Khim., 28, 1011 (1973). (223) Rohm. Timothy, J.. Nipper, Henry C., Purdy, William C.. Anal. Chem., 44, 869 (1 972). (224) Rozhkov, I, N., Bukhtiarov, A . V.,
(241) Stepanenko, V. E., Krichmar, S. I., Zavod. Lab., 38,1200 (1972). (242) Stock, J. T., J. Chem. Educ., 50, 268 (1973). (243) Stocker, J. H., Jenevein. R. M., J. Chem. Gal’pern, E. G., Knunyants, i. L., Dokl. SOC. D., 1478 (1971). Akad. Nauk SSSR, 199,369 (1971). (244) Stojkovic, Darinka J., Glas. Hem. Drus., Boegrad, 35,443 (1970). (225) Schmulbach, C. D.. Oommen. T. V., Anal. Chem., 45,820 (1973). (245) lbid., p 497. (226) Schwing, Jean P., Fr. Demande 2,060,166 (246) lbid., p 487. (Sept. 5, 1969). (247) Stojkovic, Darinka J., Dravic, Svetlana R., ibid., p 437. (227) Sement, E., Rousselet, F., Girard, M. L., Chemla. M., Ann. Pharm. F r . , 30, 691 (248) Sturua, R. I., Shaveev, Sh. R., Chanturiya, 11 ~ 973) ._._,. V. A,, Vop. Teor. Prakt. Obogashch Rud., (228) Sement. E., Rousselet, F. Girard, M. L., 1971,69. Chemla. M.. Bull. SOC. Chim. Fr., 1972, (249) Suffet, I . H., Radziul, J. V . , Goff, D. R, 835. Water Quality Instrum., 1, 1 1 (1972). (250) Suzuki, M., Swaada, S., Denkl Kagaku. (229) Sherlock, J. C., J. Phys. E, 6,518 (1973). (230) Shimizu, Hiroshi, Brit. Patent, 1,318,730 39,249 (1971). (Nov. 13,1969). (251) Svanhalm, U., Parker, V., Tetrahedron Lett., 471 (1972). (231) Shono, T., J. Syn. Org. Chem., 29, 865 (1971), (252)Sympson, R. F., Anal. Chim. Acta, 61, 148 (1972). (232) Shorygin, A. P.. Kazaryan. E. V., Elektrokhiniya, 9, 1223 (1973). (253) Szopory, Bela, Nehezip. Musz. Egyet., Miskolc, Kozlem., 16,213 (1970). (233) Shpak, I . E., Dmitriev, Yu, S., Blank, M. (254)Tackett. Stanford L., Chem. Techno/, 2, S., Tr. Molodykh-Uch. Saratov. Univ. Vyp. 734 (1972). Khim., 2,90 (1973). (255)Tackett, S. L., J. Chem. Educ., 49, 52 (234) Sioda, R. E., Kambara, T., Sci.. Hokkaido (1972). Univ., J. Electroanal, Chem. lnterfacial Electrochem., 38,51 (1972). (256)Taitiro, Fujinaga, Talanta, 19,657 (1972). (257)Takata, Yoshinori, Muto, Giichi, Anal. (235) Sistig, Eberhard, Reinermann, Karl Heinz, Chem., 45,1964 (1973). Ger. Offen. 2,103,089(Jan. 23,1971). (258) Takahashi, Takehiko, Nomura, Eiichi, (236)Skyarenko. I . S.,Mikhailov, V. M., ChubuYamamoto, Osamu, Denki Kagaku, 40, kova, T. M., Zh. Anal. Khim., 27, 1991 595 (1972). (1972). (259) Tasaka, Akimasa, Watanabe. Nobuatsu. (237) Sklyarenko, I . S..Senturin, I. G.. ChubuZ. Anorg. Allg. Chem., 385,156 (1971). kova, T. M , , ibid., 28, 131 8 (1 973). (260) Tenygl, J., Fleet B., Collect. Czech. Chem. (238) Sobkowska, A,, Radiochem. Radioanal. Commun., 38,1714 (1973). Lett., 8,357 (1971). (261)Thomich, Wolfgang, Arch. Eisenhuettenw, (239) Soucek. Jaroslav. Slavicek, Ivan, Czech. 43,239 (1972). Patent 138,147(Sept. 15, 1970). (240) Stenina, N. I., Agasyan, P. K., Nikolaeva, (262)Thomsen. Agnete D., Lund, Henning, Acta Chem. Scand., 25,1576 (1971). E. P., Chernykh. L. N., Venyarskaya, I . (263)Trenkler, George, U.S. Patent 3,613,002 N.. Tr. Urai. Nauch-lssled. Khim. lnst., (Oct. 12,1971). No. 26,37 (1971).
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~
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~
,
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(1972).
Ion Selective Electrodes, Potentiometry, and Potentiometric Titrations Richaid P. Buck William Rand Kenan J r . Laboratories of Chemistry, University of North Carolina at Chapel Hill, Chapel Hill, N.C. 27574
The literature compiled for this review includes developments in the general areas of fundamental and applied potentiometry published since the last review (168). The final issue of Chemical Abstracts consulted was Vol. 79, No. 23, December 10, 1973. Again I have emphasized ion selective electrodes and their applications in all fields of applied science. To achieve a review of practical length, nonaqueous titrimetry, potentiometry in molten salts, electrodes and systems pertaining primarily to batteries, fuel cells, and electrochemical synthesis have been omitted. Nearly 300 references to complex ion equilibria and acid-base equilibria, followed potentiometrically, have been deleted. More tables and less discussion characterize this review over those in the past because the literature in the field continues to increase. Ion selective electrodes in particular find applications in biology, medicine, natural water, and air chemistry and even solid state physics. Conversely, fundamental literature in these diverse fields has an impact on the development of improved electrodes. Important fundamental papers are included where they are immediately pertinent.
BOOKS, REVIEWS, AND SURVEYS Only two books have appeared (183, 795) which are exclusively concerned with ion selective electrodes (ISE’s). However, others are in preparation. Geddes’ book on elec28R
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trodes (346) is aimed a t applications in biophysics while edited volumes by Eisenman (290), the Specialist Reports of the Chemical Society (201), and Vijh’s volume on semiconductor electrochemistry (1207) provide important background reviews on materials and transport properties as well as potentiometric results on systems closely related to ISE’s. A further supplement of “Stability Constants of Metal-Ion Complexes” has been issued (1068) and a new volume on interfacial electrochemistry which bridges the gap between electrodics and colloid science has appeared (879). A full review of the theory and application of ISE’s including literature through the end of 1971 is by Koryta (588). Other reviews of general nature in English, except as noted, are by Baumung, Ger. (99), Clerc and Pretsch, Ger. (212), Clerc, Kahr, Pretsch, Scholer and Wuhrmann, Ger. (213), Fiori and Formaro, Ital. (316), Hozumi, J a p . (464), Hulanicki, Pol (467), Ijsseling, Neth. (475), Oehme, Ger. (866), Omang, Norweg. (874), Pretsch, Scholer, Kahr, and Wuhrmann, Ger. (935), Sapio and Braun (1014), and Wilson (1244). Reviews emphasizing heterogeneous membranes of the Pungor type are by Pungor and/ or Toth (940) Serb. (943, 945, 948, 949, 1162, 1164). The latter four emphasize selectivities, mechanisms, and time responses. Klara Toth has also described potentiometric research in Hungary (1163). The Matrafured (Hungary) Conference on ISE’s produced a number of important pa-
Richard P. Buck received his BS and MS degrees in chemistry from the California Institute of Technology in 1950 and 1951, respectively, and his PhD in chemistry from the Massachusetts Institute of Technology in 1954. Since then he has been assistant research chemist, California Research Corp., 1954-57; research chemist, California Research Corp., 1957-61; principal research chemist, Bell 8 Howell Research Center, 1961-65; senior scientist, Beckman Instruments, 1965-67: associate professor of Chemistry, University of North Carolina and assistant director of Crystal Growth and Analysis Laboratory, 1967 to the present. His work includes many facets of electrochemistry. Among these are theory and practice of electrode process identification and measurement, coulometric methods for batch and continuous analysis, and construction of ion-selective electrodes and crystal membrane interface and transport studies. He is also currently working in spark source mass spectrometry and atomic absorption spectrometry for trace analysis of nearly pure solid materials. H a is the author of several articles on electrochemistry and fuel cells in technical publications. He is a senior member of the American Chemical Society and was a National Science Foundation Fellow in 1952-53 and a Du Pont Fellow, 1953-54. He was cochairman of the 1964 Gordon Research Conference on Electrochemistry and Chairman of the 1965 Conference.
pers on selectivity and sensitivity of ISE’s (798), heterogeneous polythene electrodes (661), and the relation of membrane and conventional electrodes of 1st and 2nd kinds (782). Proceedings of the IUPAC-sponsored conference on ISE’s a t Cardiff, Wales, in April 1973 have not yet appeared. A new extensive review of principles and applications is by Tenygl (1140). The Czech single crystal (CRYTUR) electrodes are reviewed by Manek (728) and other new electrodes are disclosed by Gavach (341) and Luftig (702). Application reviews are by Warner (1223), and Conti and Wilde (225) in sea water: Weber (1226, 1227), Sakai, J a p . (1012)‘ and Manahan (726) water pollution; Maienthal (719), McClelland and Mancy (764), Suffet, Radziul, and Goff (1114) and Yasuda, Jap. (1256), water quality; Liberti and Mascini (660) air pollution. Continuous monitoring is reviewed by Riseman (977, 978), Cornish and Simpson (229),Fleet and Ho (320),and Kaludjercic, Croat. (533). Use of ISE’s in specific fields are: latex products, Provorov et al., Russ. (937); metal finishing, Simpson (1074); flotation pulp, Abramov et al., Russ. ( 4 ) , ferrous metallurgy, Henriet, Fr. (434), chromatography detector, Polesuk (922)and plating baths, Tobias (1151). Biological and biochemical application reviews are: Protein-protein and protein-ion interactions, Carr (187) and Laskowski and Finkenstadt (647); protein titrations, Beukers, Neth. (124);ultramicro-analysis, Alimarin et al., Russ. ( 2 6 ) ; pharmaceuticals and pesticides, Kuettel, Hung. (618); redox potentials, Jacob, Ger. (500), Havas and Kiszel(423), Suzuki, Jap. (1120). Reviews of new zero current potentiometric titration developments are by Ijsseling, Neth. (473), Kraft, Ger. (594) and Songina, Russ. (1092). Constant current potentiometry has been reviewed by Ijsseling, Neth. (474), Stock (1104)and Rosset, Fr. (987). Glass membrane electrodes are reviewed by Bulawa and Dolbniak-Leonowicz, Pol, (17 4 , while p H measurement is the topic of two books (673, 789). pH measurement reviews include the systems: drinking water, Fiker and Santora, Czech. (315);soil extracts, Aleksandrova and Gubareva, Ukrain. (24); watery process media, Jungck and Woytowicz (527), microbiological systems, Munro (811); nonaqueous, Mun, Korean (810). Interferences for solid membrane electrodes are tabulated by Sasaki, J a p . (1016); sensitivity limits are stressed by Parthasarathy et al. (891);temperature coefficients are given for ISE’s and reference electrodes by Negus and Light (835); and some lab exercises are presented by Lamb et al. (641).Selectivity coefficients or ratios are discussed critically by Moody et al. (796, 797). Dynamic responses of five ISE’s determined by a pulse method are reported by Markovic and Osborn (733). Fundamental reviews on membrane phenomena by
Lakshminarayanaiah (6.39). and Ti Tien (1149), general theory for membrane electrode potentials (1254), and properties of thick neutral carrier membranes (657) are recommended. Other significant surveys cover standard electrode potentials by Covington (234) and Bates (80), determination of ionization constants by potentiometry (703), and various types and applications of oxygen-sensing electrodes (103). Other specific papers on these topics occur throughout this review. T E C H N I Q U E S F O R I M P R O V E D DATA ACQUISITION, HANDLING, AND REPORTING A group of papers describe the known-increment (standard addition) and known decrement techniques with graphical, including Gran’s, data handling methods (74, 309, 318, 400, 542, 756). Matsushita has also described ISE’s used in null-point potentiometry (757) and in differential potentiometry (758). The theory of Gran plots for minimizing titration errors is given by Buffle, Parthasarathy, and Monnier (172, 173, 890); for chelatometry by Johansson (518) and Carr (188); for acid-base titrimetry (763), redox titrimetry (1170), precipitation titrations (1272),end point determinations in general (1047) and F determinations (1045). Anomalous redox titration curves have been interpreted on the basis of free radical adsorption (933).Free radical participation in membrane potentials has already been suggested by Piruzyan et al. (919). The area method of end-point determination has been applied and defended by Cormos and Marusciac (227, 228). Three papers by Anfelt and Jagner report digital computer applications to end-point determinations (34, 416) and semiautomatic titrator data processing (35). Four papers by Ebel describe the evaluation of titration data by digital computer using the Gran principle (283-286). Continuous monitoring using a computerized Gran plot method was reported by Fleet and Ho (321). Fully computer-operated titration apparatus was described by Gobom and Kovacs (358). Computer data handling procedure without Gran linearization using nonlinear regression was given by Waldmeier and Rellstab (1219). Computer programs for graphical treatment of potentiometric data are GRAPE (520) for complex equilibria, another for Gran plots (708) and WATEQ for distributions of species in natural waters ( 1 1 71). Other procedures reported include determining stability constants from pH-metric data (824), and pM data (125, 431, 514), experimental design in titrimetry ( l o % ) , statistics of titration curves, most probable titer (239), and automatic control of pH-involved processes (960). Computer calculations of pH in mixtures by iterative methods are described by Machado (710-713), while determination of isopoly-complex equilibria from pHmetric titration curves are discussed in a continuing series (186). Vasil’ev and Vasil’eva give formulas for reducing formal stability constants and electrode potentials to thermodynamic values (1195). Bykova and Petrov (182) review the entire field of nonaqueous acid-base equilibria and titrimetry, including scales of solvent acidity, selection of solvents and shapes of titration curves. Theoretical potentiometric titration curves for acids and bases in nonaqueous solvents are given by Kreshkov et al. (605, 606). Bronsted acidity (584), neutral salts (1025), ionic strength (1271) and leveling effects (577) are discussed in relation to potentiometric titrimetry. Methods are described for extracting instability constants of intermetallic compounds in mercury from potentiometric data (621, 1107, 2108). A patent (479) claims an assay of redox enzyme activities (hydrogenase) based on a potentiometric cell. Potentiometric titrations of polyelectrolytes continue to provide information about conformational changes and electrostatic charge effects on dissociation constants. A series of papers emphasize proteins, particularly pepsinogen (goo), polymethacrylic acid (14,823), carboxymethyl cellulose (976), poly-L-tyrosine (1049), poly-(S-carboxyethyl)-L-cysteine (716), polyacrylic acid (793), poly(L-histidine) (1143), poly(acry1ohydroxamic acid) (1153j, polyuronic acids (570) and some copolymers containing COzH, OH, and NH2 (196). Four articles give theoretical interpretations of polyelectrolyte titration curves (717, 731, 769, 1115). Effects of surface-active agents on polycarboxA N A L Y T I C A L C H E M I S T R Y , VOL. 46, N O .
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Table I. Properties and Applications of Fluoride-Selective Electrodes Topic
Review of mechanisms and applications Studies of varying solubilities of LaF3 in relation to applications Response mechanism studied by ‘*F transport Similarities between glass and LaF, membranes Nonspecific response of LaF3 membrane electrodes Micro determination of F - using Gran plots Studies of potentiometric titrations of F Measurement of F - in dental pastes in enamel in glass in Cr plating baths in wood preservatives in sugar cane in drinking water in natural waters in clays in aluminum processing in welding fluxes and coating in phosphate processing in silicate rocks in pickling baths in Pu-containing oxides in H F production in urine
Reference(8)
(484) 1307) 11095) (1204) (1268) (1046) (209, 300, 429, 1137)
i738) (646) (79, 862) (324) (635) (697) 1110, 167) (1222) (1251) (883, 1118, 1150) 1139) 1277, 413, 613) 1505) 1299, 301) (720) (614) (221, 377, 1177)
ylic acid titration curves are presented by Tamaki et al. (1132). Four papers describe potentiometric methods applied to surfactant systems (129, 563, 727, 1152).
SOLID STATE MEMBRANE, NON-GLASS ELECTRODES AND APPLICATIONS Fundamental papers which describe preparation, responses, selectivities, and applications of non-glass solid state membrane electrodes continue to appear. It is now clear that supported membranes, so-called heterogeneous membranes, containing the same salts as used in single crystal or pressed pellet membranes, are sufficiently similar in their responses that they can be included in the groupings based on ion-exchanging material. Placing fundamental studies first in each section, compilations of fluoride-selective electrodes are reported in Table I while the other solid state electrodes are listed in Table 11. Among the several papers which describe preparation, the extensive study by Mascini and Liberti (743) of the mode of formation of CdS prior to inclusion in an electrode is illustrative of the precautions needed to obtain Nernstian response. Storage of electrodes in reducing media is stressed in (914).Preparation of electrode surfaces is thoroughly investigated by Johansson and Edstrom (519). Many electrodes in this tabulation use “all solid state” co,nfiguration in which a conductor is attached to the inner reference side of the membrane to remove need for an inner reference filling solution. The EO values for these electrodes are sensitive to stoichiometry of the crystals and become equal to EO for the equivalent M / M + electrode only when the crystal contains excess free metal. “All solid state” electrodes and the equivalent membrane between two solutions, “membrane configuration,” yield 30R
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Reference(8)
Topic
in biological
samples in plants and vegetation in organics containing B and P in organics in household products in wine Determination of activities in multicomponent systems Determination of dissociation constant of H F (student experiment) Determination of formation constants of U(VI), V(1V)-F - complexes Determination of formation constants of N b N ) - F - complexes Determination of formation constants 1st row divalent transition metal ion-F - complexes Determination of formation constants Al(II1)-F - complexes Indirect determination of Si, Al, Fe, Ca, and Mg A continuous monitor for F Use with furnace as gas chromato. graph detector Use as a membrane for reference electrode in F - melts An electrode for sensing Ca2 and M g 2 +using CaF? and/or MgF, with LaFl An improved LaF3-EuF, membrane electrode Properties of LaOF as a solid electrolyte +
(408, 581) 165, 466, 502, 503, 1146) (982) 1433) 11026) (252, 804) 1659) 1236) 112) (643)
(496) (571) (164)
1321) (66) (897)
different potentials at unit activity of metal ion. The behavior is now well understood on thermodynamic grounds as described in the last section of this review. The “all solid state” electrode responses are independent of the electrode lead wire, provided that the membrane contains excess metal and the circuit is completed through a common metal such as copper used at the measuring device for both the ion sensing and reference electrodes. Particularly interesting examples are the Selectrodes based on graphite. At least four papers describe these electrodes and atmlications (412, 642, 1003, 1004). Finally, new supported ion exchangers for Cs+ and T1’ are included with further examples of electrodes based on virtually nonconducting salts, BaCr04, BaS04, and ferrocyanides. Two solid state sulfate selective electrodes based on Ag2SPbS-PbS04-Cu2S (792, 968) and on PbIz (422) were characterized and demonstrated.
HOMOGENEOUS ION EXCHANGE MEMBRANES These membranes as potentiometric sensors predate the modern ion selective electrodes and still have many uses despite their lack of specificity. Two papers describe responses and applications in measuring surfactant activities in dilute solutions (1043, j060). A type of membrane with fixed sites inside, but not on the surfaces were prepared and tested electrochemically (515, 516). Five papers described acid or monovalent ion responses (6, 302, 830, 1059, I I O O ) , divalent ion responses (146, 203, 204) and anion responses (7, 108). A polyquinhydrone-HCOH membrane, stable over a wide pH range, was patented for pH measurement (1042),and nylon membranes have been reported sensitive to C1- (384). Ion exchange cellulose paper has been used for potential measurements (966).
Table 11. P r o p e r t i e s and Applications of Solid-state M e m b r a n e Electrodes Part A. Primarily Silver Halide Membranes Reference ( 8 ) Topic
zomparison of responses of :ommercially available (CRYTUR) tlectrodes with heterogeneous memwanes and 2nd kind electrodes Zomparison and selectivity of single :rystal and heterogeneous membrane dectrodes 4ctivity measurements in high ionic itrength aq. solutions Applications in microanalysis of volatile organics 1C1.- and Br-) Applications t o monitoring of reaction kinetics Potentiom. titration of N a pentacyanonitrosyl ferrate Use of C1- electrode to study Cd(I1) and Zn!11) chloro complexes Determination of C1- in sweat Continuous monitoring of C1- in natural water Determination of C1- in soils and soil extracts Determination of C1- in sea water Determination of C1- in silicate rocks Determination of C1- in milk Determination of C1- in sugar industry Monitoring of C1- in refinery control Determination of C1- in pulping liquors Determination of C1- in acetonitrile Determination of C1- in brewing water Estimation of Br - in plasma Determination of SCN - with AgBr membrane electrode Determination of Br-- in soft drinks Following R r - in oscillating chemical reactions Influence of pH on response of a C N sensing electrode Diffusion barrier model for the C N sensing electrode New model for the response of C N a t an I - sensing electrode Response of the I - selective electrode Response of the I - selective electrode in concentrated aq. electrolytes Potentiometric measurements in nonaq. media with Br - and I - selective electrodes Use of I - electrode to detect Au(II1) Use of I - electrode to determine Bi(II1) Determination of S O . , - with I - selective electrode Determination of rhodanase with C N selective electrode Cyanide determination after distillation Cyanide determination in presence of chelating agents Cyanide determination in mineral waters Cyanide determination in solutions Apparatus for free and combined C N Determination of CN - in cigarette smoke Determination of CN - using standard addition Potentiometric titration of C N - and c1Determination of CN - in waste waters
(78)
Topic
Referencc(s)
(42) Determination of CN - in flowing
1319)
systems ( 4 3 ) Determination of azide with an AMEL
1152)
(Italian) sel. electrode (1021)
(1121) (827) (355, 612, 1048) (868) (428) (432) (735) (925) 1888)
(653) (1166)
1255) (580)
( I 176) (585) (742) (305) (153) 1265) (801) (314)
Part B. Primarily Silver Sulfide and Mixed Sulfide, Selenide, Telluride Membranes Topic Reference@)
Responses of a series of AgSSmembranes showing varying Eovalues with methods of preparation Comparison of three methods of sulfide titration using ISE end-point detection Determination of silver in ZnS, ZnSe, CdS, CdSe Determination of silver in fixing baths Use of S 2 - sensing membrane to study o-acetylserine sulfhydrylase Micro and semimicro determination of thiols Determination of thiourea and p-urazine Potentiometric titration of trace sulfur in petroleum Potentiometric titration of thiols (comparison of ISE with 2nd kind electrode) S 2 - determination in solids S 2 - determination in slurrys S 2 - determination in organics AgSS ceramic electrodes-responses Ag2S ceramic electrodes-redox behavior Ag2S ceramic electrodes-statistical study of Ag response Ag2S ceramic electrodes-influence of preparation conditions on Ag + response Ag,S ceramic electrodes-as chromatographic detectors Field of existence of Ag2S(II) Ag- sens. electrode made from AgZSe, Ag,Te C d 2+,Zn2+,Cut +,P b 2+-sens. electrodes from 25 mole % metal telluride with 7 5 mole % Ag2S Responses of PbSe, PbTe-AgSS electrodes M n 2 Co2+,Ni2 and (Cr3+) sens. electrodes from 25 mole % metal telluride with 7 5 mole % Ag2S Cr3 is detected with Ni2 electrode Response of a Cd2'-selec. ceramic electrode Response of a P b 2+-selec. ceramic electrode Responses of a natural Cups electrode to s2Responses of a synthetic CUSSelectrode t o Cu2 Use of a synthetic C U ~ electrode S to study Cu(1) complexes in acetonitrile Preparation and responses of CUI electrodes CRYTUR-single crystal electrodes, selectivities and other properties Applications of CRYTUR electrodes Properties of the -Cui ,Se CRYTUR electrode Behavior of PbS, PbSe, PbTe-based +
(477) 1470) (899) 1437, 577) (1232) (382) (701) (1205) (325) (223) (979)
1476, 849)
(480) (1213) 1841) 11044) (617 ) (628) (902) 127) 13) (1084) 1680, 690) 1927) (684)
+
+
(1231) (174)
(1203)
1928) 1689) (145) (445) 1444, 446448) (451) 1441, 442) 1443, 449) '452) (450) (147) ! 1022)
+
(430) 1856)
15) (1112) 11201) 1721)
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
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T a b l e 11. ( C o n t i n u e d ) Part B. Primarily Silver Sulfide and Mixed Sulfide, Selenide, Telluride Membranes Topic Reference(s>
electrodes in buffered P b 2 solutions Metal selenides, tellurides, and sulfides (1202) as materials for ISE’s Microelectrodes based on materials (243, 426) used in membrane ISE’s Responses of mixed sulfide electrodes (33) for Cu2+, C d 2 + ,Pb2+, Hg2+, Nil+, Co2+,or Zn2+ Behavior of CuS-Ag2S electrodes (519) Cu2 determination in water by (1088) standard addition Effect of C u 2 +on algal growth (1087) Optimization of composition of (363) PbS-Ag2S and CdS-Ag2S electrodes Potentiometric titration of SOa2-, (420) Ba2 and Sr2 using PbZ+ sel. electrode Potentiometric titration of sod2-in (744) mineral and sea water with P b 2 sel. electrode‘ Flow-through electrodes based on (1147) Cu2+, Cd2+,and P b 2 sens. compositions Durable, two-layer construction for (83) ISE’s Potentiometric titrations using Cu2 (880) and P b 2 +sel. electrodes +
(34) (35) 136) (37) 138) (39) (40) 141)
+
+
(42)
+
(43)
+
(44) (45)
+
Part C. Supported Solid-state (Heterogeneous) Membranes Topic Reference( 8 )
(1) Responses and calibration of silicone (2) (3) (4) (5)
(6) (7) (8) (9) (10) (11)
rubber electrodes for low ionic activities Dynamic responses of precipitate based ISE’s Temperature coe5cients of ISE’s in non-isothermal cells Applicability of silicone-based electrodes in nonaq. solvents Factors in constructing stable heterogeneous electrodes Selectivity coefficients of sulfide-sens. electrodes Studies on thioacetimide with S 2 - ISE Dete-ination of p-urazine with S2ISE Applications of ISE’s in organic analysis Determination of S2-and S22- with S 2 - ISE Potentiometric determination of tetraphenyl borate with Ag using halide ISE Potentiometric determination of anions in presence of interferences with C1-sensitive ISE
(63, 64) (1160, 1161, I 165) (672) (553) (249, 947) (1029, 1030)
(1080)
+
(12)
Part C. Supported Solid-state (Heterogeneous) Membranes Topic Reference(s)
(13) Applications of Br--sensitive ISE in
organic manufacturing (14) Determination of alkaloid halides using halide-sensitive ISE’s (15) Determination of C1- in pesticides (16) Application of anion-sens. membranes in pharmaceutical quality control (17) Potential of and salt diffusion in parchment-supported AgI membranes (18) Mercurimetric determination of halides and pseudohalides (19) A polythene-supported Ag2S-CdS electrode (20) A silicone-supported Ag2S-CdS electrode (21) A silicone-based Cu(I1) sens. electrode (22) A collodion-para5n membrane selective to Cu2 and Ni2 (23) A silicone based, CUZ-.S, Cu2+-sense electrode (24) Applications of the previous electrode (25) A polythene-based P b 2+-sens. electrode (26) A silicone based Cs-12 molybdophosphate Cs +-sens. electrode (27) Potentiometric determination of Cs + using former electrode (28) An epoxy-based Cs +-sens. electrode (29) An epoxy-based T1++ens. electrode using Tl(1) molybdo- or tungstophosphate (30) Chromate-responsive membrane electrode using silicone rubber supported BaCrOl (31) Parchment-supported BaS04 membrane which is primarily pH responsive (32) Patented-sulfate selective electrode based on Bas04 in silicone rubber (33) Conditioning and conditions for selectivity of BaSOa-cellophane membranes (34) Potentials across Co2Fe(CN),supported membranes; properties of Mn, Co, Ag, Cd, ferrocyanide membranes (35) C1 --sensitive electrode using hydrous zirconium oxide in silicone rubber (36) Potentiometric and voltammetric applications of silicone rubber-based graphite electrodes to acid-base titrations and drug analyses (37) Electrode sensitive to potassium using potassium tetra-p-chlorophenylborate or potassium tetraphenyl borate in PVC +
(398, 399) (531) (1182) (532, 598) (104, 105)
( I 082) (743)
+
(406, 704) (675, 679, 687, 692) (1019) (454) (885, 1065)
(1138) (941, 942, 944, 1124) (251, 1109)
T a b l e 111. Applications of Glass Electrodes Part A. Mainly pH Measurements Topic
(1) Intramucosal gastric acid measurement (2) (3) (4) (5)
32R
Reference(s)
(1245)
(microelectrodes) I n vivo pH and pNa in the myocardium (1194) imicroelectrodes) pH electrode for nanoliter samples (546) (micrQelectrodes) Direct intracellular pH measurement (882) (microelectrodes) Analyses of parameters affecting glass ( I 179) microelectrodes 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
Part A. Mainly pH Measurements Topic
(6) Capillary glass electrode for small blood volumes (7) Electrical resistance of glass capillary electrodes (8) Continuous monitoring of pH in blood of heart coronary sinus (9) Apparatus for pH determination of gastric contents (10) Telemetric measurement of gastric acid (11) Measurement of gastric juice acidity
Reference@)
(111) (1133) (344, 768) (116) (549) (730)
Table 111. (Continued) Part A. Mainly pH Measurements Topic
Design and use of micro pH electrodes for measurements in the near-electrode region during electrolysis Measurement of alkaline reserve in crustaceans Measurement of soil pH Study of the acidity region of molten KHSOi Determination of acidity of aluminosilicate catalysts Alkali determinations in the aluminum industry Compact electrode system for environmental use Patents on pH electrode (and system) designs (see also a later section for related patents) pH glass composition patent Seals for pH glass electrodes pH meter for concentration readout Instrument for direct measurement of glass electrode resistance Table of pH and nanoequivalents for pH 7-8 Methods for establishing and measuring the isoelectric potential iL.e., a constant potential value a t all temperatures for glass electrodes us. Ag AgCl ref.)
Reference(s)
1348-351, 615, 1193) (260) (1023, 1069) (1208) 1596) (630, 1156, 1185) (1236) (273, 312, 638. 761. 1008, 1134) (754) 1388, 390) 1762) (601) 1633) 1562)
Part B. Mainly p N a L and p K + Measurements Topic Reference(s)
Following axa in active transport in multicellular membranes Potentiometric determination of N a in whole blood
(820) +
(736)
The revival of interest in alkaline-earth metal soap films has produced three papers on membranes responsive to mono and divalent cations (151, 381, 459). Selectivities were calculated (151). Grigorov thinks selectivity occurs through microcrack transport. This argument has been advanced before, for other electrodes including heterogeneous electrodes and open tip electrodes. Cation (338) and anion (339) selective electrodes made from denatured globin were reported by Garg and Narwani. Persistent potentials across nonuniform membranes (671), another interfacial theory of fixed site membrane potentials (1035) and membrane potentials dependent upon solvent (EtOHHzO) (478) were described. A flow cell method for measurement of ion exchange membrane potentials was compared with a membrane strip method (631).
GLASS ELECTRODES, MACRO AND MICRO, FOR HYDROGEN AND CATION ACTIVITY MEASUREMENTS The oldest ion selective electrodes continue to fascinate workers in a variety of scientific disciplines. Each brings his technique and insight to bear on the details of glass electrode response. A short book describing glass electrodes has been written by members of the pioneer group under B. P. Nikol’skii (851) while Csakvari summarizes new developments by the Hungarian School of glass electrode technology (242). Steuerwald and Corbach have correlated H20 diffusion with H + and/or Na+ surface ion exchange and potential-time response (1102) of simple glasses related to Corning 015. Csakvari et al. distinguish two surface layers on exposure to water. The inner layer is characterized by a n alkali ion concentration gradient (241). Wikby
Topic
Reference(s
Sodium ion analysis in clinical medicine Intracellular sodium activity and sodium pump in small neurons Sodium and potassium activities in muscle Analysis of sodium and potassium in corn and sugar beet tissues Analysis of sodium in soda-industry products Monitoring tablet dissolution Analysis of sodium in ceramics Continuous determination of sodium in high purity water Potentiometric analysis of sodium in river and mineral waters Rapid potentiometric determination of sodium in drug solutions Determination of sodium in waste solutions Sodium determination in mill liquors
(896)
Analysis of saline soils Studies of sodium tartrate complexes pH adjusting solution for pNa measurement Determination of potassium in inorganic and organic substances Determination of sodium and potassium activities in dilute solutions Increasing sensitivity of a sodium electrode by Ag pretreatment Response of sodium silicate glasses t o univalent and divalent cations A potassium sensitive glass electrode composition Use of Cs/Cs glass electrodes
11116) (279) 1298)
(1144) (46)
(195)
1870) 748) 863) ‘266) i (
11189) 589) ‘965)
1610, 654, 812)
115) (181, 551) (1264)
+
+
1923, 924) (189) 132)
has measured surface film resistance and correlated results with increasing Li+ in inner layers (1238-1240). Baucke has also determined Li+ profiles in the surface layers of glass electrodes (86). Exchange rates and transient potential responses have been reported by Karlberg (543-545). Ion exchange has been followed by radioactivity (792), and deuteron-proton exchange (357). Transfers of ions to silica (954) and to porous glasses (438) have been characterized by electrical measurements. Boksay (142) has produced a transport model accounting for alkali ion vacancies. Response time and reproducibility of pH glass responses in methanol, DMF, and acetonitrile are reported by Moon (799) while two papers describe lithium ion error responses in aqueous and nonaqueous solvents (755, 809). Determination of solvent autoprotolysis constants (185) and, in particular, the values for HzO in the presence of K N 0 3 (510) are described. Responses to pH of a number of new glasses were documented: LizO-PzOa-Al~03 (1371, N ~ z O - A ~ Z O ~ - B Z O ~ - S ~ O Z (1269), and lithium borosilicate, lithium borate (136). E M F measurements on Pyrex and fused Si02 membranes in molten salts are reported by Van Reenen and De Wet (1191) and Lesourd and Vallet (656).Responses of Corning 015 to Na+ and H+ suggest that Eisenman’s n-type nonideal behavior is insufficient to fit the data (278). A similar observation prompted Buck to propose an alternate theory of glass electrode response (170) based on solid state principles and applying to heterogeneous and homogeneous site glasses. Diffusion and conduction in alkali lasses are topics of four papers (308, 709, 1139, 1142). bive papers and patents describe progress of the Nikol’skii group on the fabrication and responses of electron-conducting glasses (25, 58, 852, 853, 1063). 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
33R
Table IV. Applications and New L i q u i d Ion Exchange Electrodes Part A. Cation-sensitive Electrodes Topic
(1) Measurements of calcium in serum and
plasma
(2) Applications in sugar beet industry ‘3) Applications to detergent builders ( 4 ) Application of C a Z and divalent ion +
electrodes in water analysis ( 5 ) Electrodes with Baz+-and Srt+-selec-
tive responses (6) Electrodes for selective response to onium cations ( 7 ) Electrodes for measuring choline and applications to analysis of acetylcholineesterase and organophosphate pesticides (8) Electrodes sensitive to vitamins B, and
Reference (9)
(154, 327, 328, 634, 668, 953, 956, 1072, 1111) (435) (131) (550, 737, 740, 872, 8 73) (658, 749) (1031) 191-93, 95)
(485)
B6 (9) Electrode sensitive to potassium using ion exchanger in plasticized polymer membrane (10) Microelectrode selective t o potassium (11) Applications of liquid ion exchange microelectrodes for potassium Part B. Anion-sensitive Electrodes Topic
(1) Dependence of selectivity of NOi-
over C1- on organic salt concentration in a nitrate electrode (2) Nos- selective electrode using Orion liquid in polyvinylchloride (3) NO3 - selective electrode composition patent (4) Nos - selective,membrane electrodes ( 5 ) Determination of nitrate and nitrite in
mixtures (6) Determination of nitrate in mineral waters ( 7 ) Determination of nitrate in cotton petioles (8) Determination of nitrate in plants, soils (9) Application of C1- electrode for salt in cheese (10) Perchlorate selective electrodes and responses (11) Iodide selective electrode composition (12) Determination of boron with BFI-selective electrode (13) Bicarbonate-selective electrode compositions (14) Effect of structure of carboxylate anions on response (15) Electrodes selective to maleic and phthalic acids (16) Electrode selective to trifluoroacetate 117) Electrode selective t o thiocyanate (18) Electrode selective t o aromatic sulfonates 119) Electrode selective t o bisulfite (20) Electrode selective to picrate (21) Liquid ion exchange membrane assemblies (22) Liquid microelectrode construction
34R
196) (1253) 1557, 559561, 1212, (1218) Reference (9)
1246) 1250) (1247) (362, 364, 365, 374) (806) (773)
A detailed analysis of high precision p H measurements has been given by Ducksbury and Telford (276) and a somewhat less detailed analysis is given by John and Pajdowski (521). A statistical standardization procedure has been reported (988).Problem areas in the use of glass electrodes, the suspension effect (202, 786, 787) and measurements in high ionic strength solutions (98, 892, 893) including sea water (427)were discussed. A detailed study of the p H response of a Na+ sensitive glass electrode (1258) points out the failure of the simple Nikol’skii equation. Several commercial cation selective glass electrodes were evaluated by Phang and Steel (908). The time response of an Orion 94-llA Na+-sensitive electrode is measured and found to be more rapid than others available in Japan (16). Applications of glass electrodes involving p H measurements are listed in Table 111, Part A. Measurements using sodium and cation-sensitive electrodes follow in Part B.
SENSITIZED ELECTRODES USING INTERPOSED CHEMICAL REACTIONS Use of electrodes coated with a reagent, which reacts with a desired soluble substance in solution to produce a stoichiometric product ion sensed by the underlying electrode, is one example of interposed chemical reactions. The principle is quite general, however. Determination of any substance which removes or adds an electroactive substance in the system is a more general concept as pointed out by Oehme (867).Guilbault (394) has reviewed the principles of immobilized enzyme electrodes. The fact of diffusion control of reactants and products through coated electrodes is treated theoretically by Racine and Mindt (952).Applications of enzyme electrodes have been reviewed (37). The big news in this field is the development of gas-sensing electrodes following the original idea of Severinghaus many years ago for monitoring C02. The ammonia sensing electrode based on p H shift of “immobilized” NH4C1 surrounding a p H sensing glass electrode has been evaluated and found numerous applications (68, 180, 261, 353, 650, 1188). Ammonia can also be monitored by following the equilibrium NH4f a t fixed p H using cationic glass or neutral carrier electrodes (361, 772, 794). Improved or new enzyme-coupled electrodes include those for urea (397),D-amino acids and asparagine (392),l-phenylalanine (396), glutamine (393), and penicillin (886). Electrodes sensing C02 are described in a review (843) and in patents (401, 522, 845-847). Enzyme electrodes based on COz sensors have been developed for urea and L-tyrosine (395). Other enzyme electrodes assay serum cholinesterase (240),rhodanase (694),/3-glucosidase (693), and blood glucose (407,864).
(159)
SEMICONDUCTOR ELECTRODES
139)
The effects observed when semiconductor electrodes are made part of an electrochemical cell depend upon rates of surface reactions. This statement is, of course, true for all electrodes. However, due to the electronic conductivity, the variety of effects is great for semiconductors. Most of the comments here apply to nonstoichiometric salts such as silver halides, as well as conventional semiconductor materials. For highly ionic crystals, oxidants and reductants in solution have little effect because the redox couple cannot oxidize or reduce the crystal (inject holes or electrons). Ion exchange by whichever ion can exchange most nearly reversibly tends to dominate and determine the interfacial potential. For pure electronic conductors where ion exchange is inhibited as in Pt, the redox couple determines the potential by rapid electron exchange. In between these extremes are semiconductors whose response depends on the extent to which surface equilibrium is achieved in a given electrolyte environment. Two recent articles should be consulted (162, 807). The chalcogenide electrodes developed a t Texas Instrument Company (513, 1168) respond to Fe(II1) by injection of holes and Fe(I1) has no effect on the potential. Applications include determination of sulfate (511, 522). Hole injection by oxidants or acids is the basis for analytical monitors of Ge, InSb, and Si (765).Frumkin has published data on InSb electrode potentials (1209).Other systems studied electrochemically include ZnTe (1015) which does not respond to
(959) 155, 373, 481, 818) (483) 11241) (375, 1248) (871) (486) 1487) f 489) 1482, 488) 1107) 154) (609, 800) (1101)
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
Zn2+ activity, As&
glasses (62), PbO2 (1220), MnOz
(194), and MoSi2 (295-297).
LIQUID ION EXCHANGE MEMBRANE ELECTRODES The relation of salt extraction (partition) equilibria to the selectivities of liquid membrane electrodes has received attention recently. An immense review of partition coefficients has been compiled by Leo, Hansch, and Elkins (655). The role of solvent extraction parameters have been discussed and applied by James, Carmack, and Freiser (507), Back and Sandblom (56), Baum (94), Ivanov (490), Materova and Mukhovikov (751), and Dubini-Paglia, Galli, and Mussini (274). Buck and Sandifer treat theoretically and by digital simulation the response of mixed valence electrolytes ( I 71). Time responses have been studied for anion-responsive membranes by Reinsfelder and Schultz (969). Current-voltage curves of an Orion Ca2+ -selective electrode were obtained by Gavach (340) and upsetting effects of current flow on potentiometric responses were observed by Liteanu, Popescu, and Hopirtean (683). Xew organic ligands for use in liquid ISE’s were reviewed by Simon and Morf (1073). Other topics include sources of error in Ca2+ measurements (178), bi-ionic potentials across n-butanol membranes (664), new optimized compositions for Ca2f-selective membrane electrodes (232, 378, 379, 750, 986), and applications of the Ca2+ electrode in titrimetry (468). Further examples follow in Table IV. APPARENT NEUTRAL CARRIER MEMBRANES The word “apparent” is used in the sense of a presumption because the mechanism of function of these electrodes is still obscure. Based on rather abundant literature on lipid bilayer membranes and facilitated transport of alkali metal ions by hydrophobic macrocyclic carriers, the thick membranes of commercial electrodes, responsive to alkali metal ion activities, have been presumed to operate on some variation of the Ciani-Eisenman-Szabo theory for bilayers. A t the present time, this theory without modification is untenable. Thick hydrophic membranes containing various neutral carriers, particularly actins, cyclic depsipeptides and polyethers must be electrically neutral. The overwhelming problem is to explain permselectivity for alkali ions, typically as the complex KVal+, when anions of comparable or smaller size than the oil soluble complex are present in the membrane as well. Elementary electrochemical argument demands that the membrane potential will be sub-Nernstian for potassium ion bathing solutions except when anions are immobile or otherwise not transported through the membrane bulk. However the problem is not so acute as it once was because Boles and Buck (143) have shown that Nernstian response to potassium for a valinomycin-based electrode is not as general as first supposed. Potassium salts of the large halides, pseudo-halides and most organic anions show Nernstian responses at low activities and the potential passes through a maximum and decreases with further increase of salt activities. Potassium picrate shows a negative slope at all accessibles activities. Facilitated transport by oil-soluble macrocyclic neutral carriers is most interesting in connection with cell membrane transport. Flux rates for facilitated transport by polyethers are reported by Reusch and Cussler (972) while Rechnitz and Eyal have measured alkali ion potentiometric selectivities and correlated them with complex formation constants (967). Molecular parameters needed for selectivity have been worked out by Morf and Simon (805). Ion pairing, which is a key to the behavior of these materials in electrodes, has been discussed for K F crown ether species (1131). New, substituted crown ethers in PVC are the bases for improved potassium selective electrodes (1005, 1006). Polyether complexes with bromine (1058) and KCoX4 salts (130) have also been reported. Simon’s group has developed a number of noncyclic neutral carrier for di- and monovalent cations (28-30). Properties of silicone rubber-based neutral carrier electrodes for K + have been reported (911, 913). Patents (230, 231) disclose the composition of the Beckman solid version of neutral
carrier electrodes. Further plastic supports and solvents are given two other patents (166, 1109). A fairly basic patent on neutral carrier systems was issued to Duke University, Inc. (1159). Applications of K + selective microelectrodes include measurements in membranes from Escherichia coli B (150, 695), muscle venous blood (457, 458), epithelial cells of the small intestine (651), and molluscan neurons (1OOO). Other applications include K + in sea water (36), soil (67, 1020), and monitoring dissolution of tablets (1145). Recent reviews of neutral carrier transports are by Eisenman et al. (211, 291, 1122), Tosteson (1158), Junge and Schmid (528), Pate1 (894), Funck et al. (330, 376) and Hauser et al. (421). Important theoretical analyses are by Hladky (456), Bdzil et al. (101), MacDonald and Bangham (707), and Lauger’s group (636, 637, 1097-1099). Two studies of thick membranes, including a Volta potential measurement appeared in Russian (391,877). A number of other membranes may involve noncyclic neutral carriers or they may be liquid ion exchangers due to hydrolyses of one or more components. The membranes do respond potentiometrically to H + (165, 208) and other monovalent ions (208, 461, 640, 676, 678, 685, 686). These membranes are polymer films containing a variety of uncharged plasticizers such as tricresylphosphate and phthalates.
CONVENTIONAL ELECTRODES OF ZEROETH, FIRST, SECOND, AND THIRD KINDS INCLUDING REFERENCE ELECTRODES These studies are listed in Table V Parts A, B, C, and
D.
ELECTRODES I N NONAQUEOUS SOLVENTS The fundamental problems of ionic energies in nonaqueous solvents, medium effects, acidity scales in nonaqueous solvents (with and without reference to aqueous acidities), thermodynamic properties, and equilibria of ionic substances in nonaqueous media received further attention in this biennium. The exchange between Popovych (929) and Salomon (1013) makes clear the status of free energies of solvation theory. Acidity via H2 electrode has been studied in pentamethylphosphonic diamide (652), sulfolane (219), methanol-Hz0 (113) methanol-acetonitrile (113), ethanol-HzO (367), 1-propanol water (99.9, propylene carbonate-Hz0 (990), formic acid (20), amyl alcohol (114), trifluoroacetic acid (905), dioxane-water (813, 814), acetic acid (21), pyrrolidone (499), formamide (832), and N methylpyrrolidone (280). Acidity in isopropanol- and ethylene glycol-water (Hammett acidity) (1167), buffer pH in the same mixture (23), activity coefficients of NaOH and pH corrections in dioxane-water (1062, 1255), dissociation of KCl in ethanol-water (541), effects of salts on acidbase titrations in nonaqueous solvents (372, 688, 1085), activity coefficients of divalent metal perchlorates in acetonitrile (662), acid-base equilibria in dioxane-water (1178), in acetic acid-chlorohydrocarbons (574), in alcohol- and THF-water (1252), and in formamide (248) have been reported. Electrode potentials for several electrodes of the zeroeth, first, and second (reference electrodes) kinds are summarized in Table VI. APPARATUS, CELLS AND ELECTRODE DESIGNS In addition to those items mentioned in previous tables, many new systems and electrochemical components have been reported, primarily in the patent literature. These are listed in terse form in Table VII. Automatic titrators have been reviewed by Franck and Huber (322). POTENTIOMETRIC STANDARDS AND LESS COMMON REAGENTS IN TITRIMETRY Activity standards for ion-selective electrodes used in body fluid analyses are reported by Durst, Staples, and Paabo (282). Divalent metal ion buffers (1250), anion and cation buffers (424), copper(I1) standards (135), solutions for calibration of pH meters and gas analyzers (1242), and a standard solution for redox potential measurements (666, 1117) are solutions for establishing fixed points on ISE response curves. Two new secondary pH standards, 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
35R
Table V. Conventional Electrodes of Zeroeth, First, Second, and Third Kinds, Including Reference Electrodes Part A. Zeroeth Kind Electrodes (' 'Inert" Electrodes) ElecTopic trode Reference(s)
Potentials of nitrite solutions Formal potential of nitrosyl sulfonate/ hydroxylaminedisulfonate system Std potential of the sulfite,' dithionate system Formal potential of Se(IV)/ Se(V1) system Formal potential of Cu(III)/ Cu 111) tellurates Formal potential of ferri/ ferrocyanide Formal potential of ferri/ ferrocyanide Formal potential of Fe(II)/ FelIII) pyruvates Std potential of Fe(II)/Fe(III) 5-35 "C Potentials of Fe(II)/Fe(III) halides Formal potentials of binuclear metallocenes df Fe, Ru, Os Formal potentials of Sn(II)/ Sn(1V) in chloride media Formal potential of ruthenium ammines Formal potential of Ir(III)/ Ir (IV) Formal potential of p-molybdosilicic acid Potentials of Ce (111)/Ce (IV) us. p H Potentials of Ce(III)/Ce(IV) to measure megarad dose rates Potentials of TcIIV)/Tc (V) thiocyanates Formal potentials of NpIV)/ ND(IV)in O H PotentiaIs of substituted guanidines Potentials of substituted bisphenols Std potentials of T C N Q TCNQ Potential of Brilliant Cresyl Blue Potentials of hipyridylium, bipyrylium and hithiopyrylium salts Potentials of short-lived radicals Adsorption of H - on Pt a t reversible H '/'H2 potential Hydrogen electrodes in acid media Stand ird hydrogen electrode conc'c ?)t Improved hydrogen electrode with Raney Pt Behavior of platinized Pt at H, evolution potentials Parameters of the normal standard H2-electrode us. Ag AgCl Potentials of the Pd-HL electrode, 25-200 "C Potentials of the a @
Pt,Au,C Pt
(629) (40)
Part A. Zeroeth Kind Electrodes ("Inert" Elm:trades) ElecTopic trode Reference@)
P d hydride electrode 25-195 "C (34) NMR study of Pd-H2 electrode system (35) Iridium/iridium oxide electrode for in vivo p H (36) Effect of electrode pretreatment-Pd electrodes
Au
(254)
Pt
(593)
Pt
(996)
Pt
(1123)
ZnO
(1186)
Pt
(564)
Pt
(1237)
Pt
(1089)
(41) (42)
Pt
(1086)
(43)
Hg
1262)
(44) (45)
...
1667)
BC
(498)
Pt
1272)
Pt
1540)
Pt
( 760)
(49) (50)
Pt
11040)
(51)
Pt
11071)
Pt
(337)
C
(50)
Pt
(472)
Hg
11181)
...
1465)
Hg
1369)
(39) (40)
(46) (47) (48)
(52)
(865) 1133) 1126)
...
(128)
...
(907)
...
(576, 578)
A N A L Y T I C A L CHEMISTRY, V O L . 46, N O . 5, A P R I L 1974
..
(714)
... ...
electrode Adsorption of inorg. ions on ... Pt Rate of potential equilibrium ... on P t , Au, Sn02, Ir Pt-O? rest potentials and ... electrode pretreatment P t , C12 electrode applications ... Poisoning Pt with surfactants, . . . amines, sulfides Surprising effect of IR on Au ... electrode potentials Reversibility of Au electrodes . . . Surface physics of metal ... electrodes Temperature coefficients of ., , electrode potentials Graphite and carborundum ... electrodes as indicators Glassy C, graphite oxide, ... fluoride, and impregnated electrodes Carbon cloth electrodes ... Use of tungsten-bronze ... electrodes Use of Au, P t , Bi, Ti, Ni, ... and C in potentiometric titrations Stainless steel electrodes as .,. indica tors Part B. Electrodes of First Kind Topic
(1) Potentials of high-purity metals in sea
water (2) Use of aluminum electrodes (3) Titanium and MnO? anodes (4) Mo and W electrode potentials in aq. H?O? (5) Reversible Cu electrode with adsorbed S (6) Effect of ultrasonic fields on electrode potentials of Fe, Ni, Ti, steel, Cu (7) Copper electrode in HF (8) Mechanochemical behavior of Cu/Cuz+ (9) Thermodynamics of P b / P b * + electrode 110) Thermodynamics of Zn Zn2- single crystal electrode (11) Thermodynamics of Hg/Hg electrode (12) Std potential of Cd,Hg, 'Cd2 (13) Behavior of metals on amalgams in fluorine-containing electrolytes (14) Std potential of NH4-amalgam (15) Formal potential of molybdenum amalgam (16) Formal potential of Cu 'Sn amalgams (17) Std potential of Cs-amalgam +
+
(644)
,
(37) Properties of Ru as a n (38)
...
+
(404, 405, 674, 677, 691) (745) (552, 906) (1270) (436) (600) (829) (264) (616 ) (648) (289, 783) (767) (722) (410) (573, 1228) (491) 171, 554)
Reference(s)
1383) 1197-200) 1530) (335) (70) (1090) (850) (419) (1196) (148, 149) (884) (205) (356) (1105) (555) (1106, 1267) 1815)
Table V. ( C o n t i n u e d ) Part C. Electrodes of Second Kind Topic
Part B. Electrodes of First Kind Topic
Electrodes of second kind a t low concentrations of common ion Std potential of thalamid reference electrodes Antimony-oxide microelectrodesconstruction Antimony-oxide microelectrode application in kidney measurements Antimony-oxide electrode application to COP monitoring Std potential of Sb/Sbe03 electrodes Nb/Nb20a response to pH W electrodes in potentiometric titrations Oxides for hydrogen electrodes in acid M n 0 2 powder electrodes Oxygen redox electrodes
Use of T1-amalgams for monitoring dissolved oxygen Review of measurements with amalgam electrodes EO values of some M/Mn+ electrodes Formal potential of Ag/l,lO-phenanthrolines Formal potential of Au/AuClOH-, Au/AuBrOH Std potentials and heats for Am/ Am(I1I) Std potential of R h / R h ( I I I ) Part C. Electrodes of Second Kind Topic
Review of reference electrodes in many solvents including molten salts Review of Weston cells Reference electrodes for pH measurements Ag/AgCl electrodes-properties, behavior Ag/AgCl electrodes-new constructions Ag/AgClrJ - reference electrode Ag/AgBr-temperature coefficient Ag/AgI in flowing solutions Use of Ag electrodes in C N solutions Std potential Ag/Ag,S Pb/PbCL; Pb/PbBr2; P b / P b S 0 4 electrodes Calomel electrode construction Radiation effects on calomel and Ag/AgCl electrodes Std potential Hg/Hg(I) picrate Pt-foil Hg/HgS electrodes
F&ference(s)
(69) (784) (778)
Referencei s )
(88, 89) (85, 87)
(565) (724) (926) (1197, 1198) (1262) (494) (222) (955) (134, 271, 876, 1172) (332) (237, 669, 670, 779) (698, 1154) (734) (828)
C/Chloranil pH electrode Cd/CdS04 and Cu/CuS04 reference electrodes Theory of potential-pH diagrams Potential-pH diagrams, Fe/H20 Potential-pH diagrams, Sulfide minerals Potential-pH diagrams, Cu/Cl/HZO Potential-pH diagrams, Cu/SOd/H20 Potential-pH diagrams, S/HZO Potential-pH diagrams, metals/S/Cl/ HzO Potential-pH diagrams, Cd/H20 Potential-pH diagrams, Fe/S/H20 Potential-pH diagrams, Pt/H20
(352, 547) (385, 583, 878, 904, 1155) (718) (781) (73) (881) (603, 604) (495, 529, 1057) (463, 1265, 1266) (597)
(536) (535) (1184) (1135) (700) (127) (699)
Part D. Electrodes of t h e Third Kind Topic
Reference@)
Review of electrode of 2nd and 3nd kinds Hg/Hg, Cu mercaptobenzothiazolates for Cu2 measurement
(235) (1243)
1602) (999)
+
Table VI. N o n a q u e o u s Electrode Potentials Topic
k / I - potentials in propylene carbonate Ferrocene, cobaltocene, I3-/I -; Bra-/Br- potentials in chloroform L-/I - potentials in liquid SO2 Potentials of C u ( I I ) / C u ( I ) in acetonitrile Potentials of quinone/hydroquinone and chloranil electrodes in dry acetic acid Potentials of dihydroxyflavone derivatives in dioxane and in trifluoroacetic acid Potentials of formamidine disulfide/ thiourea in dioxane-H20 Potentials in ethyl pyridinium bromide as solvent Poly (4-vinyl pyridine) bromine complex in propylene carbonate, potentials Potentials of M,/M + (sodium, potassium, lithium) in methanolpropylene glycol
Topic
Reference(s)
(11) Potentials of M / M +, M/M2+ iH, Li,
(12) (13) (14) (15) (16) (17) (18) (19)
(20) (21)
(22)
Na, K, Rb, Cs, Ag, Cu, Zn, and Cd) in nonaqueous solvents Potentials of M / M +,M/MZ+ (Ag, Cu, Zn, Cd, Hg, Sn, Pb) in dry methanol Std potentials of Ag/Ag +, Hg/Hg2+ and halide complexes in acetonitrile Potentials of M / M + (Li, Na, K) in ethylene glycol-H?O Potentials of P b / P b * in liq. ammonia Potentials of Cs(Hg)/Cs+reference in nonaq. solvents Potentials of Cs(Hg)/Cs+reference in aq.-nonaq. mixtures Arguments for reference electrodes in same solvent as test solution Potentials of P t , Cu, Ag, and Hg in pyrrolidin-2-one and half cells with salts Ag/AgCl in formamidemethanol mixtures Ag/AgCl in urea-water mixtures Ag/AgCl in N,N-dimethylacetamide +
A N A L Y T I C A L C H E M I S T R Y , VOL. 46, NO.
5,
1224) (840) (220) (624) (645) (816) (817 ) 11180) 1160, 1079) 1592) 1626) 11261)
A P R I L 1974
37R
Table VI. (Continued) Topic
Topic
€7 efprence ( 8 )
mixtures
Ag/AgCl and Ag/AgBr in methanolpropylene glycol Ag/AgCl in anhydrous methanol Ag/AgCl in ethanol-H20 mixtures Ag/AgCl in 1-propanol-HzO mixtures Ag/AgCl in isopropanol H 2 0 mixtures Ag/AgCl in 1-butanol and H20 mixtures Ag/AgCl in tert-butanol-H20 mixtures Ag/AgCl in phenol-H20 mixtures Ag/AgCl in glycerol Ag/AgBr and Ag/AgI in ethanolacetone-H20 mixtures Ag/Ag halides in glycerol-H20
(34) Ag/AgI in ethylene glycol-H20 (35) (36) (37) (38) (39) (40) (41) (42)
i
mixtures Ag/AgIOa in formamide Ag/Ag acetate in formamide Li/LiBr in diglyme and propylene carbonate TlIHg)/TlCl in dimethylformamide Calomel electrodes in methanol Cu/Cu soap electrodes in methanol Aromatic polynuclear hydrocarbon and ions as references in liq. NHB, H2S0,,HS03F, and molten SbCl, Reference electrodes for cryolite
625)
(833) ‘834) 1077, 1078) (1070) 112061 (11) 190) ‘194)
Table VII. Apparatus, Cells and Electrode Designs Topic
Reference@)
(304, 402, 715, 1007) Probes and cells for CO, monitoring Probes and cells for O2 monitoring 175, 777, 790, 855, 974, 980, 981, 1199,1235) 152, 665, 836, 837, 936) Reference electrode construction (117, 155, 1091) p H devices based on transistor properties 1109, 288, 310, 409, p H meter and accessor designs 469, 556, 854, 921, 958, 1136) (41, 158, 306, 370, 732, Primarily flow-through electro776, 971, 1027) chemical cells (53, 119, 313, 595, 842, Electrochemical cell designs for titrator and other uses 1039, 1246) 18, 13, 84, 115, 179, Various membrane electrode
Reference (SI
Topic
designs
387, 389, 7ZC3,759, 775, 808, 838, 839, 932, 1037, 1192) Continuous analyzers ‘123, 368, 534, 57.9, 753,802, 10.?8,1094) Automatic potentiometric titrators 151, 120, 132, 156, 157, 190, 244, 245, 274, 263, 267, 275, 303, 403, 440, 517, 608, 705, 746, 780, 831, 901, 920, 938, 970, 1024, 1083, 1093 1157, 1234) Fast-flow mixing apparatus 11148)
Table VIII. Selected Newer Reagents and Aqueous Titrations Redox titrations using
Hypobromite ICN, BrCN Pu (sod)2 Dichloramine-T N-C hloroacetamide Co(II1) Lead tetraacetate Hydrazine Hydroxylamine Hg (1) Borohydride Ascorbic Acid Fe(I1)-mannitol sulfate Fe(I1)-EDTA TilIII) V(I1) Mo(II1) Precipitation titrations
Sulfate analyses Use of tetraphenyborate for organic bases Use of thiourea Dithiocarbamates Bisthiosemicarbazones Dithiooxamide 38R
Reference(s)
1859) 1889) (825,957) (501, 826) 11075, 1076) (411) (8211 (858, 962, 964) 1525, 526, 860, 861 1214-121 7 ) (771) ( 788) (57, 210, 439, 961, 101 7 ) 12 70) (1067) (233, 343, 747, 1001, 1002) (17-19, 934) 1293, 294) Reference(.=,)
(106, 359, 524, 572, 983, 1061) (916) (333) (1173) (184) (118)
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
Precipitation titrations
Reference (s)
Mercaptoquinoline (121, 122) Cupferron (492, 493) Reinecke salt l 60.1’1 Evaluation of methods for ZnZ 1590, 1066) Comparative study of methods for (1230) thiols Determination of azide 172) LaiIII) 1770: +
Complex formation titrations
F e f I I I ) with E D T A PbiIV) with E D T A Divalent ions with DCTA Divalent ions with T E P A PclII) with E D T A and thioglycolic acid C a 2 - with EGTA
Reference ( s )
11187) 1822) (1225) (1224) (1183) 1663.1’1
Organic and biologically important analyses
Sulfur. halogens and metals in organics Diazotization methods for: Sulfanilamide derivatives Aromatic amines Derivatives of acetoacetic acid. Acid-base derminations include: Amitrole (3 amino-1,2,4-triazol) Antithyroid drugs Pseudothiohydantoins
Reference(8)
(10, 1210, 1211) (214,1126) ( 752) 1607
(12291 (918)
‘1174.1’1
T a b l e VIII. ( C o n t i n u e d ) Organic and hiologically important aiialyses
lirotropine Monuron Fulvic acid Prothrombin coagulase 2',3'-Cyclic nucleotide 3'I)hosphnhydrolase Nucleoproteins of tobacco mosaic virus Ovalbumin-CsCl
Organic and biologically important analyses
Reference(s)
Reference@)
B-Latamase Adenosine Other organic analysis are for: Isoniazid by V (V) Unithiol by CulII) Malathion Theophylline Some throstatics by Ag(1) and Hg'II) titrimetry
( 3 17)
(1259) (334) (931)
(627) (895) 1471)
1632)
1529) 1963)
1347) ( 785) 1253, 939)
(917)
Table IX. Electrode Configurations with. S a l t / M e t a l I n t e r f a c e s Conductor
Pt
Coated support
Ingredient or second layer
Stearic acid
Inside interface response
MethyltriProton exchange n-octylammonium with PtOH? stearate Pt PolyvinylQuaternary ? chloride ammonium salt Pt PolyvinylCa didecylphosphate ? chloride in dioctylphosphonate Determination of nitrogen oxides using coated-wire nitrate electrode Patent Sulfonated Ion exchange material ? polystyrene Pt Percl .:orate Electron exch. salt9 of radical cations Pt Pb, CU, PhrAs Electron exch. salts of radical anions Patents on radical ion-based electrodes P t or Ag ? PolyvinylKBPhr chloride Wire Octadecyldimethylbenzyl ammonium chloride or thiocyanate Oxidized Block p-Dodecyldinitro Proton exch. metal copolymer phenol, etc siloxane, carbonate Oxidized Block Gramacidin, Proton exch. metal copolymer valinomycin, etc. siloxane, carbonate Graphite PolyvinylCa2 ion exch. Proton exch.? chloride Graphite Xylene Cu(I1) dithizonate Proton exch.? Graphite Silver Electron exch. salts, etc. Graphite Liquid ion Proton exch.? exchangers or neutral carriers in solvents C -paste AgC1Electron exch AgLS mix Pd, Pt-Rh, Glaze of Electron exch.? ion-selective Cr, F e glass C u , Ag, Co. Glass Ion selective glass Electron exch. Cd metal halide Glass membrane H g + ion exch.? Hg Cu, Hg, F e Oxide? Borosilicate glass Electron exch.? AI (3 p diam.) Ag-film Corning 015 glass Electron exch.? Ag Pt HE HgS Electron exch. +
+
Pd
PdO
THAM and TRICINE, are reported by Bates and Robinson (81, 82). Buffers for dioxane-water mixtures (22), sea water (415), and for measurements a t elevated pressures and temperatures (326) have also been reported. Other in-
Outside interface response
Ref.
Proton exch.
t 1221)
Anion exch.
1508)
C a 2 - exch.
(192)
Ion exchange
1566) (509)
CIOa- exch.
( 1054-1 056)
Ion exch.
f 1053)
Ion exch.
(1052) 1251) i1110)
Proton exch.
848)
Ca2 or K * exch.
1848)
C a 2- exch.
138)
+
Cuz exch. Ag' exch.
(
176) 1003)
Ion exch.
f
1003)
Ag+ exch.
1774)
H +,K
i
+
+
exch.
1
844)
H * exch.
'10.2, 903)
H exch. H exch.
(
+
H exch. H g 2 +or S 2 - exch. H H + +e+
(161) 729)
1345) (1243) (386)
formation includes activity coefficient calculation by nomograph (1263), activity coefficients of HC1, NaC1, and KC1 in mixed electrolytes (206, 207), and acidity constants for carbonic and boric acids in sea water ( 4 2 4 ) . 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
39R
Table X. Liquid-Liquid Interfaces and Junctions Topic
Liquid-liquid interfaces as potentiometric sensors: n-butanol-water as sensor for acids and bases Liquid-liquid electrodes-glass frit containing alcohols, ketones, ether Measurement of the impedance of the interface between two immiscible electrolyte solutions Interfacial potentials and ion exchange equilibrium between two immiscible electrolyte solutions Calculation of liquid junction potentials including non-sym. binary electrolytes, time dependences and self diffusion Evaluation of changes in liquid junction potentials with solid-state ISE’s Liquid junction potential and vacancy structure in concentrated aqueous solutions of nitrates Liquid junction potentials between electrolytes in different solvents Liquid junction potentials between electrolytes by the sucrose gap method Activity and transfer of ions in concentrated electrolytes Transference number of ions from liquid junction potentials
References
Phase boundary potentials in cells with transference between water and organic solvents E M F of a cell with transfer and Volta potential for studying water-isoamyl alcohol interface Determination of shifts in standard potential scale and liquid junction potential in mixed solvents by measurement of zero charge potential Surface potential of 1,4-dioxanewater mixtures Ionic entropies of transfer from water to nonaqueous solvents Calculation of H medium effect in ethanol-water, based on surface potential constancy Activity coefficients of single ions in N-methylformamide-water Ionic product of a mixed solvent with a common ion Generalized correlation of activity coefficients of electrolytes t o 6M Generalized DebyeHiickel theory for concentrated electrolytes Refined Debye-Hiickel theory and ion association Ionic hydration and single ion activities
(462) (1051)
(342) (360, 803, 915, 1175)
(97)
+
(11
(238) (869) (1064) (371)
A section which thoroughly treats inorganic potentiometric titrations has been severely culled because few titrations are more than reworking of old methods. One curious idea is the use of ionic strength shifts in the Fe(II)/ Fe(II1) and Ce(III)/Ce(IV) activities (at constant concentration ratio) to follow ordinary precipitation titrations such as BaC12 + NazS04 (587). An unusual titration is that using Crz072- to determine redox capacity of a n electron exchange resin (951). Two theoretical treatments and applications are given for determining weak acids in mixtures (539, 950). Other titrations involving unusual reagents are summarized in Table VIII.
SOME NEW DEPARTURES AND FUNDAMENTAL PROBLEMS I N POTENTIOMETRY A number of new electrode configurations have appeared, and a t least four fundamental topics on the construction and function of ISE’s and cells have received attention during this biennium. These topics were mentioned in the previous review. They are: (1) potential and potential distribution at salt/metal interfaces with reversible exchange of a common ion or electrons, (2) potential and potential distribution at liquid or solid electronic conductor interfaces without reversible common ions, (3) liquid junction potentials, and (4) charged species transport in liquid and solid membranes. Topic 1 was interpreted thermodynamically by Sato (1018) and reexamined by Marton and Pungor (739). Interfacial potentials of salt/metals, defined in terms of the electron’s electrochemical potential, shows that “complete” equilibrium is crucial to the definition and value. Salts equilibrated with common metals show responses quite different from salts equilibrated with elemental “anion.” Photo effects are predicted and can be explained. There is a minor effect of dopants on the Fermi level a t constant stoichiometry, pointed out in Jaenicke’s review (504), but there is no basis for Hoffman’s correlation (460). An improved version of Wagner’s theory of mixed conductivity solid electrolyte cells has been advanced by Sudarikov (1113). Hladik and Jaumer (455) have com40R
Topic
References
(681, 682)
A N A L Y T I C A L CHEMISTRY, V O L . 46, NO. 5, APRIL 1974
(1036) (140) (506)
(259) (2) (1009)
(258)
(898) (163) (287) (1257) (984, 985)
pared Ag/AgNOs . TlNOS(s) interfacial potentials with Ag /Ag+. Some unusual electrodes involving “all solid state” configuration are listed in Table IX. Speculation by this author on the potential determining processes are included. Liquid-liquid systems and properties of, or related to, liquid junctions are listed in Table X. Topic 4, transport in ionic membranes, has received extensive theoretical treatment by solution of the flux equations for various boundary conditions, numbers, charges, and mobilities of species. Recommended are studies by Macdonald (706), Buck (169), Stishkov (1103), Malvadkar and Kostin (725), Barry and Diamond (fixed sites) (76, 7 3 , Kobatake (5681, Kataoka (548),Arndt, Bond, and Roper (47) and computer solutions by Onega (875). Reviews of electrochemical phenomena are by Teorell (1141) and Franck (323). Exact solutions of steady state transport of ions of one kind in thin membranes are by DeLevie, Seidah, and Moreira (256, 257). Hydration of ions (1169), activity coefficients (537), concentration profiles (619), permselectivity relations (538, 582, 1096, 1200), self-diffusion coefficients (599), transport us. concentration gradients (1249) and salt diffusion (975) in ion exchange and hydrophilic membranes have been discussed. Models giving conditions for high level ionic transport in the superionic conductors have been presented by Rice and Roth (973), Koda (569), and Van Goo1 (1190). In a continuing series of papers, Takahashi describes conductivities, applications and experimental techniques for superionic conductors (1127-1130). Kummer has also reviewed the properties of p-alumina (620). Ag/Ag,RbIs interface reversibility (1041), cell e.m.f‘s with dissolved IZ (43), interfacial kinetics (42), interfacial impedances (including other solid silver electrolytes) (44), double layer capacitance (including P t , C as well as Ag electrodes) (445) have been reported. Papers on impedances of the Ag AgSSI interface (1260), AC and DC responses of the cel Ag/AgBr/Pt (1233), conductivity of AgCl single crystals over a wide frequency range (226), and three papers on the DC properties of pure and doped PbBrz (10321034) have appeared. Three papers deal with the meaning of the electrochemical potential (59, 417, 418). An interesting commentary on the interfacial potential components of the standard hydrogen electrode is given by Gil-
i
eadi and Stoner (354) and Bockris (138).Since the electron electrochemical potential of the Cu/Pt interface is defined, there has been previously no reason to question whether there is in fact, an inner potential difference a t this interface. For those readers who follow the arguments relating conventional interfacial potentials, rational POtentials based on the potential of zero change (p.z.c), and surface potentials, three new papers have appeared on the isoelectric points a t a solution-air interface (2921, real POLITERATURE CITED Abraham, M . ; Hechler. J J.; Electrochim. Acta 1972. 1 7 ( 1 0 ) , 1849-55 ( F r ) . Abraham, M. H., J. Chem. Soc., Faraday Trans. 7 1973, 69 (Pt. 8 ) . 1375-88. Abramov. A. A,: Mashevskii, G. N.; Roi, N . I . ; Fedoricheva. T. V.. Obogashch. Rud 1971, 1 6 ( 4 ) , 27-31 (Russ). Abramov. A. A,; Alekseev. V. P.; Gordeev, A. A,; Mashevskaya. G. V.: Mashevskii, G. N.; Serov. G. V.: Fedoricheva, T. V . , Otkrytiya. lzobret.. Prom. Obraztsy. Tovarnyne Znaki 1972, 49 (13), 181. Adametzova. H.; Gregr. J.. Chem. Prum. 1977. 21(10), 506-9 (Czech). Adhikari, M.; Ghosh, D . , J. Inst. Chem.. Calcutta 1973, 44(Pt. 6 ) , 194-6 (Eng). Adhikari, M.; Biswas. G. G., J. lnst. Chem., Calcutta 1973, 45 (Pt. l ) , 14-16 (Eng). Adolph, R. J.; Bernstein. A. H.. U.S. Patent 3,607,788 (21 Sept. 1971). Agarwal. R. P.; Moreno. E. C.. Talanta 1971, 1 8 ( 9 ) . 873-80. Agterdenbos, J . : Haarsma. J. P. S.. Fresenius' Z. Anal. Chem. 1973, 264(5). 347-8 (Ger). Ahmad, S. I . ; Malik, W. U., Tenside 1977. 8 ( 5 ) ,256-9 (Eng). Ahrland, S.; Kullberg, L., Acta Chem. Scand. 1971,25(9), 3457-70. Akazawa, T.. U.S. Patent 3,713,992 (30 Jan. 1973) Apazidi, A. I,, Dokl. Akad. Nauk. Uzb. SSR 1972, 29(6). 33-4 (Russ). Akimoto, N . ; Hozumi, K., Bunseki Kagaku 1971, 20(9), 1186-91 (Japan). Akimoto, N.; Hozumi. K.. Bunseki Kagak u 1972, 21 (11). 1490-7 (Japan). Akinchan, N. T.; Prasad, S. N., Trans. SOC. Advan. Electrochem. Sci. Technol. 1971, 6 ( 3 ) . 91-2. Akinchan. N. T.; Prasad, S. N.. lndian J . Chem. 1972,10(8), 845-7. Akinchan, N. T.; Prasad, S. N.. Trans. SOC. Advan. Electrochem. Sci. Technol. 1973, 8 ( 2 ) , 71-2. Aleksandrov, V. V.; Pan'kova, S. A,, Khim. Tekhnol. (Kharkov) 1971, No. 20, 135-8 (Russ) , Aleksandrov, V. V.; Burakhovich. A. A,. Fiz. Khim. Rastvorov 1972, 154-9 (Russ). Aieksandrov, V . V.; Grineva. N . F., Zh. Fiz. Khim. 1973, 47(6), 1614 (Russ). Aleksandrov, V. V.; Spivak, L. L.; Bezpalyi. B. N.; Koz'yakova, T. N., Zh. Fiz. Khim. 1973, 47(8). 2172 (Russ). Aleksandrova. A. M.; Gubareva, D. N.. Agrokhim. Gruntozn. 1970, No. 15, 191-7 (Ukrain). Alekseev. V. A,; Peshekhonova, N. V.; Shul'ts, M. M., Zh. Prikl. Khim. (Leningrad) 1972, 45(5), 976-80 (Russ). Alimarin, I. P.; Petrikova, M. M.; Kokina, T. A , , Ref. Zh., Khim. 1973, Abstr. No. 4G25. Allam, A. I . ; Hollis, J. P., Soil Sci. 1972, 1 1 4 ( 6 ) ,456-67. Ammann, D.; Pretsch, E.; Simon, W.. Anal. Lett. 1972, 5(11), 843-50. Arnmann, D.; Pretsch, E.; Simon, W., Tetrahedron Lett. 1972, (24), 2473-6. Ammann, D.; Pretsch. E.; Simon, W., Helv Chim. Acta 1973. 5 6 i 5 i . 1780-7 (Ger) Amosse. J.; Rubaud, M.; Barbier. M . J., C. R. Acad. Scl.. Ser. C 1971, 273(25), 1708-10 i F r ) . Andreeva, 0. S.; Danilkin. V . I . , Elektrok h m i y a 1972. 8 ( 1 ) , 56-8 (Russ) Anfalt, T.; Jagner, D.. Anal. Chim. Acta 1971, 56(3) 477-81.
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P.Z.C.
and pH
ACKNOWLEDGMENT The author gratefully acknowledges the help of his students A. J. Bentz, S. E. Riffle, and J. R. Sandifer. Some library and clerical expenses were provided by National Science Foundation grant GP-20524.
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