuEd)

investigated ANALYTICAL CHEMISTRY, VOL. 44, NO. 5, APRIL 1972

303R

Photometric Methods for Metals (Contiwed) Method or Reagent Material [Wavelength; molar absorptivity] ... 3-(6-Methyl-2-pyridy1>5,6-diphenyl12,Ptriazine [491; 9.55 x 10’1 0-Hexyl hydro n butyldithiophosphcnate (C9H48) 1,5-Di-&na hthyliocarbazone (CHCb) ... Picramine rw: 3.1 x _ .1041 ~4-(%k’yridylazo)resorcinol (BuaPOd) ... [MO; 1.% x 1041 pResorcyhdenethosemicarbazone [374;*1.*24x 10’1 8-Quinohol. Dvndine Sa2-naphthol 1560; 2 . 2 8 x 1041

Table 1. Consitituent cu

... ...

.---

Rr

2

... ... ... ...

[5io. 4,30 x 1041 P(Z)Tha~olvlazo b2na~hthol (580; 2.00 k 1041 Pyridinecarboxaldehyde (thio-l-naphAlloys thoyl) hydrazone Antipyrine-rl-azc-b(baminc-N-methy1Brass anabasine) Lead djethyldithiocarbamate (PhMe) Lead BathoDhenanthroline Lead, nickel PDTA, triethylenetetramine Plating bath 6-Methyl-3-mercapto-l,2,4-triazine Steel (EtOAc) Oxalic acid bls(cyclohexy1ideneSteel N,~,driride) iphenylthiocarbamohydroxamic Steel acid Brilliant reen (COHO) Ferrochromium l-(>Pyri8ylazo )resorcinol Tungsten ZThenoyltritluoroacetone Water Tiron ... i9i.Oi Indirect; reduction of PAR Indirect; iron(III), 2,2’:bip ridine Samarium Picolinaldehyde thosermcariazone ... [580; 5.8 X loz] Chrome azurol S .. 1630; 5.5 x 1041 Chrome azurol S, zephiramine [634; 1.5 X l W ] 2-H droxy-5-methylacetophenone ... ... BisB,10-phenanthroline iron(11)azide [510; 1.68 X lo4] Iron(II>2,2’-bipyridine, n-caproic acid (CHCb) [520; 1.4 X IO4] ... Iron(III>gqumolinol-5-sulfonic acid, zephiramine (CHCla) [595; 3.12 x lo;] l,l@Phenanthrohne, thiocyanate(is+ ., PrCOMe) [515; 2.25 X lot] .. Tris(benzylsulfoxlde)iron(I11) thiocyanate (CHpCl) ... Tiron, di hen 1 anidinium salt (is+ am 1 Tris(l4pentanodionate) iron(II1) Al alloy (PkOd Carbon tetrachloiride Bathophenanthroline (CHCla) Methyl xylenol blue Dolomite 2,6-Di-(%pyridyl>4-p-methoxyphenyl> Metals E&Yridine yl bls [ (l-sodio-H-tetrazol-5-yl)azo]Water acetate Di-Na-3-(2-pyridy1>5,6-bis(PsulfoWater phenyl>l,2,4triszine “Ferrozine” [562;.2.79 X lo4] 5-Amno-3 [ (3-chloro-2-hydroxy-5nitrophenyl)azo]4hydroxy-2,7-naphtk$enedisulfonic acid “Gallion” Basic blue K-chlorogdate ( C a r MeZCO) [620; 6.0 X IO4] (Continued)

-

Eu Fe

BH-&&~)

Ga

304‘ R


and optimum conditions for the determination of antimony have been delineated (928). Six 0,o’dihydroxyazo compounds were studied as r e agents for zirconium and as to the d e c t of substituents on the stability and absorptivity of the complexes. Picraminazochrome and picraminazo-H were selected as suitable reagents (118). The color reactions of picramine r e agents containing the 0,o‘dihydroxyazo group with niobium(IV), zirconium(W), molybdenum(VI), copper(II), scandium(III), indium(III), and gallium(II1) have been described (174). A selective reagent for molybdenum(V1) is bis(B-aminoethy1)dithiocarbamic acid (186). Tungsten as the W020H+ s p e cies reacts with 8-mercaptoquinoline to give a 1:1 complex which is extractable with a 1:1 isobutyl alcohol-chloroform mixture (68.9). The various procedures for the spectrophotometric determination of tungsten by the thiocyanate method have been reviewed (896). The color reactions in which certain platinum metals (Rh, Pd, Os, Pt, and Ru) react with pnitrosodimethylaniline and the wavelengths of maximum absorbance have been used to devise spectrophotometric methods for these metals (386). The use of diantipyryl methane, diphenylguanidine, and tribenzylamine has been investigated as reagents reacting with either iridium-tin-bromide or rhodium-tin-bromide complexes to give suitable colored systems for the determination of iridium and rhodium (677). Oxidobenzotetronic acid has been suggested as a chromogenic agent foF the determination of osmium, iridium, platinum, palladium, and ruthenium (467). Comprehensive r e views have appeared concerning photometric methods for niobium and tantalum (906),iridium and rhodium (183), ruthenium (121),and osmium (126). Nonmetals. A number of anions (Reo4-, SCN-, clod-, 1 0 4 - , I-, BE-, CIOs-, NO*-, Br-, NOz-, BrOs-, and C1-) react with the tetraphenylarsonium bromophenol complex in chloroform to liberate the bromophenol blue anion to the aqueous phase (664). The optimum p H ranges for the development of molybdosilicic acid in nitric, perchloricic, hydrochloric, and sulfuric acid have been determined and a procedure based on the standard addition technic has been developed for the determination of silicon in steels (660). The heteropolymolybdate complexes of phosphorus, arsenic, silicon, and germanium have been discussed in respect to their analytical and spectral properties. The existence of a- and 6-forms of these heteropoly acids is indicated (985’). Molybdophosphoric acid forms a 1:3 complex with bis(4dimethylaminopheny1)antipyrylcarbinol which is suitable for absorbance measurements (878).

A study of the nucleophilic displacement reaction of organic disulfides with cyanide ion showed that 5,5'dithiobis(2nitrobenzoic acid) is a suitable reagent for determinining cyanide by measurement of the absorbance due to the displaced thiol anion (317). I n a critical evaluation of the pyridinebenzidine method for the determination of cyanide, it was found that heterocyclic and other nitrogen-containing organic compounds caused positive errors ($88). The oxazine dye "Nile Blue" reacts with traces of iodide and bromide to form complexes which are extractable into chloroform (446). Iodide also forms an ion associate with tris( 1,IO-phenanthroline)iron(II) which is extractable into nitrobenzene and the stable colored extract is m w u r e d at 516 nm (869). I n studying the indophenol reaction in respect to the determination of ammonia, it was found that NazFe(CN)sNO] was the best catalyst in producing rapidly a stable color. Excess base resulted in instability of color and a loss of sensitivity ($89). Organic Constituents. Five reagents for determining aliphatic amines were compared. Tropeolin 00 was considered better than methyl orange, picric acid-neutral red, cresol green, and bromcresol purple in the determination of total aliphatic amine as a salt or as a free base (880). A study of the relation between the structure of adiketones and the resultant color in the Voges-Proskauer reaction indicated that the condensation of a free amidine group and the methyl keto group in an adiketone is necessary for the reaction to occur (647). Salicylic acid forms a complex with crystal violet which is extractable into chlorobenzene (897).

Table 1. Constituent Ga


Material

... ... ... ... ...

... ... ... ... ... Ge

GaAs S i c a t e rocks

..

... ... ... ...

...

*.. .. Hf

... ... ...

.. ...

Simultaneous Spectrophotometric Determinations. A simultaneous spectrophotometric method for uranium and rhenium has been proposed in which both crystal violet associates are co-extracted a t p H 4.1 and then only the rhenium complex is extracted a t pH 2.5 (704). Sodium p-(mercaptoacetamido)benzene sulfonate is the reagent used in a simultaneous method for rhodium and platinum (87). Vanadium and either molybdenum or chromium can be determined simultaneously using tert-butyl pyrocatechol (160). Aluminum and iron in plutonium have been determined spectrophotometrically by measuring the absorbance of the 8-quinolinol complexes in chloroform a t 390 nm and 470 nm, after the removal of plutonium (608). Bismuth, and antimony are determined initially together as iodide complex, and then the bismuth is determined in another aliquot to which citric acid has been added to mask the antimony (437). A simultaneous spectrophotometric method for arsenic and antimony is

Method or Reagent [Wavelength; molar absorptivity] 5.7-Dibrom&quinolinol (CsH4Clt) Rhodamine S (CsHrEt,O) Rhodamine 6G ( C a s ) 6 ( 2 P ridylazo>3,4-dimethylphenol (C6LI [570;-i'x 1 0 4 1 Picramme RG Pyrogallol red [530; 1.o x 1041 3.5.7.4'-Tetrahvdroxvflavone Xylenol orange I551; 3.6 X +Or] ZBromo-4,~ydroxy-4'-aaobensenesulfonic acid [ao; 2.4 x 1041 8-Quinolinol (CHC4) [393; 7.12 x 1081 Differential; pyrocatechol violet Acridine orange NO (CnH4CL) Astrazon pink FG, molybdogermanic acid

t520; 7.55. x 1041 Catechol vlolet, cetyltrimethylammonium bromide Crystal violet, molybdogermanate [590; 1.8 X 1061 Gossypol [545, 1.1 x 1041 Modfied heteroDolv blue [825; 3.58 X lb4]" Pyrocatechol violet Tl'i4(2,2'-bipyridine)iron(II>tris(Pnitrocatechol)germanium(IV) (C*H4Cl?) Bromopyrogallol red, diphenyl guanidine (uoamyl OH) [550; 3.8 x 1041 Picramine [520; 4.03 X lo4] Reduc. of Hf-Mo heteropoly acid, tin(I1) oxalate [730;'6.'7 X lo*] Gallocyanine MS 2-(4-Antipyrylazo)-5-dieth laminophenol Brilliant een, mercury(I6 bromide ccar8C4) [645; 1.15 X 1061 Brilliant green, mercury(I1) chloride

(ca4)

[645; 1.04 X 1061 [4,4'-Bis(dimethylamino)diphenylaminel-"Bindschedler's green" [740; 1.7 X lo6] Bis(Mimet h laminopheny1) (1,3-diphenyl-4-c&or~oxo-2-pyra~olin-4-yl)carbinol, bromde (CsHs) 1644; 5 . 8 x 1 0 4 1 Cry$& yiolet, mercury(I1) chloride (u4He)

...

... ... ... ... ...

[605; 8.2 x 1041 Cr stal violet, mercury(I1) iodide &hMe) [Di-K3-(&hydroxy-7-quinolylazo)-1,5naphthalenedisulfonate [540; 4.38 X lo4] P(2-Pyridy1azo)resrcinol [500; 6.8 X lo4] Schiff base-phenyl glyoxal NADH

Thiot

... Selenium In

...

i605; Z.'o3 x 104 Indirect: cop er(I1) diethyldithiocarbmate &I,)

PAminophen yl-4-ethylbenzylamino-

antipyrinylcarbinol ZBromo-4,5-dihydroxy-4'-azobenzene sulfonic acid [465; 2.3 X 10'1


305 R

Table 1. Constituent In

Material

... ...

... ...

...

... ... .*. *..

...

... *..

K

...

La

... ...

Li


Ferrites

... ... ...

...

Mn

Method or Reagent [Wavelength; molar absorptivity] References ~~-(4-Carboxyl-2-thiazoyl~zo>B-naph- (197) tho1 5,7-Dibromo-8-hydroxyquinoline(EtOAc) (419, 630) N-6’-[(’2-hydroxy-l-naphthyl)azo]-l(166) me thy lanabasine Gallion [mo; 2.2 x 1041 Meldola blue-tetrabromoindium(II1) (PbCl) [585; 2.34 x 1041 l-Methylanabasine-cu-azo-3,4-dimethylphenol Pyrocatechol violet Pyrocatechol violet, cetylpyridinium chloride Quinalizarin Rhodamine B (CsHa-isePr20ise BuCOMe) Nile blue A Stilbazo [ a o ; 1.6 x 1041 3,5,7,4’-Tetrahydroxyflavone Pyronine G tetrabromoindate (CsHa) [530; 9.5 x 1041 Methylene blue (PhNOrCsHs) Leucocrystal violet Kinetic; oxidn of diphenylamine by cerium(1V)sulfate N.N’-Di(a-naphthyl >p-phenylene’diamine (CHCl,) Differential; di icrylamine Indirect, NaBPK; Cu(Phen)aBPh(EtOAc) Chrome azurol S [ ~ o o 1; . 5 x 1041 Salicylic acid; rhodamine S (CaHe) [549; 9 x 1041 4-(5-Nitrophenyl>l- henyl-3-methyl5-pyrazolone (DM$ Chrome azurol S [550; 1.95 X lo4] 1,l’-Dihydroxy-2,2 ’-azonaphthalene4,4’-disulfonic acid Eriochrome black T ; C14HzsMer (PhCHp)NCl(C*H4Clrr) Thymolphthalexon [605; 1.57 X lo4] Xylidyl blue I1 “Ma non” 6’-[(Aminohydroxypfenyl)azo]-lmethylanabasine p20; 7.57 x 1041 Biacetyl oxime thiosemicarbazone Dithizone, p ridine (CHCla) Diphenylcargazone (BuaPO4) [525; 6 X lo4] ~

... ... ... *..

A

h 4

... Mo

Garnet Steel

... ... ... ... ... ...

... ...

[t””,

1.2.7-’

Gluconic acid Differential; 2-methyloxine (CHC13) Bromopyrogallol red[630; 4.89 X lo4] Chrome szurol S 1600; 1 x io41 1,l’-(2,2 ’-Dlsulf04,4’-biphenylene)bis(3-hydroxy-3-phen yltriazene) Differential; peroxymolybdic acid (BQPO4) Magneson (isoamyl OAc) Phenylfluorone [526; 4.38 X lo4] Phenvlfluorone [520;“2.8 X 10‘1 Pyrocatechol violet, dialkylmethylbenzylammonium chlonde (CHCla) [560; 6.25 X lo4] Chromotrope 2B

Kinetic Spectrophotometric Determinations. A kinetic method based (398) (808)

(Continued)

306R


based on determining both elements by the silver diethyldithiocarbamate in chloroform reagent. After the removal of arsenic by distillation from another sample, only the antimony is determined and the arsenic is determined by diiTerence (516). A new simultaneous method for copper arid iron involves the use of 3-(%pyridyl)-5,6diphenyl1,2,4-triazine which forms complexes with iron(I1) and copper(1). The absorbance of the combined complexes in isoamyl alcohol is measured. After the addition of cyanide to convert the copper chelate to the cyanide complex, the residual absorbance due to the iron complex is measured (664). Copper and iron are determined from absorbance measurements at 438 nm and 510 nm of the chloroform extracts of the morpholinium morphine-NdithioIsocarboxylate complexes (86). nitrosoacetylacetone is the chromogenic agent used in determining simultaneously iron, nickel, and palladium (767). A simultaneous method for cobalt, nickel, and copper has been proposed in which the colored complexes formed with Z,&quinoxaline dithiol a t pH 2 are measured a t 510, 606, and 665 nm. At pH 6, the copper complex does not form but the nickel and cobalt complexes are formed (116). The spectrophotometric determination of two- and three-component systbms consisting of the molybdoheteropoly acids of phosphorus, arsenic, silicon, and germanium have been achieved by altering such parameters as reaction medium, acidity, molybdate concentration, a- and 8-modifications and wavelengths of measurement (683). Heteropoly chemistry was also involved in B simultaneous sequential spectrophotometric method for the determination of germanium, arsenic, phosphorus, and silicon (709). Germanium is determined in one aliquot of the sample solution using the isoamyl alcohol extract of the phenylfluorone complex. After removal of silicon by a perchloric acid dehydration, the molybdoarsenic and molybdophosphoric acids are formed, extracted with isobutyl acetate, and determined spectrophorometrically by the simultaneous method. Another aliquot is similarly treated to remove the germanium. The molybdoarsenic, molybdosilicic, and molybdophosphoric acids are formed. Upon addition of citric acid, only the molybdosilicic acid remains and its absorbance is then measured. on the catalytic effect of copper(I1) on the oxidation of 4-hydroxy-3-aminobenzenesulfonic acid t o o-benzoquinone-4-sulfonic acid by hydrogen peroxide has been applied to the specof trophotometric determination traces of copper in high purity salts

($69). The catalytic effect of vanadium on the reaction between branate and anthranilic acid has been used in a photometric-kinetic method for the determination of minute amounts of vanadium (698). A kinetic method for palladium is based on the catalytic effect of palladium(I1) on the reaction of tin(I1) chloride and arsenious acid (816). Kinetic-photometric methods for the determination of traces of cobalt (266) and chromium (198) have been reported. The catalytic effect of phosphate on the reduction of molybdenum(V1) by ascorbic acid is used in a kineticspectrophotometric method for phosphorus (639). The kinetics of this reaction has been investigated and equations developed for the three stages, each with a different reaction rate (871). I n an analogous kinetic method, the catalytic effect of phosphate in the reduction of molybdenum(V1) with tin(I1) is used, the rate of reaction being linear with phosphate concentration (416). A differential kinetic method for the simultaneous determination of silicate and phosphate utilizes the faster formation of the heteropoly blue of phosphorus and is performed using an automatic reaction rate apparatus (381). A new spectrophotometric reaction rate method for the determination of silicon involves the measurement of the initial rate of formation of @-12-molybdosilic acid (987).

Constituent Mo

Material

[Wavelength; molar absorptivity] Gallein, cetyltrimethylammonium bromide Bis(&sminoethyl)dithiocarbnmic acid *.. Thiocyanate, salsolidine (BuPh) *.. Sulfonitrophenol K [650; 5 X 10‘1 ... Thioglycolic acid (CHCls) ... Salicylfluorene,antipyrine (CHCls) ... Wt-Octylpyrogallol Alloys 5,7-Dibromo-&quinolinol (CC4) [390; 7.76 X 1081 All0 steel Thiomalic acid steef 5,7-Dibrom&quinolinol Steel Pyrocatechol, diantipyrinyl methane (CHCls) Steel Extrn. with O,O,S-triethyl dithiophosphate; thiocyanate Steel T m (l,l0-phenanthroline)iron(II)molybdate (PhNO2) Tungsten steel Thiocyanate (BuOAc) [470; 1.87 X lo4] soils WMercapto-p-pro ionophenetidide (CsHeLsoamyl8H) [360; 4.55 X 1081 ... Nitroanthranilazo [4-(2-carboxy-4-nitrophenyl)&meth l-l-phenyl-2pyrazolin-5-oney *.. Alizarin red S *.. Butylthiocarbamate (CHCla-isoamylOH ) ... 6‘- [ [Hydroxy(diethylamine)phenyl] azo]-1-methylanabwine [585; 6.95 X 1041 ... Propyl-3,4,5-trihydroxybenzoate ... N-Methylanabasine a -azoresorcinol ... 3,3’- (N-Methylimine)bis(methylene)dichromotropic acid “Tichromin” 1414; 1.7 x 1041 ... Ti yrogin 5;!3.[ 1.48 x 1041 ... Tichromin ... BuzHPO4(CaHa) ... Salicylic acid Alloys Benzohydroxamic acid (CHCla) [380; 7.7 X loa] Copper alloys 1-(2-Pyndylazo)resorcinol Ores 4(2-Pyridylazo)resorcinol Steel Picramine-a Zirconium, niobium Hydrogen peroxide alloys Steel ZBenzylaminopyridine, thiocyanate [4w; 3.5 x 1041 Steel Sulfochlorophenol S, diphenylguanidine (BuOH) 5,7-Dibromo-S-quinolinol (CHCla) *.. 2,3-Bis(salicylideneamino)benzofuran ... (CHCls) [535; 1.22 x 1041 Dimethylaminoethanethiol hydrochloride Isonitroacetylacetone (CHCl,) ... [340; 2.2 x 1041 p-Hydroxydithiobenzoic acid ~372;6.0 x 104: 530; 1.5 x 1 0 4 1 Mercaptothiadiazolyl azo naphthol 1638; 1 . 5 x 1041 Nickel (I1~8-hydroxy-5-quinoline-sul... fonic acid, zephimmine (CHCls) (400; 1 . 3 x 1041 ... Reduc. of nickel-molybdophosphoric acid complex p 5 ; 1.30 x 1041 ... Diphenylcarbazone (BUaPOd) ~530.7 .x 1041 ... 4-(2-byndylazo)resorcinol [496; 7.3 X lo4] Lead, antimony Dimethylglyoxune (CHCls) Rocks Furil dioxune (CHCls) ... 2-Aminodithio-1-cyclopentene-1-carboxylic acid ... Hexabromoosmic acid ... 1-Phenyltetrazoline-5-thione (CHCla)

...

...

Na Nb

PHYSICS

Topics relevant to the measurement of radiant energy in the visible region will be included in this section of the review. These topics include mainly measurement, methodology, and instrumentation. It has been proposed that the sensitivity of spectrophotometric methods be based on the calculation of two parameters; the sensitivity of the chromogenic reaction and the sensitivity of the analytical method (870). According to this recommendation, the sensitivity of the reaction is determined using the following expression: S = [(C, C n ) / ( A m - A,,)]c,where C, and C, are the concentrations from the calibration plot, A,,, and A , are the corresponding absorbance values, and c is the sensitivity of the photometer. The sensitivity of the analytical method is evaluated by determining the effect of interfering ions, masking agents, losses in the preparation of the sample, etc. on the calibration plot. A paper discussing the estimation of errors of indirect measurements is relevant to direct spectrophotometric methodoiogy (111). The errors derived from the measurement of absorbance using nonmonochromatic radiant energy have

Table I. Photometric Methods for Metals (Continuedl Method or Reagent

Nd Ni

os


(477)

307 R

Table 1.

Photometric Methods for Metals (Continued) Method or Reagent Constituent Material [Wavelength; molar abeorptivity] oe ... Thio anate l - ( Z ~ b z o l y l a z o > Z n ahthol ... Pb ... Z(5-Bromopyrid~laeo kethvlamhohenol - 4.9 x 1041 .. Indirect: anti yrine-klithiomrboxyliarboxylio acid (CHCI$, nickel(I1) nitrate 7-[ ~~-(~Methoxycarbonylaniline)benzyl] ... gqulrlohol [410; 4.5 X 10’1 D$h+ne (CCL) Cast iron D i t h n e (CHCL) Steel Am rhodine 2G -’ Pd ... Araenam ... [w;.1.22 x 1041 ... dnunobenzophenone (benzyl OHCHCb) 1-(5-Bromo-Zthiazolylazo)-%napht hol3,6disu~onic‘acid 1618; 1.38 x 1041 Chromocitromine BH, or chromolan ... orange ... Chromocitromine BH 1470: 1.o x 1041 Chromolan orange ... Cadion 2B ... 1-(ZCarboxy4sulfonatophenyl)-3... hydrox -3-phenyltriaaene Congo or benzopurpine 4~ pia; 1.06x 1041 [590. 7.45 x io*] ... Dimethylglyoxime (CHt)lr) ... 1,l-(2,2 -Dlsulf04,4’-biphenylene)bia-

[A;

A,

... ... ... ... ... ... ,.,

...

... ... ... ...

... ... ...

... ...

... ...

Pr Pt

308R

Catalysts Zircon

...

...

(3-hydroxy-3-phenyltriisaene )

N-Dimethylaminobenzylidene rhodamine

x 1041 Diantipyrylmethane, tin (11)bromide 2,4-Dintrosoresorcinol ~ F u r i dioxime l (CHCb) [380; 2.5 X 10‘1 Eriochrome wanme RC (550; 1.35 2 1041 2-Hydroxy3-sylfo-bnitro henyl[azo]-1naphthylamine3,6-disu~onicacld [482; 1.8 x 1041 5-Hydroxychromone (Cas) 7-Iodo-8-quinolinol-5-sulfonicacid (BuOH) 1430; 9.58 X 1081 2-Mercaptopyridine-l+xide (CHCb) ZMerca tolmidazole &Methy?-& henyl-1,2-dithiole-3thone (CkCb) Nitroso-Rsalt [500; 9.0 x IO’] Nitroso-R-salt - . ..- - . -. - _ .. [505; 1 . 0 5 . ~1041 N-Nitrosodlphenylamine [w;5.3 x 1041 3-Ni troso-2.6-~vridinediol [GO; 2.6 x id41 >Nitroso-1-naphthol (PhMe) [370; 2.15 X .lo4] l-Pheny1-2,3-dunethyl-b yrazolone 1-(2Pyridylazo )-%napht!ol (CHClr1 [624; 1.66 X lo4] %(p-Sulfophen !azo)-l,yh drox 3 6naphthalene&sulfonate &AD&S” ~[l-.pTo~yl)4imidazolylmethylene] rhodamne 1440; 1.92 x 1041 Tin(I1) binary halide complex Tetra henylarsonium alladium(I1) trichorostannate (&IC&) 1-(%Thiazolyl>2-naphthol-3,6onic acid [e+; 1.2 X lo4] 1-Nitroso-%naphthol Direct 3,PDiaminobenzoic acid Diphenyl dithiophosphate [413; 1 X 10’1 (500; 2.33


been calculated (16). Photometric random errors, such as shot and Johnson noisea, sampling, source and optical system fluctuations, scale readability, and systematic errors, such as s h y light, finite slit width, fluorescence, photometric nonlinearity, cell reflection, and sample birefringence, were discussed (84). Multifactor dispersion analysis was used to show that that the most significant factor a!Tecting the correctnegs of spectrophotometric measurements was the inaccurate calibration of the transmittance scale or readout device (401). Better precision in routine repetitive spectrophotometric measurements was reported to be achieved by determining an average daily blank value for each spectrophotometric method and then subtracting this value from the corresponding absorbances of the analytical samples (890). A method for analysing multicomponent systems, especially those with overlapping absorbance maxima, baaed on the mathematical scanning of the absorption spectrum in terms of Gaussian components has been desoribed (40). An equation to be used in choosing between a photomultiplier and a vacuum photodiode for a particular spectrometric application has been derived on the basis of the signal-&noise ratio (389). I n a study of spectrophotometric errors originating from the instability of the instrument and its sensitivity, an equation was derived for the relative measurement error. The equation was tested experimentally and the most unfavorable conditions for measurement were for systems whose absorbance is less than 0.43 (400). I n another experimental evaluation of the accuracy and precision of a linear absorbance spectrophotometer, it waa concluded that errors decrease with an increase in absorbance (430). The solvent effects on photometric measufements has been r e vibwed with special attention to organic systems of environmental significance (668). Special Methodology. Quantitative reflectance photometric measurements of thin layer chromatograms for the determination of amino acids, amino acid derivatives, and nucleic acid derivatives have been investigated (886). The spectrophotometric determination of small disks from paper chromatograms by the use of a special adapter has been described (300). A review on the determination of compounds in mixtures using spectrophotometric measurements discusses several different methods of polycomponent analysis (840). The concept of “normalized absorbance” has been introduced into the classical mole-ratio method for determination of the composition of complexes and a new linear plotting method

used to obtain quantitative information (601). The "normalied absorbance" concept has also been utili5ed in the continuous variations plot method of determining the composition of metal chelates and the corresponding extraction constants (4.4.4). Calibration. A set of three neutral glass filters, designated SRM 930,for checking the photometric scale of visible spectrophotometers is available from the National Bureau of Standards (498). Cells. Single use absorption cells constructed of two superimposed strips of transparent sheeting which are heat-sealed to form a series of pouches have been described. Arrangement of these flexible cells between rigid glass plates provides control of the optical path of these discardable cells (38). A technic based on the use of deformable plastic bags which are transparent in the ultraviolet and visible regions and employing movable jaws with transparent disks to control the optical path length has been described (148). A microvolume flow cell permits a small volume of liquid to be trapped in the cell, the cell to be positioned in the optical beam, and then the movement of the cell into the flow line for flushing (638). A titration cell for the Cary 15 spectrophotometer is coupled with a pH-stat automatic titrator and permits simultaneous spectrophotometric and potentiometric titrimetry (109). A 1 W m l titration cell for the Unican SP 700 spectrophotometer also enables the continuous and simultaneous measurements of absorbance and pH to be made (411). Spectrophotometers. Several new commercial spectrophotometers have been marketed. Varian Techtron has introduced a new model 635 ultraviolet-visible (180-850 nm) double beam spectrophotometer featuring solid state electronics, four scan speeds, and choice of digital readout or meter linear readout in absorbance, transmittance, or concentration (841). Heath/Schlumberger have announced two new instruments, the EU-721 and the EU-707 (8.97). The EU-721 programmed cell ultraviolet-visible (185,850 nm) ratio recording spectrophotometer involves automatic alternate posltioning of reference and sample cells in a fixed optical path. A grating monochromater coupled with a programmable filter assembly gives low stray radiant energy. A 4digit readout of absorbance and transmittance and recorder capability are additional features. The EU-707 double beam ultraviolet-visible ratio recording spectrophotometer uses a rotating mirror to alternately transmit the optical beam through the reference and sample cells and also has recorder readout or a 4digital readout. The Coleman Model

Table 1. Constituent


Material

... ...

Pt

Method or Reagent [Wavelength; molar absorptivity]

...

pu

... ... ...

Rare e a r t h

...

...

... ... ... ...

...

... ... AI oxide Re

*..

... ...

... ... *..

...

...

[600; 4.5 X 10'1 h n a z o . complexon 111 Amenazohdu Carminic acid Carboxyamnazo, diphenylguanidinium salt Chlorophosphonaso 111 Dibensoylmethane 6,7-Dihydroxy-2,4-diphenylbenzo'pyran01 . PhenyMuorone [536; (5.2-5.6) X lo4] l,lO-Phenanthroline, tetrabromofluorescein 8-Quinolinol SalicyMuorone; 1,lO-phenanthroline Tiron Eriocbrome cyanine RC Chrome asurol S Antipyrine oran (CHCII) Brilliant green (EHs) Crystal vlolet (PhMe) [6io; 4 . 4 . x 1041 Dithioamline (4,4'daminodipheny 1)sulfide ~ Q O 1.3 ; x 1041 Nile blue A (C*H4ClS) Thiocyanate Thiosalicylic acid Tris(dipyridine)iron(11) sulfate (Me-

- NO,)

T T-_m t,hinl-

Mo ore Molybdenites Tungsten alloy Rh

... ... ... ... ... ...

Ru

... ... ... *..

... Sb

... ... ... ... ...

...

... ...

...

... ... ...

[330;*3.7x 10'1 Acndme orange (C1HtCL) [505; .7.5 x 1041 a-Funl h o m e , tin(I1) chloride Dimet hylglyoxime [445; 1.47 x 10.41 Enochrome cyanine RC Nitroao-R-sah ~490;1.3 x 1041 P(2-Pyndy1aso)reeorcinol [510; 7.0 X 107 l-(2-Pyridylaso)-2-naphthol (CHCla) [594; 4.66 x 1041 Tin(I1) chlonde Tin(I1) chloride-HCl-HClO, Acenaphthenequinone monoxime [550;.1.5 x 1041 3,PDiamnobenzoic acid 2-Mercaptobenzix+dasole (CHCla) 3-Nitroso-2,6-pyndinediol [555; 2.6 x 1041 Phenylsulfonylbenzamidoxime l-(2-Pyridylazo)-2-naphthol [6$; 9.01 X 10'1 Thocyanate Tropolone (CHC4) [415; 1.87 X 10'1 Basic blue K (PhMe) [638; 6.58 X IO4] Bnlliant reen (PhMe, or PhMeBuaPOPj 2-(3,5-Dibromo-2-pyridylazo)-5-diethylrn-aminophenol [610; 6.2 X IO4] 8-Mercaptoqumoline N-Methylanabaaine- (u'-880-4 )-maminophenol [570- 5 X 10'1 4(2-!Pyridylaso)resorcinol 2-Quinolylazo-p-cresol, iodide (CHCla) [630; 9. X 10'1 6-(2-&umolylazo)-3,4dimethylphenol, iodide (CHC4) Thiocaprolactam (400; 9.84 x lo*] Xanthene dyes

(9-40)

(41.9)

(Continued)


309 R

Table 1.

Photometric Methods for Metals ( C o n t i d )

Constituent Material ores Sb Titanium dioxide steels sc

... ... ... ... ... ... Sn

Alloys

... ...

Sr Ta

Bronze Ores Mo steel Zr or Nb alloys

... ... ... ...

..

... Th

Alloy steel Steel

.. ... ...

... Ti

Rocks Water, ores Uranium ore

...

...

...

... ... ... ... *..

*..

Al alloys Alloy Ores

Method or Reagent [Wavelength; molar absorptivity] References Iodide Rhodamine S Iodide 1,&Bis(Zh droxy-3,5,6-trichloro($oi) phenyl$acet ylformazan [m;2.7 x 1041 BromoDhenol blue [480;i . 4 x 10’1 15-Diantipyrinyl-3-cyanoformazan friochmme azurol G Eriochmme brilliant violet B [562; 6.4 x 1041 Indoferron (600; 9 . 6 X 10’1 4(2-Th1azolylazo)resorcinol [540; 5.06 x 1041 Xylenol orange Bis(hthylaminopheny1 )-antipyrinylcarbinol [635; 4 . 4 X l O f ] Methylene tetraiodate Phenylfluorone 3’-Pyridyl fluorone TI%(l,l0-phenanthroline )iron(I1)t ris(oxalate) tin(1V) (PhNOn) Pyrocatechol violet Gallein 3’-Pyridylfluorone Iron(I1) dimethylglyo?dmate 2,7-Bisazo deriv. of chromotropic acid Alizarin red S Methyl green fluorotantalate Methylene blue (CIHIClz) (660; 1.0 X lo6] Methylene blue (C2H4CL-C1HCls) [655; 6 X 10‘1 Tnmethylthionine (CzH4ClrC2HCla) [660; 6.2 X 10‘1 Malachite green 4(2-Pyridylazo )resorcinol Carboxyarsenazo [675; 3.5 x 1041 Methylthymol blue 2-Quinizarinesulfonic acid Solochrome azurine BS (600; 1.3 x 1041 Arsenazo 111 Arsenazo I11 Arsenazo I11 Antipyrine p60;‘ 1.34 x 1041 1,3-Diphenylguanidinium titanium(1V)indoferron (BuOH) [GOO; 1.8 x 1 0 4 1 ‘ 6-(Benzoylacetyl)-l,4Senzodioxan Chrome azurol S (560; 4.4 x 1041 7,8-Ethylenedioxyflavanol [4,15; .i.51 x 1041 Diantipyrinylmethane p-Dimethylamino henylfluorone Hydrogen perox&, 8-quinolinol (CHCla) [435; 8 X loa] Glycinecresol red 1490; 8 . 5 X 1081 2-Hydroxyphenylfluorone Oxdate, pyrocatechol Quercetin Quercetin, trichloroacet,ate (BuOH) Na N-(2-sulfobenzol)-N-phenylhydroxylamine [410; 4.32 X lo3] Phenylfluorone Pht,halocyaninetetrasulfonic acid Stilbazo 1520: 9.2 X 10‘1 Pyrocatechol-paihy carpine [380; 1.03 x 1041 4,4’-Diantipyrylmethane Diantipylmethane, chromotropic acid Diantipyrylmethane (Contined)

310R


46 with a wavelength range of 195-800 nm has a Littrow-type monochromater with a Mraction grating giving constant dispersion and a direct digital presentation (163). The Cary 17 has

solid state electronics and is essentially a “deluxe” modification of the Cary 14. The Model 17 is capable of computer utilieation in closed loop operation (149). The Acta line of spectrophotometers has been introduced by Beckman. Operatable in single or double beam mode, the ACTA I1 and 111 are single monochromator instrumenta. The Acta I11 is a recording instrument, and a recorder is obtainable as an accessory for the Acta I1 model. I n addition, digital linear readout in absorbance or concentration is a feature The Acta V is a double monochromator spectrophotometer (76). The Bausch and Lomb Spectronic 88 has an 8-nm bandpaas and has optional operational modes of transmittance, or absorbance, or concentration on a linear scale meter (73). The Spectronic 200-UV spectrophotometer is a single grating, double beam instrument with a 190-800 nm wavelength range. Slit widths of 0.25 nm, 0.5 nm, 1.0 nm, and 2.0 nm can be selected. Meter, digital, or recorder displays are optional (79). The new Aminco-Chance DW-2 ultraviolet-visible spectrophotometer features six modes of operation: splitbeam, dual wavelength, dual w a v e length-scanning, derivative, rapidkinetics, and single beam (30). The Unicam SP 1800 and SP 8OOO have numerous operational selections including multichannel kinetic capability, digitai readout for the SP 8O00, printout, and flat-bed recorders. The Unicam models SP 700A and SP 700C are primarily precision research spectrophotometers encompassing the ultraviolet, visible, and near infrared regions (674). The Zeiss DMR-21 recording spectrophotometer has options of ten chart speeds and eight wavelength presentations; and has a fully thermostated cell compartment and cell holders (146). Hilger has introduced three models of Uvichem, a single beam spectrophotometer with a wavelength coverage of 220 to 830 nm. A digital model has the typewriter output facility. The digital and standard Uvichems have a curve correction capability (696). Special Application Instruments. The Spectronic 400 automatic sampling system has been developed to handle the sampling, diluting, and reagent adding operations prior to delivering to the micro flow-through cells of a Spectronic 100 equipped with a DP-100 data printer ( 7 4 ) . A device for studying the absorption spectra of molten salts has been designed (433). A spectrophotometer equipped with an absorption cell connected to a vacuum system and appli-

cable to atomic absorption and atomic fluorescencespectrometric measurements has been patented (106). A scanning spectrophotometer has been designed for obtaining firstderivative absorption spectra by irradiating the sample with a measuring beam and a reference beam differing by 2 nm so that the necessity of a reference cell is eliminated (960). Two optical beams of different wavelengths are time-shared upon traversing a-single cell and the differential absorbance being measured. This dual wavelength spectrophotometric method has been proposed to analyze two component systems as one component is essentially masked instrumentally (676). A flow-through cell attached to a liquid chromatographic column and a rapid-scan spectrophotometer have been used to obtain a recorded spectrum for each fraction within 2 minutes (62). A special optical system to handle small volumes of the sample in an elongated optical path has been developed (709). A spectrophotometer has been designed for the measurement of 50 r l to 1 ml of sample solution by immersing a light pipe into the sample solution and having the readout correlated with the distance of immersion (31). Modifications in the photometric system of an automatic photometer in order to reduce light scattering errors by the use of glass fiber optical devices has been disclosed (630). A rotating disk with circularly arranged siphonable cuveh is a device which has been patented for the rapid and simultaneous analysis of many samples (36). Another apparatus for measuring a large number of samples utilizes a rotary table and an oscilloscope readout in the photometric scanning process (480). A photometer with a single light source and detector has been so designed that the sample cell windows are aligned axially in a centrifugal rotor (36). A description has been given of a photometer with a cam-operated mechanism to synchronize the tilting of an interference filter with the program of an automatic analyzer (314). An automatic colorimeter programmable to run blanks between samples a t the rate of about 6 sec per sample has been described (194). A Micro-Turbidimeter Model 560 has been designed to detect minute differences in trace concentrations of particulate matter in air and water (627). A miniature photometer for the ultraviolet and visible regions is suitable for monitoring continuously the effluents from chromatographic columns a t two wavelengths (792). A low cost double beam photon counting photometer with partially compensated dead time has been described For special application instrument construction, the SchoefEel Instrument Corp. offers a variety of monochroma-

(a).

Photometric Methods for Metals (Continued) Method or Reagent

Table 1.

Mat,erial Constituent Niobium, tantalum Ti Si-Zr Pigments

T1

Steel with Se

... ... ...

... ...

... ... ... ... U

Ores Tungsten

...

... ... ...

... ... ... ...

... ... ... ...

*..

V

Ores Sodium

... ...

...

[Wavelength; molar absorptivity] References Salicylfluorone,antipyrine, perchlorate l,S-Dihydroxy-2- [N,N-bis(carboxymethyl(ammomethyl]-3,bnaphthalenedlsulfonic acid Differential; diantipyrylmethane (390; -6.8 X lo4] Diantipyrylmethane Anthrazo 1-[p-(dmeth 1amino)phenylazo] anthraquinone zydrochloride (CHCl,) (570; 6 X lo4] Bis(khnethylaminophenyl>l-phenyl(447) 3-methyl-Pchloropyrarolin-5-yl) carbino1 3,5-Dibromo-2- yridylazo-m-(diethylamine)phenoP Indirect: TlBPh,, Hofmann's violet Indirect: antipynne4dithiocarboxylic acid (CHCls) nickel(I1) nitrate Dimethylthione [ y 5 ; 7.3 x. 1041 Trmethylthlone I6601 1 X 1061 Toluidme blue [660; 1.17 X 106 Methylene blue ( &e-PhCOME) Methylene blue ( C I H ~ C ~ ~ - C ~ H C ~ ) 1655: 1.14 X 1061 Methylene &en (CtH4ClrCtHCla) [655; 8.14 x 1041 ;Yictoria blue UR (CsHs) m: 8.5 x 10'1 Nile 'blue 1640; 8.3 x 1041 Methylene green (640; 1.22 x 1051 Tetrabromothallate, methyl green (mxylene) [645; 1.14 X 1061 Tetrabromothallate, fuchsine (1,lC~H~C~~CIHCL) (545; .g x 1041 Fuchslne (BuOAc) Methyl vlolet 3,6-Bis(4-carboxy-3-hydroxyphenylazo )-4,5dihydroxy-2,7-naphthalenedisulfonic acid (580; 1.43 X 10'1 Arsenaeo I11 (Bu Cellosolve) [653; 3.58 x' 1041 Crystal vlolet (PhMe) 1610; 7.6 x 1041 1-(1-Hydroxy4methyl-2- henylazo>% naDhthol-4 sulfonic a c i g Chrome azurol S, cetyltrimethylammonium chloride [625; 4.0 X 1061 5,7-Dichloro-&hydroxyquinoline N_ _ . oxide Phosphonazo 111 1660: [660; 6.0 X X 1041 Chlorophosphonaeo 1670; 7.96 x 10.41 Erioc-hrome cyarune R, or pyrogallol red Methyl green-benzoate complex of (7766) uranium(V1) [MO;9.7 x 1041 Trimethylthionine (CIHIC~~-C,HC~S) (776) Uranium(V1jalizarme red-l,Mi(6631 phenylguanidinium [580; 6.5 X lo*] %(%Pyridylazo)-Miethylamhopheno1 (164) Rhodamine B, 3-pyridinecarboxylic (696) acid (C&) hsenazo I11 (670) Arsenazo I11 (801) Chrome azurol S, eephiramine (307) [610; 6.83 X lo4 N-Benzoyl-9-tolyl ydroxylamine (460) N-(o-Chlorobeneoyl).N-phenylhydroxyl- (686) armne [530; 4.4 X lo*]

A

h

(Continued)


311 R

Photometric Methods for Metals (Continued) Method or Reagent Material [Wavelength; molar absorptivity] Calcichrome [a; 1.0 x 1041 ... Cinnamohydroxamic acid (l-octanol) [450; 7.0 X 10'1

Table 1. Constituent V

...

...

... ...

...

... ... ... (VOCb)

v

Titanium tetrachloride Glass Silicate rocks Mercury

...

W

... ... soils Steel Steel

...

Y

Chromium alloys

... ... ...

Zn

... Al alloy Acids

Alloys Lead

...

Zr

... ... ... ... Steel

1s alloys

312 R

0

2(3,5Dibrgmo-Zpyridylaw>5diethyl-

(630.5 . 4 x 10'1 4 (2byndylaw)resorcinol

N-Phen 1-%furan acrylohydroxamic acid 6 H C L ) PhenyMuorone [so.1.7 x 1041 6(%byndylazo)thymol (CHCL) N-Phenyl3-styrylacrylohydroxamic acid

6(2P idylszo)-3,4-dimethylphenol (CCG [630; 7 . x 10'1 N-(m-Nitrobenzoyl)-N-phenylhydroxylamine boamvl OH) [435; 3.93 x io81 ' Pyrocatechol vlolet (555; 3.68 x 1041 Tiron [570; 6 . 4 X loa] Diphenylbenzidine Thioglycolic acid Gomypol bis [N-(2-hydroxy)imine] Ammonium peroxydmlfate, pyrocatechol Dih droxythiazo[%(3,44hydroxypienylazo >ephenyl-5benmylthiawle] [ao; 7.0 x 1041 8-Mercaptoqwnoline (CHCb) [412; 3.67 X lo*] Phenylfluorone [453; 8 . 5 X 10'1 Tetraphenylarsonium thiocyanatotungstate(IV) (CHCL) zinc dithiol 5 7-Dibromo-8-quinolinoI (S,H&ls) Thiocyanate (CHCL) Salicylic acid, rhodamine S (CJI6) (551; 1.1 X 1061 Araenazo 111 Chrome azurol S [550; 4.3 X lo*]. l,lO-Phenanthrohe, bromcresol green 4(%Pyridylaso)resorcinol [493;8.3 x 1041 Victorm blue B zinc thiocyanate ( C a s BGO4) Sulfarazene 4(6Methoxy-3-methyl-%benzthiazolium-ylazo)-N-methyldiphenylamine chloride-Zn (SCN14 (Ce"sB~aP04) 5Nitrophen l(%azo-l'>2'@-scetylhydraziner napht halene 1-(ZPyridylaao >%naphthol (CHCL) pDimethylaminophenyluorone 1490; 1.2 x 1041 Araenazo 111 Indoferron [805; 3.18 x 1041 Picramine-e [ M O ; 3.73 x 1041 4- (ZF'yndylazo)resorcinol 1500; 6 . 2 X 10'1 g&ziinolinoi (xyims) (Tri-n-octyl hosphine, oxide-PhMe), pyrocatecio~violet, aniline 5.00 x 1041 Xylenol orange


Referenw (3.99) (641) (879)

tors, high energy sources, filter holders, filters, iris diaphragms, and photometers (666). An optical multichannel analymr, SSRI Model 12050 MA, can process quantitatively, display, and signal average simultaneously optical data from hundreds of channels. The prospect of recording simultaneously a large number of spectral points rather than sequentially in the visible region seems to offer some interesting possibilities in kinetic and polycomponent analyses (717). APPLICATIONS

Methods of Analysis. Many new reagents, revised methodology, and a variety of sample materials have resulted in hundreds of applied publications in the past biennium. Many of these applications have been summarized in Tables I, 11, and 111. Several new and revised photometric methods are found in the Thirteenth Edition (1971) of "Standard Meth6ds for the Examination of Water and Wastewater'' (33). Color Specification. The C.I.E. system has been used to calculate the trichromatic coordination of indicators and to evaluate color changes (364,876). The Zeiss D M C recording spectrophotometer for color measurements continuously records the spectral reflectance simultaneously with the logarithm of the KubelkaMunk function. Reflectance and transmittance values are automatically printed in digital form a t preselected wavelength increments. The tristimulus values for the illuminant selected are also computed and indicated on a printout (147). Accurate color measurement, matching, and specification in terms of tristimulus color values using Beckman spectrophotometers and associated equipment has been discussed (7'7). LITERATURE CITED

1).

(8j Zbid., 18,91 (1971).

(9)Zbid. p405. (10)Zbd., p 733. (11)Adamovich, L. P.,Mirnaya, A. P., Khuthryanskay, A. K., Zavod. Lab., 35,781(1969): (12) Add, A. S., Ayazi, A. A., Ajmal, A. I.. Hashmi, M. H., Mikrochim. Acta, 1970,606. (13) Agarwala, B. V., Dey, A. K., Nat. Bead. Sci., India, Sect A , 40, 49 (1970). '

(14) Agrinshya, N. A., Goloenitskaya, V. A., Kovalenko, E. V., Tr. Nouochetkassk. Politekh. Znst., 220, l(1969). (15) Agterdenbos, J., Jutte, B. A. H. G., Elberse, P. A., Talan?, 17, 1OS5 (1970). (16) Agterdenbos, J., VI&, J., zbad., 18, 467 (1971). (17) Akaiwa, H., Kawamoto, H., Abe, M., Bull. Chem. SOC.Jap., 44, 117 (1971). (18) Akatsuka M., Amamoto, H., Yoshinaga, S., hunseki Kagaku, 20, 406 (1971). (19) Akhmedli, M. K., Granovskaya, P. B., Melikov, A. A., Uch. Zap. Azerb. Cos. Univ., Ser. Khim. Nauk, 1969, 13. (20) Akhmedli, M. K., Ivanova, L. I., Azerb. Khim. Zh., 1, 106 (1969). (21) Akhmedov, S. A., Tataev, 0. A., Sb. Nauch. Soobshch. Dagestan. Goa. Univ., Kafedera Khim., 5,32 (1969). (22) Akhmedov, S. A., Tataev, 0. A., Abdullrrev, R. R., Zavod. Lab., 37, 756 (1971). (23) Akimov, V. K., Busev, A. I., Zh. Anal. Khim., 26,134 (1971). (24) Akki, 5. B., Khopkav, S. M., Separ. Sci., 6, 455 (1971). (25) Alekperova, A. A., Alekperova, R. A., Zolotov, Y. A,, Zh. Anal. Khim., 25, 2283 (1970). (26) Alieva, R. A,, Akhmedli, M. K., Ayubova, A. M., Azerb. Khim. Zh., 6, 129 (1969). (27) Alimukhamedova, M. M., Bukina V. K., Fiz. Khim. Zssled Glinistyki Miner. Silikat. Mater., 1970, 110. (28) Alinovskaya, L. A,, Ishchenko, N. N., Ganago, L. I., Vestsi Akad. Nwuk Belarus SSR, Ser.Khim. Navuk, 6, 113 (1970). (29)Alvarez de Brito, J. M., Rev. Met. (Madrid),6,45 (1970). (30) American Instrument Co., Div. of Travenol Laboratories, Inc., Silver Spring, Md., Bulletin. (31) American Optical Corp., Ger. Offen. 1,916,074 (Cl. G O h ) , 20 Nov. 1969, US Ap 1 15 May 1968; 41 pp. (32) Zb$ Ger. Offen. 2,007,405 (Cl. G O h , B Oll), 08 Oct 1970, US Appl 19 Mar 1969; 12 pp. (33) Amer. Public Health Assoc., “Standard Methods for the Exynination of Water and Wastewaters, 13th ed., Washington D.C 1971. (34) Amin, d., Kh&tak, M. A., Pak. J . Scz. Ind. Res., 13,209 (1970). (35) Anderson N. G., Ger. Offen. 1,962,267 (Cl. G dln), 09 Jul 1970, US Appl 18 Dec 1968; 27 pp. (36) Zbid., Ger. Offen. 2,009,993 (Cl. B Oll), 24 Sep 1970, US Appl 13 Mar 1969.16 DD. (37) Ahdrade H. A., Hainberger, L., Brehmel, If. L., Z . Anal. Chem., 253, 351 (1971). (38) Andreeva, 2. F., Deikova, 2. E Dokl. T S K H A (Timirydzev. Sei? skokhoz. Akad.) 1969, No. 149 293. (39) Angermann, W Kaasner, 8. Lorenz, G., Geissler, M., Clem. Anal. (Fbarsaw), 16,261 (1971). (40) Anti ova-Karataeva, I. I., KazaM., Zh. Anal. Khim., 26, 448 nova, (19711. (41) Ardasheva 0. K., Naumova, 0. N., Probl. Anal. khim., 1, 253 (1970). I., Rev. (42) Armeanu, R a m . Chim., (43) Amlanova, N. V. M asoedova, A. S., Sudakov, F. P., Zh. , & a ~Khim., l. 26, 947 (1971). (44)Ash, K. C., Piepmeier, E. H., ANAL. CHEM.,43,26 (1971). (45) Ashworth, M. R. F., Venn, I., Anal. Chim. Actu 49 535 (1970). (46) Asmus, h., banzke, J., Schwarz, W., ’ Z . Anal. Chem., 253, 102 (1971). (47) Asmus, E., Jahny, J., ibid., 255, 186 (1971).

8

2:lg?fk%).

Table II.

Constituent

Material

...

As

Brass

B

...

Organometallic compds Pyrite cinders Steel

CblorosiiCopper alloys Organi+metallic Orgmc compds Steel Steel

Azomethine H Acet lquinalizarin Metlylene blue (CtH4C11)

...

... ...

Br-

...

BrOt -

..

c1-

... ... Metals

Rusted steel Selenium

... ...

... ... ... ... ... ... ..

co F-

... ... ...

... ... ... ..,

HrO

Hlo, I-

[Wavelength; molar absorptivity] Tetraidomethylene blue iodate 8-Mercaptoquinoline (CCL) Prelim. extractn of AsBra(CC4); heteropoly blue Heteropoly blue Heteropoly blue (BuOH-EtlO) Heteropoly blue Dianthrimide Chromotrope 2B [580; 1.3 X 1041 J+US peep, BF:(GHtClt-C&) II 8umahzarin ~ Hd304-HOAc urcumm curcumin Ammethine H

...

ClO: clodClO, CN -

Photometric Methods for Nonmetals Method or Reagent

Fossils Rocks Uarnium oxides Water Org. solvents Org. solvents Org. solvents Org. compds

... ... ... ...

... ... ... ... ... ...

...

Malachite green chloramine B Nile blue A (CdCb) Triphenylbenzyl hos honium salt, sodium pyrosulfite (Cl!L4CP,) [359; 3.29 x lo*] Antipyrine, nitrite [525; 2 X 10’1 Indmect; mwcur (11)thiocyanate, crystal violet sulfate (6bC1) Indirect; cbloropyridine mercury(II), dithizone o-Tolidine Indirect mercury(I1) t+iocyanate, iron (111) Konig reaction; barbituric acid Crystal violet (PbC1)

Indirect; mercury(II), copper(I1) diethyldithiocarbamate -(CC4) 2.9 x 1041 Indirect; sdver(I), 1,l0-phenanthro1inel bromopyrogallol red Indirect; mercury(I1) chloranilate Silver sodium sulfamoylbenzoate Alizarin fluorine blue Cerium(III)-alizarin (n-pentanol, EtrN) Iron (111), N,N ‘-b.is(Bhydroxypropyl-ophenylenediamme ) Indirect; scandium pyrocatechol violet Thorium-arsenazo Zirconium-solochrome cyanine R Zirconium-gallein, cetylpyridinium chloride Alizarin fluorine blue Decolorization; aluminum-arsenazo Zirconium, xylenol orange Aluminum-eriochrome cyanine R Dichromate Lead tetraacetate ( c a s ) 1-MethyL6hydroxyquinoliniumbetaine Cobalt(I1) chloride Leucocrystal violet; horseradish peroxidase Ferroin (PhNOs) Chem. amplification; periodate-iodateiodine Indirect; silver(11, 1,10-phensnthroline, bromopyrogallol red Indirect; mercur (11)dithizone Crystal violet (PKc1) Chloramine B; brilliant green Nile blue A (CHCL) Neutral red (PhNOr) 1552: 3.25 x 1 0 4 1 Eiidaiiine S (Et&&&) 3,4,5,6-Tetrachloro-3’,4’,5‘,6’-tetrahydroxy. . . ’ duoran Me ester Triphenylbenzyl hos honium salt, sodium pyrosulfite ( ~ 2 % & )

[e;


313 R

-

(318)

(48) Asmus,E., Noak, K., ibid., 249, 122 (1970). (49) Asmus, E., Weinert, H., ibid., p 179. (50) Attari, A., Igielski, T. P., Jaselskis, B., ANAL.CHEM.,42,1282 (1970). (51) Ayres, G. H., Arno, J. A., Talantu, 18, 411 (1971). (52) Baba H. Shindo, Y., Fujita M., Yamazaki, ‘k., Kogyo Kagaku Zhashi, 73,2131 (1970). (53) Babenko. A. S.. Ukr. Khim. Zh.. 37. ’ 273 (1971). ’ (54) Babko, A. K., Shkoravskii, Y. F., Ivashkovich, E. M., Zh. Anal. Khim., 26,854 (1971). (55) Baiulescu, G., Danet A. F., Papagheorghe, M., An. dniu. Bucuresti, Chim., 19, 107 (1970). (56) Baiulescu. G., Marinescu, D., Greff, C., Analyst, 95, 661 (1970). (57) Bakal, G. F., Lisetskaya, G. S., Ukr. Khim. Zh., 37, 594 (1971). (58) Bakunina L. I., Murashova, V. I., Zh. Anal. Khim., 25, 142 (1970). (59) Balasubramanian, S., Kuloor, N. R., Indian J . Chem., 9, 273 (1971). (60) Balica, G., Ciobanu, L., Rev. Chim. (Bucharest),21, 643 (1970). (61) Baresel, D., Jaetsch, K., Z. Anal. Chem., 249, 234 (1970). (62) Bartos. J.. Chim. Anal. (Paris). 53.. ‘ 384 (1971). ’ (63) Bartos, J., Pesez, M., Ann. Pharm. Fr. 28,459 (1970). (64)bartos, J. Pesez, M., Bull. SOC. Cham. Fr.! 1950, 1627. (65) Basarm, N. N., Akhmedli, M. K., Islamov, S. U., Zauod. Lab., 37, 269 (1971). (66 Basargin, N. N. Akhmedli M. K., dafarova, A. A,, dh. Anal. Khim., 25, 1497 (1970). (67) Basargin, N. N., Akhmedli, M. K., Shmnov, M. M., Tr. Novocherkassk. ‘Politekh.Inst., 220, 74 (1969). (68)Basargin N. N., Ayubova, A. M., Akhmedli, k. M., Azerb. Khim. Zh., 3, 126 (1970). (69) Basargm N. N, Yakovlov, P. Y., Panarina, d. A., Sowem. Melody Khim. Tekhnol. Kontr. Proizvod., 1968, 102. (70) Basargin, N. N., Yakovolov, P. Y., Panarina, N. A., Zh. Anal. Khim., 25, 746 (1970). (71) Baszrgin, N. N., Yakovlev, P. Y., Panarina, N. A., Gnuchina, G. V., Zavod. Lab., 37, 143 (1971). (72) Bausch and Lomb, Anal tical Systems Div.. Rochester. N.%., 14625, Bulletin. . (73) Zbid., Bulletin 33-6059. (74) Zbid., Catalog 39-6023. (75) Bausova, N. V., Lebedeva, E. M., Tr. Znet. Khim., Akad. Nauk. SSSR, Ural. Filial 1968; No. 18, 40. (76) Beckman Instruments, Inc., Scientific Instruments Div., Fullerton, Cal. 92634, Bulletin. (77) Zbid., Data Sheet DK-78-MI. (78) Behrends, K., Klein, H., Z. Anal. Chem., 249, 165 (1970). (79) Belcher, R., Hamya, J. W., Townshend, A., Chim. Anal. (Bucharest),1,23 (1971). (80) Bermejo Martinez, F., Branas, G., Mikrochim. Acta, 1971, 489. (81) Bermejo Martinez, F., Rodriguez Compos, J. A., Acta Cient.Compostelana, 6.95 (1969). . , (82j Bermejo Martinez, F., Rodriguez Compos, J. A., Inform. Quim. Anal., 24, 77 (1970). (83) Bermejo Martinez, F., Vila Brion, J., Acta Cient. Compostelana, 7, 107

(616)

(84) Bertolacini, P. L., Boll. Lab., Chim.

Table II. Photometric Methods for Nonmetals (Continued) Con stituent

NxHi NHa

NOS-

Method or Re ent [Wavelength; molar %orptivity] References ... Victoria blue B (COHO) (6881 Soils Kinetic; oxidn of iron(II1) thiocyanate by (609) nitrous acid Molybdotungstophosphoric acid ... (740) [680; 2.7 X 1081 1-(4-P ridy1)pyridinium chloride ... (46 ) Indopzenol ... (638) Indophenol; Ncm[Fe(CN)sNO]aa catalyst (889) ... Indophenol, thymol ... (9911 [660; 1.16 X 10‘1 Indophenol, m-cresol (886) Indophenol, thymol (iso-BuOH) (883) Chloramine TIthymol ... (486) Guaiacol ... (8841 o-(Benzenesulfonamid0)-pbenzoquinone ... (413) Mercury (I1) methylt hymol blue (408) [610; 5.84 X IOa] Indophenol; automated Steel (168) Indophenol, thymol Uranium (893) Indophenol, thymol Zirconium (8941 Brucine ... (846) 3,3’-Diaminobenzidine, toluene-3,4-diamine (446 ) [350;,3.5 X lo8] 2,3-Diarninonaphthalene (869) Modified Griess; CHCla extractn, retro... (4641 grade extractn Sulfanilamide, N-l-naphthylethylenedi... (637) amine dodec lbenzenesulfonate (CC14) 3,4 5,6~etrac~ro-3’,4’,5’,6’-tetrahydroxy-(606) duoran Me ester Iron(II), barbituric acid ... (178) Uranium compds 2,PXylenol (PhMe) (380) Brucine ~. ... (646) ... Reduction; Griess (439) [528; 6.0 X loa] Crystal i.iolet (PbCl) ... (886) 2,4-Xylenol Uranium compds (7961 N ,N-Dimethylaniline Gas mixt. (93) Di-cyclopentadienyl titanium(II1) dichloGas stream (867) ride on porous substrate Organic compds (313) Convefsion to CO; 1 9 0 s ; iodine in inert carrier gas Semi-automatic; dihydroxytartaric acid (170) Na aluminate solns 2 4dinitrophenylosazone “Alkalone I” ... Moiybdophosphoric acid (373) Molybdophosphoric acid, crystal violet (808) ... (BuOAc-MetCO) [590; 2.49 X lo6]. Molybdophosphoric acid, crystal violet (64) .. (BuOAc) Molybdophosphoric acid (PrCO&HC18) (348) ... ... (669 Molybdovanadophosphoric acid [400; 3.11 X loa] ... Molybdovanadophosphoric acid (667) I . 75 x 1031 ... Heteropoly blue-extraction (9641 ... Heteropoly blue; ascorbic acid, K anti(863) monyl tartrate ... Heteropoly blue, titanium(II1) chloride as (734) reductant [@io;2.9 x 1041 ... (878) Bis (4dimethylaminophenyl)antipyrylcarbinol, molybdophosphoric acid [620; 3.8 x. 1041 ... Indirect; acid chrome violet or acid (43) chrome black special Molybdophosphoric acid (BuOAc); hetero- (834) Aluminum pol blue Organic compds Molyidophosphoric acid (670) Steel Molybdovanadophosphoric acid (108) Steel Molybdovanadophosphoric acid (iso(438) Material

...

NOS-

OS

OH P

~~

Wheat leaves Zirconium, titanium, tungsten

P,o,~Sa-

... ...

~

BuCoMeb

Heteropoly lue, ferrocene as reductant Molybdovanadophosphoric acid (isoBuCOMe) [400; 3.1 X loa] Trans-dichlorobis(ethy1enediamine)cobalt-

...

(736) (668) (678)

(Continued)

314R


I

.

I,

~

(1970). ~ - .,. .

Prov.. 20. 119 (1969). (85) Beyer: W., Likussar, W., Mikrochim. Acta, 1971,610.

(86) Bhadra, A. K., Banerjee, S., Indian

J . Chem. 7,936 (1969). (87) Bhandari C. S., Bhandari, M. R., Sogani, N. d., J. Indmn Chem.Bot., 46, 975(1969). e (88) Bhargava, 0. P., Hines, W. G., T a b n h , 17, 61 (1970). (89 Bhargava, 0. P., Pitt, G. F., Hines, G., ibid., 18,793 (1971). (90) Bhargava, S. P., Sogani, N. C., Z. Anal. Chem., 255,36 (1971). (91) Zbid., p 260. (92) Bhat A. N., Gupta, R. D., Jsin, B. D., Indian J. Appl. Chem., 32, 52 (1969). (93)-Bhatty, M. K., Townshend, A,, Anal. Lett., 4, 357 (1971). (94) Bhura, D. C., Tandon, S. G., Anal. Chim. Acta 53, 379 (1971). (95) Bhura, b. C., Tandon, S. G., Indian J . Chem., 8 , 1036 (1970). (96) Blazejak-Ditges, D., Z . Anal. Chem., 247,20 (1969). (97) Zbid., 251, 11 (1970). (98) Blazejak-Ditges, D., Klingeleers, H., ibid.. 248. 18 (1969). (99) Biyum I.‘ A., ‘ “Extraction-Photometric dethods of Analysis with the Use of Basic Dyes,” Nauka, Moscow, 1970, 219 pp. (100) Bodart, D. E., 2.Anal. Chem., 247, 32 (1969). (101)’Bokra, Y., Luca, C., Chim. Anal. (Bucharest), 1, 44 (1971). (102) Boltz, D. F., Gupta, H. K. L.. “Ultraviolet and. Visible Absorption S ectrophotometry,” M. N. Sastri, E$. “Vlstas in Analytical Chemistry,” Chand, Delhi, 1971 p 1-23. (103) Boltz, D. F., h e l g n , M. G., ANAL. CHEM., 36, 256R (1964); 38, 317R (1966): 40. 255R (1968): 42., 152R . (1970j: (104) Bolynkin, N. I., Tekh. Kino Tolev., 13,34 (1969). (105) Bordonali, C., Baincifiori, M. A., Ger. Offen. 2,048,862 (C1. GOlj)22Apr 1971, Ital. Appl. 04 Oct 1969; 26 p . (106) Bosch Serrat, F., Inform. &im. Anal., 25,17 (1971). (107) Bosch Serrat, F., Rodriguez Polo, D., Guardiola, J. L., ibid., p 91. (108) British Iron and Steel Research Asoc., J. Iron Steel Znst., London, 209, 364 (1971). (109) Bruice, T. C., Maley, J. R., Anal. Biochem., 34, 275 (1970). (110) Budesinsky, B. W., Svec, J., Microchem. J., 16,253 (1971). (111) Budyak N. F., Gryaznova, I. S., Zh. Prikl. khim. (Leningrad), 44, 669 (1971). (112) Bugaevskii, A. A,, Blank, A. B., Zh. Anal. Khim. 26, 11 (1971). (113) Buganova, k. G., Bagdasorov, K. N., Tataev, 0. A.. Sb. Siutei Molodvkh. U&. Dagehn Fii. Akad. Nauk SSSR, 1969,198. (114) Bunikiene, L., Ramanauskas, E., Jankanskaite, Z., Liet. TSR Aukst. Mokyklu Mokslo Darb., Chem. Chem. Technol., 10, 37 (1969). (115) Burke R. W., Deardorff, E. R., Talanta, I f , 255 (1970). (116) Burriel-Marti, F., Cabrera-Martin, A., Marinas, J. M., Inform. Quim.Anal., 24,200 (1970). (117) Buscarons, F. Canela, J., Iturriaga, H., Quim.Ind. (dadrid),17,6 (1971). (118) Busev, A. I., Cherkesov, A. I., Zadumina, E. A., Isv. Vyssh. Ucheb. Zaved., Khim. Khim. Tekhnol., 12, 1649 (1969). (119) Busev, A. I., Evsikov, V. V. Zh. Anal. Khim., 25,953 (1970). (120) Busev, A. I., Gorbunova, N. N., Ivanov, V. M., Zavod. Lab., 37, 26 (1971). (121) Busev, A. I., Ivanov, V. M., Bog-

3.

Table II. Photometric Methods for Nonmetals (Confinued) Constituent

Method or Re ent [Wavelength; molar %sorptivity] Referencee Crystal violetrtetraiodomercurate(I1) ... Indirect; mercury(I1) chloranilate ... Indirect; copper(11)chloranilate Indirect; iron(II1); l,l0-phenanthroline ... ... Indirect; iron(II1); 2,4,Btri(%pyridyl> 13 &triazine ... IndLkct ; mercury(I1) chloranilate ... 4,4’-Dithiodipyridine, or 5,5‘-dithiobis(2nitrobenzoic acid) ... Nitroprusside [492; 1 x lO*a] ... Indirect; barium dih droxytoluquinone 2,7-Bisazo deriv. of ciromotropic acid ... comdex with barium 2-Amiio erimidine hydrochloride; ... nepheg metric ... Crystal violet (PhCl) ..* Neutral red *.. N, N-Bis (8-benzoylethyl>o-phenylenediamine Brilliant green ... ... 3,3 ’-Diaminobenzidine 2,3-Diaminonaphthalene [377; 2.64 x 10‘1 3,3’-Diaminobenzidine (C&) Steel 2,3-Diaminonaphthalene Steel Tellurium Colloidal; acetone reductn, gelatin Tellurium dioxide o-Phenylenediamine (PhMe) Heteropoly blue Heteropoly blue (PrCOs-CHCle) [775; 2.02 x 1041 ... Rhodamine B molybdosilicate (CHCk) ... Rhodamine B molybdosilicate [590; 2.35 X lo6] Fluorspar Molybdosilicic acid Automatic; hetero oly blue Ores, iron Molybdosilicic acidJ std. addn. Steel Tellurium Heteropoly blue (BuOH) Uranium dioxide Heteropoly blue Vanadium Hetero oly blue (Go-BuCOMe) Molybiosilicic acid Organic compds Resistor alloy films Hetero oly blue Mol bxosilicic acid Tin ... 1,46iphenylthiosemicarbazidehexabromotellurate [480; 5 X 1041 .. Hexabromotelluric acid [320; 1.6 X 10’: 440; 3.0 X lo*] ... 3,5-Diphenyl-2,6-dimercapto-4H-thiopyranMaterial

...

so1 SOP

~~

so‘’SCN Se

Si

, I

Te

... .. .. Selenium Steel Steel Steel

Pone - ___

Methyl violet, iodide [540; 1.71 X lo4] Thionaphthenic acid Victoria blue 4Rbromotellurate (CC14PhNOd [602; 8.0 X 1041 Merca tobenzothiazole (CHCla) ColloiCPal Bismuthiol I1 (CHCln) [330; 3.5 X IO4] - ’ 3-Phenyl-5mercapto-1 3 4thiazole-2(3H )thione “Bismuthiol 11’’(CCL)

danovich, L. I., Sovrem. Metody Anal. Mater., 1969, 253. (122) Busev, A. I., Ivanov, V. M., Bogdanovich, L. I., Zh. Anal. Khim., 24, 1273 (1969). (123) Busev, A. I., Ivanov, V. M., Cresl, V. G., Sovrem. Metody Anal. Mater., 1969,232. 1124) A. I.. Ivanov. V. M.. Gor. bunova, , Busev. - h!. N., bresl,V.’G., Tr.’Kom. Anal. Khim., Akad. Nauk. SSR, 17,

(127) Busev, A. I., Rodionova, T. V. Anal. Lett., 3, 235 (1970). (128) Busev, A. I., Rudzit, G. P., Tsurika, I. A., Zh. Anal. Khim., 2 5 2154 (1970). (129) Busev, A. I., Shshkov, A. N., Natura (Plovdiv), 3, 71 (1970). (130) Busev, A. I., Shvedova, N. V., Akimov, V. K., Zh. Anal. Khim., 24, 1679 (1969). - -, (131)Busev, A. I., Shvedova, N. V., Akimov, V. K., Fursova, E. G., abid., p

(125) Busev, A. I., Ivanov; V. M., Khvostova,, V. P., Bogdanovich, L. I., Sowem. Metody Anal. Mater. 1969,272. (126) Busev, A. I., drysina, L. S., Zholondkovska a, T. N., Pribylova, G. A., Krysin, E. $., Zh. Anal. Khim., 25, 1575 (1970).

(132) Busev, A. I., Solov’eva, N. G., ibid., 26, 751 (1971). (133) Busev, A. I., Teternickov, L. I., Anal. Lett., 4, 53 (1971). (134) Busev, A. I., Zholondkovskaya, T. N., Teplova, G. N., Zh. Anal. Khim., 26, 1133 (1971).

260 (1969) ---

\

1R.?.? --”-.


315 R

Table 111. Constituent Acetone Acetone Alcohols, aliphatic

Photometric Methods for Organic Compounds Material

Acetic acid

...

terl-AlcohOls Alcohoh, or amines Aldehydes Aliphatic amines

... ... ... ...

Amines, alkyl, p

...

Amines, prim. and

...

aryl

MC.

Amines, alkyl,

...

prim and sec. Amines, paryl ... Amines, aromatic, ... aliphatic, alicyclic Amino acids l-A*oanthraTech. pr'dducta quinone ... Aminobenzoic acid ... -p+odiethylandine Aromatic carboxylic ... acids ... Aromatic hydroxy and amino compds Aromatic is+ ... cyanates Barbituric acid .... .. Benzene derivatives Benzethonium Capric acid Carbazole Carbonyl compds Carbonyl cpmpds Carbonyl compds Catechins

Galacturonic acid

Furfural

H y + a z o + m e ; diazotized sulfad c acid Aromatic aldehyde, HtSO4 Tropeolin 00; nitrous acid Guaiacol o-Benzeneaulfonamido)-pbenzoqumone l,%Naphthoquinone; extractn of Naminonaphthoquinone (CHzClz); 2,4diitrohydrazine 2,4Dinitrofluorobenzene,Janovsky reaction 3 5-Dinitrobepzoyl chloride ~ S Z tetrazolium ; blue Chloranil 2,4Dinitrobenzoyl chloride o-Phthalic acid, KBH4 TLC; (MeZCO) Diazotization, 1-naphthol Diazotized sulfanilic acid Basic dyes, e.g. rhodamine 6G 2,4Dinitrodiazobenzene

Carbamate-amine conversion; diazotization Glutaconaldehyde (48) Janovsk reaction (nitration (68) MeN& MelPhCHZN+OH-) ... Tetrabromo henolphthein ethyl (814) eater (c,$cL) Acetic, or formic Acridine orange (4061 acid ... Xant hydro1 (9361 .... .. 2,4Dinitro henylhydrazine (69) 2(Diphenyyacetyl 1,3-indonUione(676) . . . . 1-hydrazone Carbohydrates 2,4Dmitrophenylhydrssine (663) ... p (Dimethy1amino)cinnamaldehyde (794) 1638: -1 X loSl ... &Dimethylaminobenzaldehyde (697)

Cyclohexanol, and cyclohexanane ... 6,fJ-Dichlorooctamide Dicyclohexylamine Na cyclamate Diethylpyrocar... bonate 2,6Dimethoxy... phenol ... Eserine Formaldehyde

YEtrptivity]

[Wavelength; Methodmolara Or o-Nitrobenzaldehyde

Methioi Neutral monosaccharides

Glyoxal

...

2- [ (2-Hydroxy-lnaphthol)azo]-6

...

na hthalenes d o n i c acid ... Hydroquinone ... Itaconic acid ... 2-Methyl-3-aryl4 quinazolonea Mercaptans, organic ... Metol Myristic acid Acetic, 'dr' formic acid Nitron ... Nitrophenols *.. Octylamines ... ZOxoglutaric acid ...

+

+

Hydroxylamine hydrochloride, iron(111) chlorate Brqmophenol blue (CHC4) Induect; Camnoantipyrine

(707)

2,2-Diphenyl-l-picrylhydrazyl

(661

Tetrabromophenolphthein ethyl ester Chromotro ic acid Dichlorosufktomercurate, pararosaniline hydrochloride Carbazole

(817)

3-Methyl-Zbenzothiazolinone h drazone T L ~extractn ;

(818)

(608)

(311)

(719) (8.w

(698)

-

(786)

Diazotized sulfanilic acid Pyridine in A h 0 p(Dimethylamino)benzaldehyde, HClOi Janovsky reaction Diazotized sulfanilic acid Acridine orange

I%{

Methyl orange (Ca4C13) Basic dyes Methyl orange (CHCL) Diazotized sulfamethirole

(63) (408) (799)

(606)

(646) (1041

(40s)

(648)

(Continued)

316R


8 p p (1970): ' (163) Coleman Instruments Div., PerkinElmer Corp., Maywood, Ill. 60153, Bulletin A-336. (164) Cook, E. B. T., Geroghty, A,, Nd. Inst. Met.. Revub. S. A f t . . Rm. . No. 1145, 22 pp'(l971). (165) Costache, D., Popa, G., Rev. Roum. Chim., 15, 1349 (1970). (166) Coyal, S. S., Misra, G. J., Tandon J. P., Bull. Acad. Pol. Sei., Ser. Sei). Chim.. 18, 425 (1970). (167) Croitoru, V., RUSU,V., An. Univ. Bucuresti. Chim., 19.67 (1970). (168) Cyrankowska, .M., Chek. Anal. (Warsaw), 15,209 (1970). (169) Dalziel, J. A. W., Donaldson, J. D., Woodget, B. W . , Talanla, 16, 1477 I

'

(1969).

(17Oi -Danchik, R. 8.,Oliver, R. T., ANAL. CHEM.,42,798 (1970). (171) Danilova, V. N., Lisichenok, s. L., Zh. Anal. Khim. 26, 1157 (1971). (172) Dames, J. E!,. J. Oil Colour C h m . . Ass., 54,281 (i97i).

(173) Dedkov Y. M., Dymova, M. S., Yakovlev, P. Y., ~woci.M., 37, 753 (1971). (174) Dedkov Y. M., Ermakov, A. N., Koraakova k.V., opted.Miktoprimesci, 1,55 (1968j. (175) Dedkov, Y. M. Ermtrkov A. N., Korsakova, N. V.. dh. Anal. Kkim.. 25. 1912 (i97oj. ‘ (176) Dedkov, Y. M Koluzanova, V. P., Kirakoe an, A. K.,kid. p 1482. (177) Y. M., Lvina, G . P., Ibid. 26,558 (1971). (178) beGodeken, M. M., De Zamo’a, M. K., Kauffman, N., Arch. Bwquam. Quim. Farm., 15,69 (1969). (179) Deguchi, M., Okumura, I., Sakai, K.,Buneeki Kagaku 19,836 (1970). (180) Deguchi, M., bakai K., Kagaku Keisatau Kenkpsho Hofcoku, 22, 164 (1969). (181) Ibid., 168. (182) DeguL, M., Tanno, K., Sakai, K., Buneeki Kagaku 19, 1291 (1970). (183) Deguchi, M!., Yamabuki, S., Yas h h M., ibid., 20, 891 (1971). (184) beguch, M., Yamamoto, K.,Sakai, K. Kagaku Keisatau K e n k w h o Hokolk 22, 41 (1969). (185) b e Oliveira Meditach, J., Rev. Quirn. Ind. (Rio de Janeiro), 39, 17 I

.

Photometric Methods for Organic Compounds (Continued) Method or Reagent [Wavelength; molar absorptivity] Materiel pNitroaniline, azulene

Table 111. Constituent Pentaerythritol tetranitrate Phenidone Phenol(s)

...

...

D~L,

(1970).

(l86~-D&hmukhlG. S., Chattopadhyay, S. S. Indian J . Chem., 9, 498 (1971). (187) bivak, A. V., Zavod. Lab., 35, 1443 (1969). (188) Divis L., Sb. V 8 . Sk. ChemTechnol. h e , Anal. Ckem., 1969, 21. (189) Dixon, E. J., Analyst, 95, 272 (1970). (190) Dobrowolski, J., KwiatkowsksSienkiweicz, K., Chem. Anal. (Warsaw), 15, 647 (1970). (191) Dobrowolski, J., Szwabski, S., &id., p 1033. (192) Dolmanova I. F., Zolotova, G. A., N., . Peshkova, V. M., Shekhovtsova, ‘!I? Zh. Anal. Khim., 25,2136 (1970). (193) Domagaliia, E., Zareba, S., Chem. Anal. (Warsaw), 15, 1227 (1970). (194) Dorman, E. L. Jr., Klein R. I., Kreiselman, R. L., boulter, W. k., Ger. Offen. 1,950,376 (Cl. G O h ) , 16 Apr 1970 US Appl 10 Oct 1968; 39 p . (195) bouglas, L. A., Bremmer, M., Anal. Lett. 3,79 (1970). (196) Dragdescu, C., Simioneacu, T., ScW, H., Rev. Roum. Chim., 14, 583 (1969). (197) Drozdova, S. N., Monsenko, A. P., Yampol’skii, M. Z., Zh. Anal. Khim., 26,291 (1971). (198) Duce, F. A., Yamamura, S. S., Talunta. 17. 143 11970). (199) Duk< g.-K., Seahadri, T., Anal. Chim. Acta, 47, 571 (1969). (200) D’ymchenko, S. S., Agrinskaya, N. A., Petrashen, V. I., Zavod. m.,36, 23 (1970). (201) D‘ziomko, V. M., Ostrovska a, V. M., Kon’kova, 0. V., Zh. Anal. &him., 25,267 (1970). (202) Edrissi, M., Mwoumi, A., M h o chem.J., 16,177 (1971). (203) Edrisai, M., Massoumi, A., Dalziel, J. A. W., ibid., 15, 579 (1970). (204) Einaga, H., Ishii, H., Buneeki Kagaku, 18, 1211 (1969). (205) Elinson, S. V., Sovrem. M&dy Anal. Mater., 1969, 3. (206) Elinson, S. V., Pobedina, L. I., Rezova, A. T., Zavod. Lab., 37, 521

.f

\--

.--.

11971). -,-

- I .

(207) Elinson, S. V., Pyatiletova, N. M., Novikova, I. S., ibid., 36,659 (1970). (208) Elinson, S. V., Tsvetkova, V. T., abid.. 37. 662 (1971). . (209) Emka, S., Buheki Kagaku, 19,637 (1970).

... ... Water 3-Phenylimidazcr lidinone Phthalic acid Phthalic acid esters Polycyclic aromatics Pyridoxal Pyrogallol Pyrrole Salicyclic acid p-Sitosterol Sparteine

... ... ..

Organic &vents Soot

... ... ...

...

... ...

Succinate Sugars Sulfhydryl group

... *..

Tet~aethylammomum Thiourea ... Trichlorotoluene... sulfonic acid Tri- and tetranitrcr 3,3’-Dinitrophenylsulfone diphenylsulfonas Urea

Diazotized sulfanilic acid CAminoantipyrine, ferricyanide K&Oa - - CAminoantipyrine, ferricyanide (CHClr) Diazo coupling Janovsky reaction 2,&Dibromoquinone chlorimide Oxidn coupling 3-methyl-Zbenzothiazolinone hydrazone; automstion p-Dimethylaminocinnamaldehyde Turbidimetric; lead(I1) phthalate Phthalic anh dride, phenol N-Hydr oxypgt halimide Extrctn (PhCl); “absorbance No.” ZHydrazinobenzoic acid HCl, or phenylhydrazine HCl 2,ZDiphenyl-1-picrylhydrazyl p-Dimethylaminobenzaldehyde Crystal vlolet (PhCl) Benzoylperoxide Sparteine-bromophenolphthalein ethyl ether Succinate dehydrogenase,’phenazine methyl sulfate, cytochrome C 3-Methyl-1,2-benzothiazolinone; iron(II1) chloride (BuOH) p-Dimethylaminophenyl mercury acetate Tetrabromo henolphthalein ethyl ester (Cd”p1~) 3-Chloro- 1,Pnapht hoquinone Acridine orange (COHO) Ammonium hydroxide Diacetyl monoxime, thiosemicarbazide

(210) Enoki, T., Mori, I., Izumi, Y., ibid., 18,963 (1969). (211) Eremin, Y. G., Katochkina, V. S., Zh. Anal. Khim., 25, 68 (1970). (212) Erskine, J. W., Williams, A. F., Talanta, 17, 244 (1970). (213) Ewen M., Cook,E. B. T., Nat. Inst. Met., Repub. S . Afr., Rep. N o . 1179, 2 PP (1971). (214) Fedorova, N. D., Fokina, C. S., TT. Vsea. Nauch.-Isaled. Inst. Stand. Obraztaov. Spektral. Etalonov, 5, 49 (1969). (215) Fhorova, T. I., Shvedova, L. V., Yataimirskii, K. B., Zh. Anal. Khim., 25,307 (1970). (216) Fickentmher, K., Praep. Pharm., 6, 159 (1970). (217) Fikar; L., Huebnerova, J., Sb. PT. Vyzk. Chem. Vyuzit. Uhli, Debtu Ropy. 1969,227. (218) Filimonova, G. P., Khrebotova, V. M. Tr. Vsa. Nauch.-Isskd. Ivst. Zolota Re&. Metal. 29 131 (1969). (219) Filipov b.,’Nachev, I., Dokl. Bolg. Akad. ?auk, 22, 687 (1969). (220) Filippov, M. P., Zh. Anal. Khim., 25,2459 (1970). (221) Flscher, R., Z . Anal..Chem., 249,110 (1970). (222) Flaschka, H., Weiss, R. H., Microchem. J . , 15,635 (1970). (223) Florence, T. M., A u t . At. E w g y Comm., AAECITM [Rep.], A AEC/ TM-552,11, 1 (1970). (224) Fogg, A. G., Jarvis, T. J., Marriott, D. R., Burns, D. T., Analyst, 96, 475 (1971 ,- - .- ). ,. (225) Fogg, A. G., J i l l l J., Marriott, D. R., Burns, D.T., .,94,768 (1969).

(226) Fogg, A. G., Marriott, D. R., Burns, D. T., ibid.. 95,848 (1970). . , (227) Ibid., p854. (228) Fomina, A. I., Agrinskaya N. A., Petrashen, V. I., Tr. Novocbkassk. Politekh. Inst. 220, 113 (1969). (229) Fowler, 8. W., Parsons, W. H., Russell, G. B. Steele, T. W., Nat. Inst. Met., Repub. s‘. Afr., R d . Rep., No. 323, 17 p . (1967). (230) rei, R. W., Navratil, O., Anal. Chim. Acta, 52, 221 (1970). (231) Friestad, H. O., Ott, D. E., Gunther, F. A., ANAL. &EM., 41. 1750 (2: 1--

--,-

(233)Fujinuma, H., Shimada, Y., Hirano, S., Bunseki Kagaku, 20, 131 (1971). (234) Fujinuma, H., Yoshida, I., ibid., 19, 1273 (1970). (235) Fukamachi, K., Kohara, H., Ishibashi, N., ibid., p 1529. (236) Furusawa, M:,.Sato, Y., Yamada, S.. Takeuchi. T.. zbad.. D 573. (237) Furuya, K.,‘Fujim&a, K., Tsurumi, C.. Ibid.. 20.535 (1971). (238j Futekkov, L., Atan&ova, B., Natura (Plovdiv), 3, 65 (1970). (239) Ganago L. I., Kovaleva, L. V., Zh. Anal. dhim. 25, 1517 (1970). (240) Ganago, L. I., Prostak, I. A., ibid., 26,104 (1971). (241) Garcia, M. F., Herrera, C., Arias, J. J., Inform. Quim. Anal.. 25.26 (1971). (242) Gaig, B. S., Sigh, R. P., Taluntd., 18,761 (1971). (243) Garrido Fernandez, A,, Gasch


317R

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