Amperometric titrations - Analytical Chemistry (ACS Publications)

Amperometric Titrations John T. Stock, University of Connecticut, Stows, Conn. 06268

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HE PERIOD COVERED by this survey is from the previous review (271) through October, 1971. Unless otherwise specified, potentials are with respect to the saturated calomel electrode (SCE). Reviews of electroanalytical techniques (113) and of coulometric analysis (198) include amperometric titrimetry. Amperometric methods have been discussed with respect to industrial analyses (47, 1 1 4 ) and to complexometric titrimetry (157). These and other methods have been considered in reviews of amidoximes as analytical reagents (53) and of electrochemical methods for determining platinum metals and gold (82). Factors that influence the limiting absolute error of a n amperometric titration have been considered (230). A mathematical theory of linear nonprecipitating titration curves (140) and a graphical method for end point location in complexing titrations (250) have been given. The accuracy of the method of tangents in such titrations has been examined (102). Methods for end-point location on extensivelycurved plots have been reviewed and a n end-point evaluation method has been proposed (315). Accounts of the evaluation of random titration ewer (128), the statistical characterization of titration curves (178), and the elimination of dubious values during the calculation of such curves (177) have appeared. A logarithmic form of equation has been derived in a study of the differentiation of very simple mononuclear complexes fr3m polynuclear ones (103).

APPARATUS AND METHODOLOGY

The characteristics of amperome kic and other titrimeters have been discussed (183). Automatic and semiautomatic titrators have been reviewed (277) and a n automatic device for titrations a t the dropping mercury electrode (DME) has been described (275). A rotating platinum electrode (RPE) in acidified KMn04 has been used as reference electrode in the amperometric titration of alloying agents in steel (127). A helical-form rotating electrode (258) and a revolving titration vessel (34)have been patented. Descriptions of equipment 2nd technique for biamperometry include titration on a scale of 3 to 5 pl (16), improvement of titration curves by pretreatment of the platinum electrodes (139), the indicating system fixed

platinum electrode-RPE for pulse coulometric titration (269), and titration a t two DME’s (208). Advantages claimed for the latter technique are theoretically precise definition of the process, reproducible polarization curves, and errors of only 10.3% in the titration of solutions as dilute as 5 x 10-SM. Two stationary mercury indicator electrodes have been used in a new coulometric titration method for substances that undergo multistage oxidation or reduction (17 5 ) . A device for performing a biamperometric titration with the aid of a pH meter has been reported (176). A proposed amperometric method for determining the instability constants of simple complexes has been checked with iron(II1) as the indicator ion (100). Inverse polarography has been applied in titrations a t submillimolar concentrations (257). The effect of amperometric indication on the shape of the experimental curves in reactionstep coulometry has been discussed (108). Further studies of the depolarization amperometric end-point technique have been reported (77). End points in amperometric titrations have been determined by ac oscillopolarography (269) and by the second harmonic ac technique (74). ACID-BASE REACTIONS

Sodium hydroxide has been used to titrate boric acid amperometrically (239), HC1 and other acids redoxokinetically (223), highly-dilute H2S04 by the low-frequency (impedance) technique (@), and mixtures of picric acid and AcOH or BzOH biamperometrically (130). Bismuth electrodes, used in the acid-mixture titration (130), have been applied to the coulometric biamperometric titration of hydroxylammonium salts (131). Standard deviations of 0.007 to 0.009% are reported in the amperometric titration a t an antimony electrode, of K H phthalate and of BzOH with electrogenerated hydroxyl ion (321). Weak bases in AczO-AcOH medium t h a t contains hydroquinone have been coulometrically titrated to a biamperometric end point (307). Acid-base titrimetry in fused salts has been summarized (85). Alkyltin halides in isoPrOH have been titrated a t copper electrodes with KOH (159). PRECIPITATION AND COMPLEXING REACTIONS

Methods Involving Silver. Cyanide in water from coke plants has been

amperometrically titrated with AgN03 a t a vibrating platinum electrode (152). The lower limit is 1.4 ppm, but cyanide can be concentrated about 20-fold by ion exchange. Submillimolar concentrations of cyanide, either alone or in the presence of cyanate or thiocyanate, have been titrated with AgNOa a t zero R P E potential us. the Hg-HgIz electrode (122). Halogens and nitrogen in organic compounds have been determined by fusion with potassium, dissolution and titration of KCN and of halides with AgN03 (63). Titrations of cyanide and of halides in fused KNO, have been summarized (85). Cyanide-thiocyanate-sulfide mixtures have been analyzed by AgN03 titration of two aliquots (1.24). One aliquot gives the total, while the other is pretreated with formalin and gives separate end points for sulfide and for thiocyanate. Thiourea in admixture with NH4SCN has been titrated in ammoniacal medium a t 0 volt us. the Hg-HgIz electrode (120). The YH4SCN was then titrated a t pH 5 and a t 0 volt us. the SCE. Free sulfur in admixture with sulfide has been determined by boiling with KCN in 50% iso-PrOH, addition of formalin and Cd(N03)2,and titration of KSCN with (123). Conversion to and titration of KSCN has also been used to determine free sulfur in rubber (121). Amperometric back titration of excess AgN03 with K*Fe(CN)B has been used to determine HCHO in technical AcOH (304). The depolarization end-point technique has been applied to the AgNO3 titration of KaFe(CN)6, KSCN, KH2PO4, and the sum chloride plus iodide (77). Oxygen-flask combustion and titration with AgN03 have been applied to the rapid determination of chlorine in coal (238). Amperometric completion of chlorine determination in lignites is reported to be more accurate than potentiometric titration, but comparably reliable (168). Trace amounts of chlorine in polyurethanes have been titrated with AgN03 after dissolution in isoPrOH and pH adjustment (148). Chloride in Na2Cr207 and K2Cr207 has been titrated a t a n emf of 0.1 volt applied to a copper cathode and a platinum anode (187). Titration of chloride a t an RPE potential of +0.4 volt us, the normal hydrogen electrode is recommended when the solution also contains copper (527). The low-frequency titraticn of chloride with AgNO, has been studied (49). Cyanate ad-

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

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mixed with cyanide, thiocyanate, bromide, and chloride has been determined by precipitation as AgOCK, dissolution in "03, and titration with NaCI (125). Precipitation as (K,Ag),Co(X02)6, redissolution in HNOa followed by titration of silver with KC1 and of cobalt with &Fe(CX)6, have been used for the indirect determination of potassium (144). Halide impurities in polystyrene have been coulometrically titrated with silver after extraction into 2-butanone-ethanol (55). Mixtures of little bromide and much bromate have been analyzed by AgNO3 titration of bromide, reduction of bromate by H2S03,and titration of the bromide thus formed (126). Oxygenflask combustion and titration have been used to determine microgram amounts of iodine in compounds such as iodobenzoic acid (105). Submilligram amounts of iodide in water 0 have been titrated with & ' ~ 0 (26). If necessary, NaC1 is added, because reduction of AgCI a t the graphite cathode signals the end point. Biamperometric indication has been used in the coulometric titration of iodide with silver in molten ammonium sulfamate (28) or (Li,K)N03 (192). Amperometric titration with KI has been used to determine silver in mixtures with thallium and lead ( % I ) , copper and zirconium (138), and palladium (291). In the AgXO, titration of theophylline in pharmaceuticals, an emf of 0.2 'volt was applied to the silver anode and amalgamated silver cathode (318). The effect of salts on the AgXo3 titration of sulfhydryl groups in proteins has been studied (115). Sulfhydryl compounds have been titrated semiautomatically with electrogenerated silver ion (73). Disulfides in the milligram range have been titrated after reduction with hypophosphorous acid and organic phosphites (119). Amperometric titration with thiosalicylic acid has been applied to the determination of silver in ores (285). Microgram quantities of silver have been titrated with sodium diethyldithiocarbamate in the presence of CCl4 (202) or with dithizone in the presence of CHCl, or C6H6 (203). Silver in mixtures with copper or lead has been titrated with N,N-bis(p-aminoethyl)dithiocarbamic acid (60). The complexes formed by silver and 2,3-quinoxalinedithiol have been studied amperometrically (13). The ac polarographic titration of silver with 3-phenyl-2,6dimercapto-4-oxo-4H-thiopyran, or the reverse, has been reported (20). I n the analysis of binary mixtures of hexaalkylditin compounds, the reaction with electrogenerated silver ion was monitored amperometrically (324). Methods Involving Mercury. Amperometric end-point detection has 2R

been used in the coulometric titration of halide and other anions with mercury(I) (299). The biamperometric titration of chloride, bromide, and iodide (222) and of thiosulfate or thiourea (221) with H g ( N 0 3 ) ~has been carried out a t mercury electrodes. Mercury(1) and mercury(I1) in molten (Li,K)N03 have been coulometrically titrated with iodide a t Ag-AgI electrodes (192). Titration with EDTA a t a tantalum anode has been used to analyze binary mixtures of mercury with zinc, cadmium, or lead (341). Successive titration with EDTA and KI has been used for certain binary (341) and ternary (344) metal mixtures that contain mercury. The automatic amperometric titration of iodide with Hg(NO& has been described (275). Biamperometric end-point indication has been used in the coulometric titration of barbiturates with mercury(I1) (200). The stoichiometry of the reaction between Hg(ClO4)z and lithium acetylacetonate has been verified by amperometric titration (50). The coulometric amperometric titration of mercury(I1) in molten (Xa,K)SCN with sulfide has been reported (56). Microgram amounts of mercury(11) have been determined by amperometric extractive titration with dithizone (203) or sodium diethyldithiocarbamate (202). Mercury(1) has been titrated with dithizone (203). Mixtures of EtHgCl and HgC12 have been analyzed by R P E amperometric titration with ethylenethiourea (149). Submilligram amounts of mercury in organomercurials and proteins have been determined by digestion with "01HCIOa and titration a t pH 9.0 with bis(2-hydroxyethyl) d i t h i o c a r b a m a t e (81). ilmperometric titration has been used to study the complexation of mercury(I1) by dithioterephthalic acid (216). The successive titration with 8-mercaptoquinoline of mercury and silver, mercury, copper, and molybdenum, and several other mercurycontaining mixtures has been reported (302). Titration with PhHgOH has been used to determine sulfhydryl and disulfide groups in plant viruses (17). Calcium in pharmaceuticals such as the glycerophosphate has been determined by addition of EDTA-Hg complex and coulometric removal of the liberated mercury(I1) (94). The process was monitored by biamperometry a t silver electrodes. Methods Involving Lead. Lead acetate has been used to titrate nitrate in anhydrous AcOH (36), fatty acids in aqueous PrOH medium (SO), and sulfate in lake suspensions (99). Lead has been titrated with K2Cr04 to a n automatic amperometric end point (275), and with K2Cr207by second harmonic ac amperometry (74). Submillimolar concentrations of P b ( N 0 3 ) ~have been ti-


trated with (KH1)&1004 by the inverse polarographic technique (257). Thionine has been used as a photoredox indicator in the amperometric titration of lead with EDTA (251). A rotating tantalum electrode has been used for the successive titration of indium and lead with EDTA ($43). Indium is titrated a t pH 2 to 3 and 1.2 volt, then conditions are changed to pH 4.5 to 5.5 and +0.9 volt. Mixtures of bismuth, lead, and mercury have been successively titrated with EDTA and KI (344). Bismuth and lead in alloys with tin have been successively titrated with unithiol (300). Other reported titrations of lead are with sodium diethyldithiocarbamate (202), bis(6-aminoethy1)dithiocarbamic acid (59), and electrolytically generated propanethiol (181). Methods Involving Hexacyanoferrate(I1). Biamperometric titration with Ca2Fe(CN)6is one of the methods examined for the determination of potassium (144). Nanogram amounts of zinc have been biamperometrically titrated with electrolytically generated hexacyanoferrate(I1) (16). The effect of concentration on the composition of potassium zinc hexacyanoferrate precipitates has been studied amperometrically (211). Titration in tartrate medium has been used to determine zinc in the presence of impurities such as lead and iron (80). Gallium in the oxidation products of GaAs has been titrated with KaFe(CN)a a t a vibrating platinum electrode (262). The complexes formed by K4Fe(CN)6 and scandium or lanthanum in various supporting electrolytes have been studied amperometrically (267). Scandium can be titrated in the presence of calcium or lanthanum in 1M N a N 0 3 a t pH 2.5 to 3.5. The titrations with K4Fe(CN)6of uranium a t a D M E (118) and of nickel in alloys with iron by the biamperometric technique (240) have been described. Methods Involving Molybdenum and Tungsten Species. Vanadium(IV) has been amperometrically titrated with tripotassium aquo-tri-hydroxotetracyanomolybdate(1V) (132). Titration with a-benzoinoxime has been used to determine molybdenum in feldspar and glasses (298). Molybdenum in steel has been titrated with 8-mercaptoquinoline (282). Mixtures of molybdenum with iron or zirconium have been analyzed by titration with EDTA (9). Nicotine in the presence of limited amounts of pyridine has been titrated with the heteropoly-acid 0.5PzOs~6MoO3.6WO3(229). Millimolar concentrations of iron(II1) have been titrated with pIJazW04(249). The compositions of the hydroxycyanotungstates of copper, zinc, cobalt, and nickel have been studied by amperometric titration (133). Tungsten in binary alloys with

+

molybdenum has been titrated with 8-naphthoquinoline (%Oh).

Methods Involving EDTA or Anal-

ogous Reagents.

End-point indication in biamperometric titrations of bismuth, iron, and various other ions with E D T A has been provided by the addition of small amounts of t h e EDTA complexes with thallium(I), lead, or manganese (134). A thin layer of TlzOa, PbOz, or MnOz forms on the anode and the current increases when the titrant is in excess. The end points in the titration of microgram amounts of copper with triethylenetetramine (86) and of magnesium, calcium, strontium, or barium with EDTA, diethylenetriaminepentaacetic acid, or ethyleneglycol bis(p-aminoethyl ether) -N,N ,Ar ',"-tetraacetic acid (EGTA) (68) have been detected a t a mercury-coated R P E . The use of EGTA allows calcium to be titrated in the presence of a 1000-fold excess of magnesium. Thionine photoredox indication was used in the amperometric titration of copper, magnesium, or lead with EDTA (251). Microliter volumes of calcium solution have beetl biamperometrically titrated with EDTA (15). End-point indication in the biamperometric titrations of calcium and other ions with EDTA has been improved by the addition of a small amount of the EDTA complex of thallium(II1) (136). The determination of the hardness of water by biamperometric titration with EDTA has been explored (314). X platinumsilver amalgam electrode system has been used in the titration of calcium and magnesium in milk (287). A PbOl-plated platinum electrode has been used in the successive amperometric titration of calcium with EGTA and of magnesium with EDTA (117 ) . Amperometric titrations with EDTA a t a rotating tantalum electrode have been described in a n extensive series of papers. I n many cases, mixtures of metal ions were analyzed by titrating to successive end points after change of pH and of potential. Masking agents were used when necessary and sometimes titration with K I followed that with EDTA. Mixtures successively titrated include those containing magnesium, zinc, and bismuth (845), magnesium, cadmium, and bismuth (346), binary combinations of mercury and copper, zinc, cadmium, indium, lead, and bismuth (841), indium and cadmium (542), indium and lead (343), gallium and indium ($SO), gallium, indium, and cadmium (SSS), gallium, bismuth, and copper (382), binary and ternary combinations of thallium and silver, zinc, and lead ( S S I ) , or of zirconium and copper, magnesium, zinc, indium, lead, thorium, iron, and nickel (138), binary combinations containing molybdenum (9), and ternary combina-

tions of bismuth, mercury, and copper, zinc, or lead (344). Single-metal titrations include those of gallium (989), hafnium (8),and nickel (334). A standard deviation of only 0.002270 has been reported in the titration of EDTA (disodium salt) with electrogenerated zinc ion (78). The use of oxalate as a masking agent in the titration of zinc, cadmium, and manganese with EDTA has been described ($09). Biamperometric titrations with EDTA include those of bismuth (313) or iron and aluminum (317) in silicates, iron in rocks (185, 278), iron in acid solutions a t glassy carbon electrodes (316), and manganese with KaFe(CK)B as amperometric indicator (145). Manganese has also been titrated a t a n amalgamated silver or a platinum electrode (146). Uncombined iron in transformer and other oils has been titrated in H2S04iso-PrOH a t the R P E (104). The automatic titration of nickel a t a D M E has been reported (276).

Methods Involving Other Organic Compounds. Amperometric titrimetry has been used to show that the maximum metal: ligand ratio in the neptuniuin(VI)-propionate complexes is 1 : 3 (225). Precipitation from EtOH with oxalic acid, the excess of which is titrated a t a D M E with Cd(No~)p,has been used to determine sodium or potassium salts (172). Direct titration to form oxalates, citrates, or tartrates has been used to determine lanthanum, gadolinium, and terbium (168). Dialkyltin compounds have been determined by titration with oxalic acid (111). The oxalate and malonate complexes of iron(II1) (101), the tartrate and citrate complexes of vanadium(II1) and vanadium(1V) (297), and the succinate complexes of neptunium(V1) (224)have been studied by amperometric titration. Oxalate precipitation from iso-PrOH has been applied to the determination of sodium and potassium (59), magnesium, calcium, strontium, and barium (37, 38, 40), and nickel and cobalt (37). Clathrate formation by polyvinyl alcohol has been studied by amperometric titration with iodine (56). The titration of triethylaluminum and of diethylaluminum iodide with BuzO, dioxan, or tetrahydrofuran has been examined (184). Copper in copper-base alloys has been determined by amperometric titration in "3-NaOH medium with sodium picrate (201). Aromatic nitro acids, alizarinsulfonic acid, and heavy metal salts have been used as titrants for alkaloids (167). Gold and palladium have been titrated with benzidine a t a platinum or a graphite anode (309). The latter gives more accurate results. A graphite anode has also been used in the titration of titanium, zirconium (89), and niobium (88) with N-benzoyl-otolylhydroxylamine, or of niobium with N-cinnamoylphenylhydroxylamine

(87), of zirconium with N-furoylphenylhydroxylamine (90), or hydroxyphenyliminodiaoetic acid (SIO),and of Alimrin Red S with salts such as AlS(SO& or CuSOd (19). Niobium has also been titrated with Xylenol orange ($96). Nickel has been titrated with o-hydroxyacetophenone oxime (227') or 2,Sdihydroxyacetophenone oxime (110). Molybdenum in feldspar and optical glass has been determined by titration with a-benzoin oxime (298). The lowfrequency titration of palladium with pfurfuraldoxime has been reported (49). Submicrogram amounts of germanium have been titrated with diantipyrinylmethane (179). Complex formation between copper(I1) and phlorein has been studied by amperometric titration (170). Copper in leaded brass has been determined by titration with 1,2,3benzotriazole (226). The titration of palladium with N-p-tolylsulfonyl-2benzofurancarboxamide has been studied (182). Tungsten in alloys has been determined by titration with p-naphthoquinoline in the presence of KI (204). The coulometric titration of copper with propanethiol has been monitored a t a DAME (181). Copper in the presence of a 1000-fold escess of zinc, thallium(I), iron(II), cobalt, or nickel has been titrated with thioacet'amide (233). Amperometric and biamperometric titrimetry has been used to study the reaction between palladium and thioglycollic acid (306). Milligram quantities of nickel or cobalt in aqueous EtOH have been titrated with ethyl xanthate (72). Titration with thioglycollic acid anilide has been used to determine cobalt in the presence of nickel and zinc (52). Sodium diethyldithiocarbamate has been used as titrant for zinc after chromatographic separation from aluminum (248) and for microgram amount's of metals such as copper and cadmiurn by the extractive technique (202). The amperometric extractive technique has also been applied to the titration of cadmium or palladium with dithizone (203). A graphite anode has been used in amperometric titrations of gold in alloys with potassium bis(2-hydrosyethy1)dithiocarbamate (93) or phenylsulfonylthiobenzamide ( S o l ) , in electroplating baths with benzyldithiocarbamate (SO$), in ores with thiosalicylic acid (285), and in mixtures with tellurium with derivatives of 2,6-dimercaptothiopyran-4-one (312). The successive titration of gold and selenium has been carried out with the 3-pyridyl derivative, while titration with the 3-methyl-5-phenyl derivative has been used to determine selenium and tellurium in semiconductor alloys (24, 312). Amperometric titrations that involve cadmium and dithioterephthalic acid (216), methyldithioburet (70) or his(@-aminoethy1)dithiocarbamic acid (69), have been described. Kickel has been titrated with either of the latter two


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reagents (69, 70). Mixtures of copper and cadmium or nickel have been analyzed by titration under conditions where the cathodic current of copper and the anodic current of methyldithioburet are obtained (70). The reactions of 2,3quinoxalinedithiol with copper(1) and copper(I1) have been studied and applied to the amperometric titration of copper in ores (61). Various derivatives of 2,6dimercaptothiopyran-4one have been used to titrate arsenic, to determine it in iron and steel (79), and to determine selenium in ores ( 2 2 ) . Methyldithioburet has been used to titrate thallium(I), bismuth, selenium, tellurium, and cobalt (69). Selenium in semiconductor and other selenium-containing materials has been titrated with pyridyldimercaptothiopyrone or the dipropyl derivative (23). The simultaneous determination of selenium and tellurium by amperometric titration with 8-mercaptoquinoline is the subject of a patent (326). This titrant has also been used for gallium or indium (325)and in the analysis of ferrous alloys to determine vanadium, copper, molybdenum, and iron (282). Palladium in plating baths has been titrated with 2,6-dimercapto-3methylthiopyran - 4 - one (21). Palladium has also been determined by the titration of selenophen-2-aldoxime (27). Sodium tetraphenylborate has been used to titrate N,N-substituted guanidines (281) and compounds such as pethidine in pharmaceutical preparations (319). The effect of foreign ions on the titration of nitrate with diphenylthallium(II1) sulfate has been studied (76). I n a study of HCN as a ligand towards copper(1) and silver(1) in liquid HCN, analyses for hexafluorophosphate were performed amperometrically (76). Miscellaneous Titrations. After the addition of isoquinoline, azide has been titrated with Cu(N03)~(236) and copper, cadmium, or nickel has been titrated with KSCN (236). Titration with Cd(N03)2 to precipitate CdClz or CdBrz from anhydrous AcOH has been used to determine chloride or bromide (36). Zinc and cadmium in molten (Na,K)SCN has been titrated with electrogenerated sulfide (56). Biamperometric titration with ZnSO4 has been used in the determination of sulfide, antimony, and mercury in solutions of mercury-antimony ores (246). The amperometric titration with fluoride of aluminum and beryllium in D M F has been reported (91). Submilligram amounts of aluminum have been determined with NaF as reagent, Th(C104)4 as titrant, and FeC13 as amperometric indicatcjr (43). The formation and composition of thorium arsenates (243) and lanthanum arsenites (244) have been studied by amperometric titration. Titanium in the presence of EDTA has been titrated both amperometrically 4R

and

biamperometrically with

HnOS

(161)a

Copper(I1) and bismuth(II1) in molten (Li,K)NOa have been titrated with electrogenerated iodide (198). Gold(II1) (286), cadmium in alloys with zinc (w),and bismuth in the presence of diantipyrylmethylmethane or diantipyrylpropylmethane (61) o t of isoquinoline and HCOOH (834), have been titrated with KI. Milligram amounts of uranium(V1) have been titrated with NazTeO3 (71). Triphosphate has been titrated in 30- 50% EtOH with tris-(ethylenediamine)cobalt(III) chloride (212). Precipitation is not instantaneous, so that titration must be slow. Pyrophosphate has been determined in the presence of orthophosphate and tripolyphosphate by titration with Cd(NO& (264). The uses in amperometry of heteropolyacids of elements such as phosphorus and silicon have been discussed (228). OXIDATION-REDUCTION REACTIONS

Methods Involving Iron. The biamperometric titration of iron(I1) and of hexacyanoferrate(I1) with Pb(0Ac)r is reported to be more sensitive and more reproducible than potentiometric ti tration (4). The effects of the presence of iron(III), chromium(III), and &Po4 (263),electrode pretreatment (139), and factors such as applied emf and supporting solution (231) on the titration of vanadium(V) with iron(I1) have been studied. The same titrant has been used to determine vanadium in VZOS (266), shales (146), catalysts (158), and steels (262). Daylight is reported to affect the results of the amperometric titration of K2Cr207with iron(I1) in HCI (196). Titration in H z S O ~or H3P04is recommended. Amperometric titration with electrogenerated iron(I1) has been used for the high-precision assay of K2Cr207 (57, 322) and the determination of chromium in biological materials (83). Reserpine in pharmaceutical preparations has been determined by addition of excess K2CrzO7and biamperometric back titration with Fe(NH4)2(S04)2 (Mohr's salt) (112). Bivalent and total iron in ores has been determined by titrating first with K2Cr207and then with NazS~03after introduction of CuS04 (45). Addition of iron(I1) and back titration with K2Cr207 has been used to determine quinoid groups in humic acids (97). Titration with Mohr's salt has been used to determine manganese, chromium, and vanadium in silicate rocks (25) and in steel (127), uranium in nuclear fuels (290), and the 0xygen:uranium ratio in hyperstoichiometric uranium dioxide (289). A platinum electrode gave better results than a graphite one in the titration of uranium(V1) with iron(I1) (92). Slightly high results obtained in the amperometric titration of pluto-


nium(V1) with iron(I1) have been attributed to the probable formation of small amounts of H z O ~at the platinum anode (18). Submillimolar concentrations of iron(I1) in stirred solutions have been titrated with KMn04 (856). Hypochlorite has been titrated with electrogenerated iron(I1) (107). Iron(I1) in waste water has been biamperometrically titrated with electrogenerated bromine (166). Iron(I1) and hexacyanoferrate(I1) have been titrated with K I 0 4 (142) or hexamminecobalt(II1)-tricarbonatocobaltate (143). The biamperometric titration of submillimolar concentrations of iron(II1) or hexacyanoferrate (111) with mercury (I) (193) and the sources of error in the titration of hexacyanoferrate(II1) in alkaline iodide medium (272) have been examined. Total iron in iron ores has been determined by oxidation to iron(111) and biamperometric titration a t carbon electrodes with SnC12 (46),or a t platinum electrodes with ascorbic acid (44). Titration with electrogenerated chromium(I1) has been used t o determine copper and iron in cadmium metal (156). The amperometric (338) and biamperometric (810) titrations of hexacyanoferrate(II1) with H202 have been examined. Ferrocene in rubber (261), cobalt in cobalt-60 preparations (B), and potassium after precipitation as cobaltinitrite (144) have been determined by titration with K3Fe(CN)6. Nonferrous Methods Involving Cerium, Titanium, Vanadium, Chromium, and Manganese. The R P E titration of submillimolar concentrations of cerium(1V) with mercury(1) has been reported (194). Titration of cerium(1V) with arsenic(II1) has been found to be more selective than titration with hexacyanoferrate (11), hydroquinone, or ascorbic acid (336). Cerium(1V) has also been titrated with electrogenerated vandium(1V) (29) and with H202 (210, 338) or NaNO2 (339). Cerium(IV) has been used to titrate arsenic(II1) (10, 263), antimony(II1) (253),H202 or T\TaN02(340), Na2S203in the presence of 2-3 mg of K I (337), a-tocopherol and mixed tocopherol concentrates (67),and phenothiazine derivatives (217, 220). Cerium(II1) has been titrated with electrogenerated molybdenum(V) (65) or chromium(V1) (166). Mixtures of cerium(1V) and chlorate have been titrated with titanium(II1) by the reaction-step coulometric technique (109). Electrogenerated titanium(II1) has been used to titrate chlorate (107) and mixtures of hypochlorite and chlorate (109). A survey has been made of the analytical applications of phenothiazine derivatives, including the amperometric determination of titanium and tin (33). The reduction of vanadjum(V) to vanadium(1V) by amperometric titration with 2,4-dithioburet has been used to determine vanadium in ferrous alloys

and slags (979). Vanadium(1V) has with KBr03 has been used t o determine been titrated with chromium(V1) that arsenic in oxidation products of gallium was generated in H3P04 medium (156), arsenide (269), amethocaine hydrowith iodine (254), and with P ~ ( O A C ) ~ chloride (41), and sulfenamides (162). (4). Tungsten-tungsten or tungsten Sulfenamides have also been titrated anode-platinum cathode polarized elecwith bromine in bleOH (160) or in AcOH (161). Titration with Hg2(No3)2 trodes are recommended for the titraafter the successive addition of KBr and tion of molybdenum(V1) with VCl2 or Hg(SO& has been used to determine CrC12 (207). chlorine and hypochlorite jn water The titration of K~Cr207with H202has been performed amperometrically (338) (984). and biamperometrically (210). Iodide Several biamperometric titrations with electrolytically generated bromine (197) and H202(340) have been amperometrically titrated with K2Cr207. Elechave been reported. Arsenic in nontrogenerated chromium(V1) has been ferrous metals has been automatically used to titrate europium in misch metal titrated (17 3 ) . Cholesterol in serum after reduction to europium(I1) (154), has been separated by TLC, then overarsenic(II1) after the addition of K I titrated with bromine. After addition (12), atid manganese in brass by use of of Xs203, the excess is back titrated H3P04medium (156). (294). Phenol in waste water has been Manganese in Armco iron has been determined automatically (276). Compounds such as sulfonamides and local determined by biamperometric titration as manganese(VI1) with externally anesthetics have been determined by electrogenerat~ed vanadium(1V) (29). bromination (96). Compounds that The titration of I(>1nO4 with HZ02 (338) react slowly are overtitrated, then suland the determination of man,(vanese fanilic acid is added and the titration is iii alloy steels by treatment with continued to the combined end point (xH4)&08 and titration with Na2S203 (95). Isoniazid (274), procarbazine (54) have been reported. Submicro(31) ] tetraalkylammonium iodides and gram quantities of manganese in iron choline iodide benzilate ( l 6 4 ) , suxahave beeti titrated with electrogenerated methonium iodide and subecholine silver(I1) (292). Techiiiques for the (165), cysteine (163),cysteamine (273), titration without applied emf of manand nitrogen-substituted phenothiazine derivatives (218) have been all couloganese(I1) with K M n 0 4 ,of KMnOc with NalJO,, (195),and the determination of metrically titrated to a biamperometric manganese in alloy steels by biamperoend point. Semiautomatic titration has mctric titratioii in ?;a$207 with KMn04 been used t o determine sulfur in com(84) have been described. Addition of pounds such as tin mercaptides (287) and bromine numbers for di- and triescess KMii04 and back titration in methylsilyl ethers (147). Na4p201 with llnSOa has beeti used to determine HCOOH in technical -4cOH The titration of cyanide, arsenic, and other substances with electrogenerated (304). Dissolved osygen has been determined by monitoring the anodic hypobromite has been discussed (215). dissolution current of thallium during Microamounts of hydrogen in steels and titration with lInS04 (256). Tin(II), other metals have been determined by nitrite, ascorbic acid, glycerol, and hot extraction with argon, oxidation to various other substances a t low concenH20, treatment with NaKH,, and bitrations in stirred solutions have been amperometric titration of the resulting titrated with E(hftiO4 (255). The NH3 with electrogenerated hypobromite E(11n04titrations of H204(340),arsenic(320). Mixtures of hydrazine and K H 3 (111) in the presence of K I (IO),hydrahave been analyzed by titrating the zine sulfate (335),and hydrazine derivahydrazine in acid solution and then tives (305)have beeti described. Oxalic titrat'ing NH3 a t a p H of 8.2 to 8.5 (242). acid has been titrated with KMnOa by Hypobromite has also been used to the low-frequency technique (49). N titrate numerous aliphatic amines (64), substituted phenothiazines have been various constituents of e-caprolactam biamperometrically titrated with electroamination products (206), l-aminogenerated manganese(II1) (219). adamantane (283), and thiocyanate, Methods Involving Chlorine or Bromercaptoacetic acid, and fi-mercaptomine. Hypochlorite in dichromate propionic acid (214). Cholesterol has been titrated in nonaqueous medium liquors has been biamperometrically titrated with K I after neutralization with N-bromosuccinimide (293). and addition of N a H C 0 3 (186). Methods Involving Iodine. CopStrychnine has been determined by addiper(I1) and bismuth(II1) in molten tion of excess Rejnecke salt and back (Li,K)N03 have been biamperometrititration with electrogenerated chlorine cally titrated with electrogenerated iodide (137). Submilligram quantities of (192). The analytical uses of electrocinnamic acid have been titrated with generated iodine species have been diselectrogenerated I3rC1 (42). Comcussed (180,215). Titration of arsenate pounds such as aniline, glycerol, and has been used to assess the precision of thiourea have been titrated in LIeOHan automatic titrator (299). VanadiumAcOH with bromine (171). Titration (IV), nickel in the presence of dimethyl-

glyoxime, and ascorbic acid have been amperometrically titrated with iodine (254). Biamperometric titration with iodine has been used for sulfite determination in gelatin (191) and, with electrolytically generated iodine, for the determination of tin in metals such as Zircaloy (SA'S), H,S from the decomposition of organic samples (268),and microgram amounts of cysteine (163). The biamperometric titration of submillimolar concentrations of iodine with Hg2(C104)2 has been examined (193). A platinum- graphite electrode system has been used in the titration of iodine with Ka282O3, arsenic(II1) , or ascorbic acid (232). Titration of iodine with Na.26203 has been used to det,ermine tellurium(1V) in tellurite-tellurate compounds (66), micro amounts of bromate (126), and organic hydroperoxides (62, 260). Titration of iodine released from iodate-iodide niisture has been used to determine hydrogen ion produced by the hydrolysis of compounds such as hlCl3 (98). Selenium in industrial products such as converter dust has been determined by addition of either hydrazine and back titration with iodine, or of K I and titration of iodine with hydrazine (388). Tellurium in technical samples has been determined by reduction to tellurium(IV), addition of excess iodine, and back titration with hydrazine (151). -4ddition of iodine and back titration with arseiiic(II1) after standing has been used to determine H3P03(311 ) . I n a tentative method for continuously monitoring atmospheric oxidants, liberated iodine is electrolytically reconverted to iodide (280). The barbiturate Ipronal has been determined by oxidation with bromine and iodimetric determination of the excess oxidant (136). Oxidizable substances such as arsenic(111) and hydroquinone have been titrated with KIO4 (142). Mannitol, glycerol, and threonine were determined by addition of excess KIO4 and back titration with arsenic(II1) after standing, Biamperometry has been used in the microdetermination of molybdenum by its catalysis of iodine liberation (247, 295). The catalytic effect of ruthenium(1V) on the iodide-HtOz reaction has been studied ( 1 4 ) . Interest in water determination by the biamperometric Karl Fischer technique has continued. Various automat'ic titrators have been developed for this technique (106, 116, 129, 188, 245, 270). Typical examples of the determination of water are in HaPo4 (129), C6& and other organic liquids (48, 150, ~ 4 1 , 2 7 0acetaldehyde )~ (288),and gases such as SZand Freons (205). Bound water in rocks has been determined by heating, carrying off the water in a gas stream, and titrating (174). Other Reactions. 2,3-&uinoxalinedithiol undergoes a redos reaction with copper(I1) and has been used to


5R

titrate copper in ores (61). The biamperometric titration of submillimolar concentrations of copper(I1) in KSCN-KI medium with Hg2(C104)2has been described (195). Molybdenum in alloy steels has been titrated at a platinum- tungsten electrode system with electrogenerated tin(I1) (3). The RPE titration of thallium(II1) with unithiol has been reported (265) and is featured in a patent (213). Thallium(I11) has also been titrated with 8-mercaptoquinoline (326) and 4-methyl-8-mercaptoquinoline (32), Hydrazine sulfate in NaHC03-KI medium has been titrated Hydroquinone, with T I Q ( S O ~ )(536). ~ resorcinol, and metol have been biamperometrically titrated with Pb(OAC)~(5). The electrogeneration of this titrant has been studied (6) and used to titrate compounds such as thionalide ( 7 ) . The amperometric titration of NaNO2 (338) and the biamperometric titration of arsenite or sulfite (210) with H202have been described. Hexamminecobalt(II1) tricarbonatocobaltate has been used to titrate numerous substances, including arsenic(II1) , oxalate, and H202(143). The DME titration with oxygen of a nickel(1) cyclic amine complex in hleCN has been used to study this unusual reaction (308). Nitrite has been determined by using it to titrate ascorbic acid in 5N H2S04 a t the RPE potential of +1.0 volt (11). Similar conditions have been used for the titration of hydrazine or sulfamic acid with N a N 0 2 (339). The biamperometric titration of isopropyl N-phenylcarbamate (169), and the amperometric or biamperometric titration of aniline, sulfanilic acid (189), primary amines such as aminophenols (190) and vitamins B1 and B6 ( f ) , with NaN02 have been reported. Biamperometry a t mercury electrodes has been used in the determination of uranium(V1) by the new technique controlled potential coulometric titration (1‘76). The formation and amperometric titration of a product such as a hydroperoxide has been used in a patented method for the analysis of ozone (68). Precise coulometric titration t o a biamperometric end point has been used to standardize solutions of NaAsOz (322). LITERATURE CITED

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Biochemical Analysis Morton K. Schwartz, Department of Biochemistry, Memorial Hospital for Cancer and Allied Diseases; and Division of Biochemistry, Sloan-Kettering Institute for Cancer Research, New York, N. Y. 7 002 7

T

H I S Rl,:VIl,;JV WILL COVh;R developments ill the area of biochemical annlyais during the period from January 1968 through December 1971. It would be presumptuous for any reviewer to claim that he intends to completely cover all of the publications in this dynamic area. As pointed out by the last reviewer in this series ( I n ) , the large volume of pertinent reports encompasses journals in chemistry, biology, physics, electronics, and engineering. Today journals in medicine and computer and nuclear science, as well as in instrumentation must be included. There are literally thousands of references that have appeared during the four-year period of this report. The enormity of the assignment is empha-

sized by the fact that each of the bimonthly Biochemical Methods Sections o j Chemical Abstracts contains over 100 entries and the Journal of Lipid Research, which maintains a cumulative monthly listing of pertinent references to lipid methods, had accumulated 346 references in this limited area through the first eleven months of 1971 ( 5 A ) . It is mandatory that this review be selective rather than comprehensive and precludes incorporation of routine applications or minor modifications of accepted techniques or methods. This reviewer will attempt to cover the subgroupings included in previous reviews of this same title and to emphasize new developments in biochemical analysis with par-

ticular reference to those areas of interest to the writer. Limited reference will be made to the areas of biochemical methodology considered in other reviews in this series. These include clinical chemistry (SA, 4 A ) , fluorescent analysis (6=1), chromatography ( 7 A ) , and the use of enzymes in analytical chemistry (,%?A). NEW BOOKS AND JOURNALS

Of general interest is a Handbook of Biochemistry containing a vast amount of biochemical data (126B). There have been numerous volumes published in continuing series, each devoted to specific areas of biochemistry. The Methods of Biochemical Analysis series continues to present excellent and thor-


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Amperometric titrations - Analytical Chemistry (ACS Publications)

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