Anal. Chem. 1986, 58, 144R-152R (4FT) Berthoud, T.; Camus, P.; Drin, N.; Stehle, J. L. J . Phys . Colloq . 1983, 389-91. (5FT) Bykov, I.V.; Skvortsov, A. 6.; Tatsii, Y. G.; Chekalin, N. V. J . Phys. Colloq. 1983, 345-52. (6FT) Camus, P. J . Phys. Colloq. 1983, 87-106. (7FT) Corornlnas, L. F.; Navarro, r. A.; Lopez, R . J. J . Assoc. Off. Anal. Chem. 1984, 65, 888-9. (EFT) Evans, W. H.; Read, J. I. Analyst 1985, 1 IO, 619-23. (9FT) Foner, H. A. Analyst 1984, 109, 1469-74. (10FT) Ivanov, P. Pochvozn. Agrokhim. 1984, 19,88-98. (11FT) Hall, J. E.; Green, R . B. Anal. Chem. 1985, 5 7 , 431-5. (12FT) Hovis, F. E.; Gelbwachs, J. A. Anal. Chem. 1984, 5 6 , 1392-94. (13FT) Kachin, S.;Smith, B. W.; Windfordner, J. 0. Appl. Spectrosc. 1985, 39,587-90. (14FT) Kuzyakov, Y. Y.; Zorov, N. B.;Chaplygin, V. I.; Novodvorskii, 0. A. J . Phys. Colloq. 1983, 335-43. (15FT) Larkins, P. L. Anal. Chim. Acta 1985, 173, 77-87. (16FT) Luo, G. Fenxi Huaxue 1984, 12, 236-9. Chem. Abstr. 101, 162775n. (17FT) MacDonald, J. R.; Llnd, R. C.; Sipes, I.G.; Gandolfl, A. J. J . Anal. Toxicol. 1984, 8 , 155-7. (18FT) Messman, J. D.; Schmidt, N. E.; Parll, J. D.; Green, R. B. Appl. Spectrosc. 1985, 39,504-7. (19FT) Omenetto, N.; Berthoud, T.; Cavaili, P.; Rossi, G. Anal. Chem. 1985, 5 7 , 1256-61. (20FT) Omenetto, N.; Human, H. G. C.; Cavalli, P.; Rossi, G. Analyst 1984, 109,1067-70. (21FT) Pillai, C. K.; Natarajan, S.; Venkateswariu, C. At. Spectrosc. 1985, 6 ,53-6. (22FT) Rigin, V. I.Zh. Anal. Khim. 1984, 39,648-53. Chem. Abstr. 101, 83103~. (23FT) Shahwan, G. J.; Helthmar, E. M. Spectrosc. Lett. 1984, 17, 377-88. (24FT) Sthapit, P. R.; Ottaway, J. M.; Fell, G. S. Analyst 1984, 109,1061-5. (25FT) Sthapit, P. R.; Ottaway, J. M.; Fell, G. S . Anal. Proc. 1983, 2 0 , 599-602.
0. TECHNIOUE COMPARISONS
(1G) Bruce, R . C.; Lyons, D. J . Commun. Soil Sci. Plant Anal. 1984, 15, 15-21. (2G) Fogh-Andersen, N.;Wimberley, P. D.;Thode, J.; Siggaard-Andersen, 0. Clln. Chem. 1984, 3 0 , 433-6. (3G) Harrington, D. E.; Jones, J. S.;Bramstedt, W. R.; King, T. A. At. Spectrosc. 1983, 4 , 171-6. (4G) Heinrich, R.; Angerer, J. Int. J . Environ. Anal. Chem. 1984, 16, 305-14. (5G) Howanitz, J. H.; Okner, J.; Winkelman, J. W. J . Clin. Lab. Autom. 1984, 4 , 125-8. (6G) Jones, K. C.;Peterson, P. J.; Davies, B. E.; Minski, M. J. I n t . J . Environ. Anal. Chem. 1985, 21, 23-32. (7G) Kaegier, S. H. Erdoel Kohle, Erdgas, Petrochem. 1984, 37, 563-7. (8G) King, A. D.; Hiillgoss, D. R.; Wallace. G. F. At. Spectrosc. 1984, 5 , 189-9 1. (9G) Kreeftenberg, H. G.; Koopman, B. J.; Huizenga, J. R.; Van Vllsteren, T.; Wolthers, B. G.; Gips, C. H. Clin, Chim. Acta 1984, 144, 255-62. (10G) Lajunen, L. H. J.; Kinnunen, A.; Yrjankeikki, E. At. Spectrosc. 1985, 6 , 49-52. (11G) Liem, I.; Kaiser, G.; Sager, M.; Toelg, G. Anal. Chim. Acta 1984, 158, 179-97. (12G) Lin, S. W.; Julshamn, K. Anal. Chim. Acta 1984, 758, 199-206. (13G) Locatelli, Ciinio; Fagioii, F.; Blghl, C.; Landi, S.; Garai, T. Ann. Chim. 1984, 74, 521-35. 14G) Novozamsky, I.; Van Eck. R.; Houba, V. J. G. Commun. Soil Sci. Plant Anal. 1984, 15, 205-11. 15G) Salbu, 6.; Bjoernstad, H. E.; Lindstroem, N. S.;Brevik, E. M.; Rambaek, J. p.; Englund, J. 0.; Meyer, K. F . ; Hovind, H.; Paus, P. E.; et al. Anal. Chim. Acta 1985, 167, 161-70. 16G) Su, Y. S.;Burdo, R. A.; Strzegowski, W. R. Mikrochim. Acta 1984, 1 , 321-31. 17G) Worth, H. G. J. Ann. Clin. Biochem. 1985, 22, 343-50.
Organic Elemental Analysis T.S . Ma* Department of Chemistry, City University of New York, Brooklyn, New York 11210
C. Y. Wang
Department of Chemistry, Yunnan University, Kunming, Yunnan, China
This review is a continuation of the previous one ( 1 ) and covers the period from October 1983 to September 1985. During this period the authors found more than 600 articles that are concerned with the determination of one or more of the elements present in certain organic material. Over 90% of the publications deals with samples of complex nature. While no new apparatus was proposed, many papers reported on the evaluation or modification of analytical procedures using the existing equipment (2), as well as the comparision of various methods for the determination of a single element or simultaneous determination of several elements.
CARBON, HYDROGEN, NITROGEN Computerization of carbon, hydrogen, and nitrogen determinations using the automated apparatus has become a general practice in analytical laboratories where large numbers of samples are processed daily. Bramstedt et al. (3)reported on the statistical evaluation of the data and found that operator error was not a major factor in the total random errors; they also put forward a closed-loop system based on a Perkin-Elmer CHN analyzer, including elsctronic weighing and transfer of samples from a Mettler balance and preparation of formalized reports (4). Pella et al. (5) proposed calibration equations to improve accuracy using the Carlo Erba analyzer. Honma et al. (6) described a modified device for mixing the combustion products in the differential thermal conductivity method for CHN determination. Waskowski et al. (7) proposed an automatic adapter for the combustion of 0.3-0.9 mg samples. 144 R
0003-2700/86/0358-144R$01.50/0
For the determination of carbon and hydrogen in fluoro compounds, Lu (8)recommended an external absorption tube packed with silica gel-La(NO& to eliminate interferences. For the retention of Pz05in the analysis of organophosphorus compounds, Binkowski et al. (9)found that silver-impregnated pumice is the most effective reagent. For the combustion of organic peroxides, Buzlanova et al. (10) mixed the sample with quartz sand and carried out the pyrolysis under carefully controlled conditions. Lilliott et al. (11)analyzed explosive powders by a modified Dumas method in which the sample, after extraction of added solvents with methanol, is burnt in COz-Oz (8:3 v/v), using the Mettler-Heraeus nitrogen analyzer. Kirsten et al. (12) modified a Carlo Erba analyzer for high-capacity Dumas determination: approximately 100 analyses per working day can be carried out and a further 100 samples can be analyzed automatically overnight. Waskowski et al. (13) and Vecera et al. (14) investigated the gas chromatographic finish after Pregi-Dumas combustion. Dubinskii et al. (15)recommended adding an alcoholic solution of polysiloxane into the 50% KOH solution in the azotometer to prevent foaming. Zigel et al. (16) compared three methods of determining nitrogen in N-vinylpyrroridinone and its copolymers and found that the Dumas method gave results higher than theoretical values whiie Kjeldahl and automated CHN methods gave results lower than theoretical values; increasing the digestion time in the Kjeldahl procedure to 90 min gave the correct results. Haraguchi et al. (17) tested various digestion procedures to determine cimetidine by the Kjeldahl method 0 1986 American Chemical Society
ORGANIC ELEMENTAL ANALYSIS
Br- and I-, respectively, by means of NH,V03, and titrated the halides potentiometrically with 0.2 M AgNO,; Wolfbeis e t al. (26) determined the halides by a fluorometric method, which is based on the quenching of the fluorescence of quinine or acridine. Aliphatic chloro and iodo compounds can be converted to the halides by means of potassium formate, which is produced upon heating the sample dissolved in dimethylformamide with KOH (27). For the determination of fluorine, Gelman e t al. (28)sealed the sample in a polyethylene container that was wrapped in aper impregnated with K N 0 3 and burned it in the comustion flask containing water as the absorbent; the F- produced was titrated with 10 mM L a ( N 0 by means of a Fselective electrode. Kissa (29) also used the F- electrode to determine fluorine after decomposition with an oxyhydrogen torch.
! '
OTHER ELEMENTS C. V. Wanp (Wang G4kwq-n u Wang ChangYI) was Lwn In 1938 h Kurmlng. Yunnan Rwhw. Chlna. He s W a1 me
and reported that the beat resulta were obtained by hydrolysis of the cyano group before digestion with H2S0,. Treybig e t al. (18) achieved accurate determination of aliphatic amines using selenium as digestion aid, but the method was unsatisfactory for cyclic or aromatic amines. According to HjalmarssOn e t al. (19).the automatic Kjeldahl analyzer performs 30 determinations per hour with accuracy and precision equal to that of the conventional manual method.
OXYGEN, SULFUR, HALOGENS Frigge (20) determined oxygen by placing the sample in a platinum boat and pyrolyzing it in a stream of nitrogen; the resulting gases were conducted through granular carbon at 1120 "C and the CO produced was measured with a nondispersive infrared detector. Kopycki e t al. (21) found that low results in the pyrolysis of compounds containing P==O bonds can be remedied by adding hydrogen to the nitrogen or by inserting tungsten metal pieces into the carbon packing. Farina-Mazzeo et al. (22) studied the determination of oxygen in organometallic compounds using commercial elemental analyzers; addition of AgCI-NH,CI-hexamine (22:l)to the sample using the Perkin-Elmer analyzer. or addition of AgCl to the sample and use of helium containing 5 % of hydrogen as the carrier gas in the Carlo Erba analyzer gave correct oxygen values for compounds of Bi, Cd, Cu, Fe, Mo, Ni, Pb. Se. V, Ba, Ca, La, Mg, Mn, or Sr, but not for compounds of AI. Yu e t al. (23)decomposed sulfur compounds in a 500-mL cumbustion h k containing 15 mL of aqueous 30% H202;the sulfate was precipitated with 10 mM barium acetate and, after filtration, the filtrate was titrated with 0.1 M sodium tetraphenylborate potentiometrically using a tetraphenylborateion-selective or a AgzS electrode. Farroha e t al. (24) determined milligram amounts of sulfur in hydrocarbons by converting the sulfur quantitatively into S20,2- by heating the sample with Na,SO,; the S,032-was then titrated coulometrically with iodine generated from KI Burns et al. (25)decomposed halogenated compounds by closed-flask Combustion, converted the Br03- and 10, into
Wang e t al. (30) studied the optimum conditions for determining phosphorus in organic phosphates and phosphonates by molecular emission cavity analysis, covering such factors as the flow rates of hydrogen and air and horizontal positioning of the cavity in the flame. Pang e t al. (31) decomposed arsenic compounds by digestion in "0,-H,S04-HCIO,; the product was reduced by CuCl and, after extraction with benzene, the arsenic was determined hy automatic coulometric titration. Lu et al. (32) determined bismuth in pharmaceuticals by ac oseillopolarographic titration of B?+ with 0.02 M EDTA using a hanging-mercury-drop or mercury-film indicator electrode. For the decomposition of refractory boron compounds by the closed-flask technique, Xie et al. (33)added anhydrous Na&03 or Na&O, in order to form Na,B,O,, which is converted to H,BO in dilute acid solution. Wang e t al. (34) determined the Bb,3- by potentiometric titration using a BF,- selective electrode. Tytchinskaya e t al. (35)fused organosilsesquioxanes with Na20, in a crucible and determined the resulting silicate spectrophotometrically as the blue silicomolybdate. Burns e t al. (36) utilized the direct carbon furnace atomization method to determine aluminum in aluminum oxides and carboxylates. Selig (37) determined aluminum in explosives by potentiometric titration with 0.5 M NaF, using a F- selective electrode. Davydova e t al. (38) decomposed organocopper compounds by heating with H2S04-HN0,, and titrated the Cu2+potentiometrically with 10 mM Na,EDTA using a Cu2+selective electrode. Brwier et al. (39) determined iron in ferrocene and its derivatives by flameless atomic absorption spectrometry. A collaborative study of the determination of iron in chelates by atomic absorption spectrometry has been published (40). Farroha e t al. (41) determined milligram amounts of organolead in petroleum by digestion with HNO~;H,O,-HCIO, and titration with 0.2 mM Na,MoO, using a P b selective electrode. Diehl e t al. (42) determined lead in tetraalkyllead compounds by atomic absorption spectrometry. Campiglio (43) decomposed organonickel compounds by closed flask combustion; oxides of nickel deposited on the walls of the tlask were dissolved by boiling, and Ni2+ was determined by titration with 0.01 M sodium diethyldithiocarbamate potentiometrically using a S2-selective electrode.
SIMULTANEOUS DETERMINATION OF MAJOR ELEMENTS Sullivan e t al. described two methods for the simultaneous determination of several elements using the combustion-gas chromatography combination technique. In one method (44) the sample is pyrolyzed in a hydrogen-helium atmosphere a t high temperature in the presence of a catalyst, whereupon the elements are converted into hydrides. A portion of the hydride mixture is subjected to gas chromatography on a Teflon column with flame ionization detection, while a second portion is pasaed over a catalyst and subjected to gas chromatography with thermal conductivity detection; up to nine elements, iodine, phosphorus, and silicon, can be determined in compounds of molecular weight below 300. In another method (45) the sample is burnt in oxygen a t 625 "C in the presence of V,O and the combustion products are passed into the selected gas chromatographic columns: a column containing Chromosorb 102 for CO,, H20, and SO2, and a column conANALYTICAL CHEMISTRY, VOL. 58. NO. 5. APRIL 1986
* 145R
ORGANIC ELEMENTAL ANALYSIS
taining 20% of SE-30 on Chromosorb WAW for chlorine, bromine, and iodine. Separate determination of nitrogen can be achieved by passing the combustion products over a CuCuO catalyst at 540 "C in helium as carrier gas to reduce nitrogen oxides. Sakla et al. (46) performed simultaneous determination of carbon, hydrogen, chlorine, bromine, sulfur, and metals in organometallic compounds as follows. The sample is burnt in oxygen at 850 "C; H 0 and COz are determined gravimetrically. Halogens and 402 are absorbed on electrolytic silver, which is subsequently heated at 550 "C and flushed with nitrogen to liberate the SOzand then with hydrogen to liberate the halogens as hydrogen halides; SOz is oxidized to SO-:, which is titrated with 0.01 N Ba(C104)2,while halides are titrated with 0.01 N Hg(C104)2. The metal oxide remainin in the platinum boat is dissolved in HN03-HC104 (l:l),an8 the metallic element is determined gravimetrically or titrimetrically as the metal-quinolin-8-01 complex. Hara et al. (47) continued their study of simultaneous determination of carbon, hydrogen, nitrogen, and oxygen by sulfurization; the method was extended to the analysis of organophosphorus compounds. Schleisman et al. (48)used the Fourier transform near-infrared spectrometer to determine carbon, hydrogen, and sulfur by atomic emission from an argon inductively coupled plasma; simultaneous monitoring of carbon emission at 909.5 and 940.5 nm, hydrogen emission at 656.2 nm, and sulfur emission at 921.2 nm can establish the stoichiometry or chemical formula of the organic compound. Megroyan et al. (49) determined carbon, hydrogen, and mercury by combustion and gravimetry, using antomony as absorbent for mercury. Attia et al. (50) also determined carbon, hydrogen, and arsenic or selenium by gravimetric methods, Asz03 or Se02being retained in a silica tube inserted into the empty combustion tube. Seo (51) determined carbon and chlorine on bromine by gas chromatography after converting the halogen to hydrogen halide and carbon to CH4. Dingjan et al. (52)determined the atomic ratio of halogenor sulfur-containing compounds by using a microwave-induced plasma. For the simultaneous determination of all halogens, Wang et al. (53) decomposed the sample by sodium fumes at 280 "C for 1 h and dissolved the sodium halides in NaHC0,NazC03and analyzed the solution by ion chromatography using electrochemical and conductometric detectors. Osadchii et al. (54) determined chlorine, bromine, and iodine by pyrolyzing the sample at 800 "C and passing the products successively through three columns packed with powdered aluminum and maintained at 300, 200, and 100 "C, respectively, to retain Al13, A1Br3, and AlC13; each aluminum halide was then eluted and titrated with EDTA. Kan et al. (55)decomposed the sample containing halogens and sulfur by closed flask combustion and then determined F,C1-, Br-, and SO$ by ion-exchange chromatography on a column of MCI Gel CA 04s-Hitachi Gel 3011-0 with a suppressor column of Hitachi Costum 2612 using conductometric detection. After flask combustion, Miroshina et al. (56)determined halides by titration with Hg(N03)2and 502- by titration with Ba(N03)2 sequentially. Cai et al. (57) determined sulfur and phosphorus in one sample by atomic absorption spectrometry; after closed flask combustion, phosphorus was converted to molybdophosphate and molybdenum was measured at 313 nm, while S042-was precipitated as BaS04 and the excess Ba2+in the filtrate was measured.
DETERMINATION OF TRACE ELEMENTS During the past 2 years, determination of more than 50 elements was covered in the literature. Most of the publications are related to the analysis of organic mixtures (58). Various techniques of decomposition of the organic samples were studied. Ledent et al. (59) tested two mineralization methods for the analysis of plant materials, by digestion with HzS04-HN03-H202and by ashing at 450 "C; either method could be employed for the spectroscopic determination of B, Ca, and Mg, while neither method was suitable for Al, Cr, Fe, Mn, Ni, and Pb. Minagawa et al. (60)compared Kjeldahl and CuO combustion methods for measurement of nitrogen isotope ratios in biological material; the Kjeldahl method gave values considerably lower than those obtained by the combustion method. Knapp (61)found that decomposition of NBS standard orchard leaves by ashing with oxygen plasma or by 146R
ANALYTICAL CHEMISTRY, VOL. 58, NO. 5, APRIL 1986
heating in HN03 at 320 "C in a sealed silica tube gave correct values for As, Br, C1, Cr, Cu, Mn, Ni, and Zn. Adeloju et al. (62)evaluated several dry ashing methods for anodic stripping voltammetric determination of Cd and P b in biological materials; ashing at 500 "C after adding HzS04was the most suitable. Bodton et al. (63)compared combustion of biological samples in a quartz tube at 850 "C and in a Pyrex tube at 500 "C for C isotope analysis; yields for C were 28% lower in the latter. Hoenig et al. (64)studied various digestion methods for trace element analysis of plant materials by atomic absorption spectrometry; digestion by HZSO4-HNO3-H2O2gave complete recovery of As, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Sb, T1, and Zn. Hamze et al. (65)evaluated six procedures for determining Ca, K, Mg, and Na in citrus leaves and found digestion with HN03-HzS04-HC104 ( 9 2 2 ) to be most effective. Novozamsky et al. (66)recommended treatment of dry plant material with salicylic acid-Se-H2S04 for 2 h at room temperature and then at 100 "C for 2 h; after cooling, the mixture was further digested with 30% H202at 300 "C for 2 h. Allen (67)digested plant materials by heating the powdered samples in platinum boats under reflux with HC1O4-HNO3 (51) a t 190 "C for 20 min. For voltammetric determination of Cd, Co, Cu, Ni, and Pb in milk powder and other biological materials, Hasse et al. (68)heated the sample with HN03-HC104-H2S04 in a pressurized vessel for 12 h at 120 "C. For the determination of Ca, Cu, Fe, K, Mg, Mn, P, and Zn in coffee, soya bean, corn, and grass, Miyazawa et al. (69)simply heated the samples in 1 M HCl at 80 "C for 15 min, shook the mixture for 15 min, and filtered the solution. Yokel et al. (70)described a safe method to digest biological tissues with HN03-HC104-HzS04 for the determination of aluminum. Digestion media for determining arsenic in biological specimens include HN03HzS04-HC104in different proportions (71, 72)and "0,HZSO4-KzCrzO7(73).Hsu et al. (74)reported complete decomposition of carbonaceous matter by digestion of deep-sea sediments with HN03-HC104-HF for determination of Cd and Pb. Chang et al. (75)digested animal tissues with 30% H 2 0 2for determination of Ca and Mg. Decomposition of biological material for the determination of Hg and other toxic elements was achieved by heating with HNO3-HC1-H2OZ (76) or with HN03-HC104 (77). For the determination of Se in biological materials, "OB, HN03-H SO4, HN03-KzS208(7% HN03-H2S04-HC10,, or HN03-Mg(N03)2were used, the last reagent being most convenient (79). Raptis et al. (80)mineralized biological material in an oxygen plasma in the following manner. The dry pulverized sample is decomposed at 100 "C in a silica vessel placed in an apparatus with the base horizontal over the induction ring of a 20-40 W.h.f. generator; the material is exposed to a cool oxygen plasma containing 2.5% of argon excited at 27.12 MHz for 2-14 h. Hozumi et al. (81)found that ashing of organic material at 100-105 "C in an oxygen glow-discharge plasma led to a loss of C1 up to 50%. Siripone et al. (82) described neutron activation analysis of biological materials using mineralization with a saturated Mg(N03)2solution. Norris (83)determined Ti in paints by fusion of the sample with KHS04 and dissolution of the melt in H2S04. Cantillo et al. (84)fused estuarine sediments with LiBOz and dissolved the bead in HN03 to obtain the solution for dc plasma emission spectrometry. Ogner (85)proposed decomposition of plant material using "OB, H202,and UV irradiation; after dissolution of the sample in HN03 at 150 "C, Hz02and Ce(NO3I3 were added and the mixture was irradiated for 2 h at 45 "C. Many reports were published on the comparision and evaluation of methods for trace element analysis. Locatelli et al. (86)compared the determination of trace elements in materials of vegetable origin by voltammetry and by atomic absorption spectrometry; the latter method was more reproducible and faster, while the former method was more economical but cannot be used for every metallic element; for Cu, Pb, and Zn, detection limits were lower by voltammetry. Aten et al. (87)compared the determination of Fe, Mg, and Zn in fertilizers by flame atomic absorption and by Inductively coupled plasma emission spectrometry; statistically identical results were obtained. Bahreyni-Toosi et al. (88)evaluated five techniques for flame atomic absorption spectrometry of Cu and Zn in blood, including continuous aspiration, pulse nebulization, pulse nebulization into a slotted tube, atomization from a Delves cup, and vaporization from a wire loop.
ORGANIC ELEMENTAL ANALYSIS
Table 11. Determination of Trace Metals
Table I. Determination of Trace Nonmetals element antimony arsenic
bismuth boron bromine carbon chlorine fluorine hydrogen iodine nitrogen
oxygen phosphorus selenium
silicon sulfur tellurium
material analyzed
mode of finish"
food petroleum biological feed food petroleum polymer biological biological detergent biological biological oil sand detergent oil biological fabric biologica biological food biological food marine petro1eum plant wine petroleum plant biological food plant biological
aas aas aas, csv, col, tit col aas asv xrf aas, col col tit naa ir, rad tit xre naa gc, ise gc naa, rad naa, rad, xre col, naa col, gc, ise, naa, xre gc col cou col, tit tit ir ms col, naa col col aas, csv, col, flu, gc, ms, xre aas, naa, pol aas, flu, naa aas col aas, aes xre aas, col, gc, xrf aes aas
marine plant biological food plant coal plant polymer biological
ref 110 111
112-117 118 119 120 121 122, 23 124 125 126 127, 28 129 130 131 132, 133 134 135, 136 137-139 140, 141 142-146 147 148 149 150, 151 152 153 154 155, 156 157 158 159-174 175-177 178-180 181 182 183, 184 185, 186 187-190 191 192
Abbreviations: aas, atomic absorption spectrometry; aes, atomic emission spectrometry; afs, atomic fluorescence spectrometry; asv, anodic stripping voltammetry; csv, cathodic stripping voltammetry; col, colorimetry (spectrophotometry at the visual region); con, conductivity; cou, coulometry; enz, enzymatic method; epm, electron probe microanalysis; fep, flame emission photometry; flu, fluorimetry; gc, gas chromatography; ic, ion chromatography; ir, infrared absorption; isd, isotopic dilution; ise, ion-selective electrode; lam, laser microprobe mass analysis; IC, high-performance liquid chromatography; lum, luminescence; mas, molecular absorption spectrometry; ms, mass spectrometry; naa, neutron activation analysis; paa, photon activation analysis; pes, photoelectron spectrometry; pir, proton irradiation; pol, polarography; rad, radioactivity; tit, titrimetry; tlc, thin-layer chromatography; tur, turbidimetry; xre, X-ray emission; xrf, X-ray fluorescence. Howanitz et al. (89) compared potentiometry with flame photometry for determination of K and Na in blood; values for K were identical while values for Na were 2% higher by potentiometry. Al-Kinani et al. (90) determined trace elements in gallstones by neutron activation, X-ray emission, and X-ray fluorescence; the errors of neutron activation ranged from 1 to 9% for most elements while the errors of X-ray fluorescence were up to 12 % . Brix et ai. (91) reported on an interlaboratory study of the reproducibility in the determination of heavy metals in marine plants; significant variations were observed. Six laboratories collaborated on the inductively coupled plasma emission spectroscopic determination of Ca, Cu, Fe, Mg, Mn, P, K, Na, and Zn in six infant formulas; the within-laboratory and between-laboratory coefficient of variation ranged from 90 to 105% (92). Bettinelli et al. (93) evaluated the L'vov platform and matrix modification for estimation of Al in blood by atomic absorption
element
material analyzed
mode of finish"
aas col aas barium aas beryllium aas, col, xrf cadmium aas, col aas aas, aes, col, fep, ca1cium ise, tit biological aas, aes, xre chromium plant aas biological aas, col, pol cobalt aas feed biological aas, aes, col, copper ise, naa col feed col food gallium aas plant col plant germanium aas biological gold col, ms biological iron food aas col plant biological aas, afs, asv, col lead food asv marine aas petroleum aas aas plant wine PO1 col, flu lithium biological col, flu magnesium biological aas manganese biological col food rad plant aas mercury biological food aas marine aas biological col, naa molybdenum aas, pol plant biological nickel aas, naa petroleum aas plant aas biological palladium col biological platinum aas, IC, pol biological p1utonium rad plant rad biological potassium feP biological protactinium rad radium biological rad sodium biological naa food feP strontium biological aas, rad technetium biological rad plant rad thallium biological aas, asv wine asv tin bio1ogica1 asv food aas, col, flu titanium biological aes food PO1 petroleum col plant col uranium biological col, ms, naa, rad food naa, rad vanadium biological aas, naa marine col zinc biological aas, col, IC,ms, rad food flu zirconium paint col "See footnote of Table I for abbreviations. aluminum
biological plant petroleum biological biological food marine biological
ref 193-204 205 206 207 208-217 2 18-2 20 221
222-228 229-235 236, 237 238-243 244
245-255 256 257 258 259 260 261-266 267 268 269-281 282 283, 284 285-287 288 289 290, 291 292-296 297-299 300 301 302-306 307 308 309, 310 311,312 313-315 316 317 318 319-323 324 325, 326 327 328 329, 330 331 332 333, 334 335 336 337-340 341 342 343-345 346 347 348 349 350-355 356, 357 358-361 362 363-370 371 372
spectrometry; Feitsma et al. (94) reported similar study for Cd in urine. Harnly et al. (95) compared atomic absorption and atomic emission for the determination of Cr. Schneider ANALYTICAL CHEMISTRY, VOL. 58,
NO. 5,
APRIL 1986
147 R
method anodic stripping atomic absorption
atomic emission
colorimetry dc arc flame photometry gas chromatography ion chromatography ion-selective electrodes liquid chromatography mass spectrometry neutron activation
material analyzed biological food pharmaceutical biological food marine pharmaceutical plant wine biological food marine plant wine biological feed biological plant biological food wine biological plant biological biological plant biological biological
food marine petroleum pharmaceutical plant photon activation biological biological polarography food wine potentiometric stripping food radioactivity biological titrimetry plant X-ray emission biological plant X-ray fluorescence biological food petroleum pharmaceutical
elements determined Cd, Cu, Pb, Zn Cd. Pb cui Zn Al, As, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, Ni, Pb, Sb, Se, V, Zn Ag, Al, As, Ca, Cd, Cr, Cu, Fe Mg, Mn, Ni, Pb, Sn, Zn Cdg, Hg, Pb Cd, Cr, Pb, Se Ca, Cu, Fe, K, Mg, Mn, Na, Zn Al, Cd, Pb, Sn Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sn. Ti. V. Zn Ba, K, Na, Rb As, Sb, Se Al, B, Ca, Cu, Fe, K, Mg, Mn, Na, P Al, B, Cu, Cr, Fe, Mn, Mo, Pb, Si, Sn, Ti, V, Zn Ca, Cu, P, Zn Ca, Fe, Mg, P Ag, Mn, Ni, Pb, Zn rare-earth metals K, Na
373-375 376 377 378-399 400-409 410 411-412 413,414 415 416-426
427 428 429-431 432 433,434 435 436, 437 438 439 K, Na 440 K, Na 441 S, Sn 442 Ca, C1, K, Mg, Na, S 443,444 Ca, C1, K, Na 445-447 Cd, Cu, Hg, Ni, Pb, Zn 448,449 Cu, Ni, Pb 450 Al, B, Ca, Cd, C1, Fe, Mg, Mn, N, Na, Pb, T1 451, 452 Ag, Al, As, Au, Ba, Br, Ca, Cd, C1, Co, Cr, Cs, Fe, Hg, I, K, Mg, Mn, Na, Ni, Pt, Prb, 453-465
Sb, Sc, Se, Sn, V, Zn As, Cu, Mn, Mo, Zn As, B, I, Se As, Br, C1, Cu, Hg, Mn, Na, Sb, Zn Al, Br, Ca, C1, Co, Cr Fe, Hg, K, Mg, Mn, Na, Rb, Sc, Se, Zn Br, Co, Cr, Fe, K, La, Mn, Rb, Sb, Sc, Th, Zn Ca, Mg, Zr Co, Ni Cd, Cr, Cu, Ni, Pb, Sn, Zn Cd, Co, Cu, Pb, Zn Pb, Sn Am, C1, Cu, P, Pu, S, Th, U
c1, s
Ca, Br, C1, Cu, Fe, K, Mn, Ni, P, Rb, S, Sr, Zn Al, As, Br, Ca, C1, Cr, Cu, Fe, Hg, K, Mn, Ni, P, Pb, Rb, Si, Sr, Ti, Zn As, Br, Co, Cr, Cu, Fe, Ge, K, Kr, Mg, Mn, Ni, Rb, Sc, Sr, Ti, V, Y, Zn Ca, Co, Cr, Cu, Fe, Mn, Ni, V, Zn Al, Ca, S Co. Cr., Cu., Fe., Mn., Ni., Pb., Zn I
et al. (96) compared three spectrophotometric methods for Co in urine. Saltzman et al. (97) devised a computer program to evaluate analyses for Hg in urine and P b in blood over an 8-year period. Debeka (98) published a collaborative study of atomic absorption determination of P b in infant formulas. Various methods were compared for the determination of Hg in biological material (99) and in food (100). Schwedt et al. (101) evaluated four spectrophotometric methods for determination of Mo in biological material. Adam et al. (102) compared colorimetric and enzymic methods for determining serum phosphorus; correlation between the results by the two methods was good. Critical appraisal of several methods for determination of Se in biological material was reported by diffferent investigators (103-105). Atomic absorption determination of thallium was compared against colorimetry (106) and anodic-stripping voltammetry (107). Mousty et al. (108)reported good agreement for determination of V in urine by atomic absorption and by neutron activation. Sariano et al. (109) evaluated seven procedures for atomic absorption determination of Zn in blood in terms of accuracy, precision, detection limit, sensitivity, analytical recovery, and physical interference. Selected papers on the determination of single elements are listed in Tables I and 11. It will be noted that health hazards such as cadmium, lead, mercury, and selenium received the most attention; the last mentioned element was studied by 148 R
ref
ANALYTICAL CHEMISTRY, VOL. 58, NO. 5, APRIL 1986
466 467 468 469,470 471-473 474 475 476-478 479 480 481 482 483-487 488-490 491-494 495 496 497
nine different methods. Table I11 summarizes various methods for multielement determination, showing that atomic absorption spectrometry and neutron activation were most frequently employed. On the other hand, a number of papers appearing during the past 2 years recommended the use of proton-induced X-ray emission (PIXE) to determine trace elements, particularly for the analysis of biological material. Besides the references cited in Table 111,there are other papers on using PIXE to analyze human hair (498-503) and fingernails (504);the concentration and distribution of trace elements in these tissues may have implications on the welfare of the person. LITERATURE CITED
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