56) Pelc. S. R.. Coombes. J. D.. Budd. G: C., I h p . Gill Res. 24,'192 (1961). ' 57) Pepin, P., Tertian, L., Trillat, J., Compt. rend. 252, 1885 (1961). 58) Perkerson, F. S:, Reeves, W. A., Trim. V. W..Teztzle Research J . 30. 59) Phillips, R., Brit. J . A p p l . Phys. KnA
11
C / InCi\\
--- -
- - 7
(160) Ibad., 12, 551-8 (1961). (161) Phillips, V.A . , Cannon, P , Suture 187, 313-2 (1960). (162) Polymer and Fiber Microscopy hociety, meeting a t SorTvalk, Conn., hlay 1961, abstracts, J . A p p l . Polymer SCZ.5 , $8-S10 (1961). (163) Porter, B., Carra, J., Tripp, V., Rollins, A I . , Teztzle Rpseaich J . 30, 249-6i (1960). (164) Porter, B., Tripp, V., deGruy, I., Rollins. h1.. Ibzd.. 30. 510-20 11960). (165) Price, F. P.,' J.'Polymer Scz. 42, 49-56 i1960). (166) Przybylski, R J., Erptl. Cell Research 24, 181-4 (1961). (167) Quiglry, 31. B., Lijor, I., Smith, E., Sorelco Reptr. 7, 55-7 (1960). (168) Radavich, J., RCA Scz. Znstr. Sews 5, SO 2 , 1-4 (1960). (169) Rangan, S., J . Roy. JIicroscop. SOC.79, 377-8 (1961). (170) Recourt, A., deVries, G. H. F., iyature 191, 1185-6 (1961). 1171) Reisner. J.. RCd Sei. Znsfr. News ' 6,'Xo. 2, 1-8 (1961). (172) Reneker, D , Geil, P., J . A p p l . Phys. 31, 1916-25 (1960). ( l i 3 ) Ries, H. E., Jr., Cheni. Eng. A'ews 38, 40 (October 3, 1960). (174) Hies, H. E., Jr., Sci. American 204, T V ~ 2 L.". ")
IA"_ K ~ J" -G ~i i a c i ) r ,LU"I,'
(1T5) Rochow, T. G., ANAL. CHEZI.33, ( 3 A (October 1961). (176) Ibid , pp. 1810-6. (177) Rochow, T. G., Thomas, A . 31.,
Botty, &I. C., Ibid., 32, 92R-103R (1960). (178) Rouze, S., A-orelco Reptr. 7, 152 (1960). (179) Rowe, F. G., Bartunek, A., MeGlasson, R., Meyer, F., Royer, R., Chem. & Znd. (London) 1960, 712-3. (180) Ruedl, E., Delavignette, P., Amelinckx, S., J. A p p l . Phys 32, 2492-3 (1961). (181) Sawkill, J., SchTvarzenberger, D., Brzt. J . A p p l . Phys. 1 1 , 498-503 (1960). (182) Scott, D. B., Nylen, h1. U., Pugh, 11.H., Korelco Reptr. 7, 32-5 (1960). (183) Sella, C., J . Polymer Sci. 48, 207-18 (19601
(184j -Shell, J. W.,Chem. Eng. News 39,
84-5 (October 9, 1961). (185) Silvester, N. R., Burge, R. E., Nature 188, 641-3 (1960). (186) Simon. R. E.. SDroull. R. L.. J . A p p l . Phys. 31, 2224--5 (1960). (157) Sims, A. L., J . Sei. Instr. 38, 406-7 (1960). (188) Statton, W., Geil, P., J . Appl. Polymer Sci. 3,357-61 (1960). (189) Stewart, B., Stewart, P., Norelco Revtr. 7. 21-2 (1960). (190)' Stieiler, J.' 0.)'Noggle, T. S., J . Appl. Phys. 31, 1827-8 (1960). (191) Stiegler, J. O., Noggle, T. S.,Rev. Sei. Inst?. 32, 406-7 (1961). (192) Strutt, P. R.. Rev. Sei. Instr. 32. ' 411-3 (1961). ' (193) Suito, E., Uyeda, N., J . of Electronmicroscopy 8 , 25-30 (1960). (194) Suito, E., Uyeda, N., A'ature 185, 4--52.4 - (infin) ,-., __,. (195) Takahashi, N., J . A p p l . Phys. 31, 1287-90 (1960). (196) Taylor, A. R., A'ature 192, 611 (1961). (197) Taylor, A. R., Science 134, 1636-9 (1961). (198) Tennery, V. J., Bergeron, C. G., ~
Borasky, R., Rev. Sci. Instr 31, 452-3 (1960). (199) Thomas, K., Roberts, hl. W., J . A p p l . Phys. 32, 70-5 (1961). (200) Thun, R., Hass, G., Craig, D., Rev. Sei. Instr. 30, 913-15 (1959). (201) Time 78,60-6 (Nov. 17, 1961). (202) Tousimis, A,, Brooks, E., Birks, L., Adler, I., Chem. Eng. News 39, 54 (Oct. 23, 1961). (203) Trillat, J., Sella, CI., Bull. inst. textile France NO.92 (1961). (204) Tripp, V. W., Moore, A. T., de Gruv. I.. Rollins. 31. L.. Teztile Research J . 30: 140-7 11960) (205) Tkipp, 1'. iV., Moore, A. T., Rollins, ' if. hf. L., L., %d., Ibid., 31,'295-301 31, 295-301 (1961). (196i). (206) Trurnit, H., Schidlovsky, G., Chem. Eng. News 38, Y o . 27,41 (1960). Vacher, H., Burnett, H., Duff, f, R., (207) Vach Natl. B w . Standards. Tech. "fews Bull. 45. 30-1 (1961). (208j Van Huysen, G., Norelco Reptr. 8 , 95-9 (1961). (209) Veis, A,, Cohen, J., 'Vature 186, 720-1 (1960). (210) Vinogradov, G., Sinitsyn, V., J . Inst. Petrol. 47. 357-64 (1961). (211) Vook, R.; J . A&. Phys. 32, 1557-61 (1961). (212) Washburn, J., Thomas, G., Chem. Eng. News 39, No. 9, 38-9 (1961). Cruikshank, J., Laur(213) Waterson, 8., ence, G., Kanarek, A., Virology 15, 379-82 (1961). (214) Wells, 0. C., Brit. J . A p p l . Phys. 11, 199-201 (1960). (215) Westrik, R., Kiel, A. M., Xature 190, 163 (1961). (216) Williamson, G. K., Proc. Roy. Soc. London A257, 457-63 (1960). (217) Wolken. J. J.. A'orelco Revtr. 7. ' 62-6 (1960)'. (218) Zeitler, E., Bahr, G., RCA Sci. Instr. A'ews 5 , No. 1, 5-11 (1960).
Review of Fundamental Developments in Analysis
Nucleonics G. W. leddicotfe Oak Ridge National laboratory, Oak Ridge, Tenn.
T
review of significant publications in nucleonics covers the period from late 1959 to late 1961 and supplemrnts t h e previous review by lleinke (777). The trend to nucleonic applications in analytical chemistry, noted by LIrinke in his earlier reviews, continues to increase so that many more articles have appeared. I n an attempt to establish a suitable criteria for evaluating the inclusion of a reference in this review, this reviewer has accepted the responsibility of citing only those articles that have significant value to those areas of nucleonics concerned with the chemical separations of radioisotopes from other radioactive species, the measurements of their radioactivity, and their use in tracer applications. KO attempt has been made to cite all HIS
publications on conferences, reference materials, trade literature, and the like. Such information is readily available through other sources. I n establishing a format for presentation, the reviewer has recognized that certain general information must necessarily precede the more specific information. Such information establishes thoughts and ideas on prerequisites that have been necessary before each scientist could accomplish his investigation in this unique area of analytical chemistry. The sequency of specific information-radiochemical separations, radioactivity measurements, and radiotracer applications-has been accepted as being an adequate means of giving as much information as possible on the fundamental developments in nucleon-
ics. V i t h regard to the bibliography presentation, reference is made sometimes to a second source, for example, Nuclear Science ilbstracts, only to assist the reader if it is difficult to locate the original article. GENERAL
The impact of radioisotope methodology in the discipline of analytical chemistry can only be emphasized from the number of authors cited in this review. Many existing analysis problems are now being solved through the use of radioisotopes and their phenomena. Aebersold (I@, in his discussion on the economic implications of radioisotopes in everyday application, very aptly establishes a pattern for the inVOL. 34, NO. 5, APRIL 1962
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creased use of such powerful analytical aids. Special sources of information on radioisotope applications, availability, and potential value have been prepared by Blaetus (126) and others (66, 70, 123, 364, 531, 746, 846, 983, 997). Forsling (343) has recently reported on the future of transuranic elements and a review has been made by Crane (249) on the possible applications of the transplutonium elements, Cm242, Cm244,and PuZs8 to space technology. The compilations by Millett and Wilson (791) and Voress, Jacobs, and Smelcer (1176) contain many references to bibliographies and literature surveys on the use of radioisotopes. Special sources of information have been published on radioisotope applications in biochemistry (166), in chemical research (260,460,607,795, 1133),in drug research (372), and in industrial problems (67, 260, 261, 308, 318, 365, 406, 774, 980). Cameron (203) gives many references on the use of radioisotopes in nondestructive testing, and Maedu (735) reports on their use as sources in quality control of fabrication processes. Such information sources as the revised Isotope Catalog of the Oak Ridge National Laboratory (885) reports on the availability of radioisotopes. Atomic Energy of Canada, Ltd., also has issued a revised radioisotope handbook (71). A catalog of radioisotope data is also available from the United Kingdom Atomic Energy Authority (33). Stiennon-Bovy and Geladi (1107) have issued a nomogram for radioisotope utilization. Typical of the reports issued on the type of laboratory and equipment needed for the processing of radioactive materials is that by Scott (1034). This report contains a bibliography of a t least 126 references on the design and construction of radiochemical laboratories. Fundamental rules relative to the construction and management of an analytical laboratory for handling plutonium have been reported by Metz and Waterbury (786). Similar reports on radiochemical laboratories and their equipment have been given by Grinberg (417), Gadda and Scaroni (368, 559), and Triulzi (1135). Other general articles show that there has been an increase in the interest of providing training in the techniques of radioisotope handling. Daudel (262) and Danforth and Stapp (260) have published excellent handbooks for use in training personnel to utilize radioisotopes in chemical and industrial problems. Chase (217) has prepared a laboratory manual that can be used primarily as an introductory guide in radioisotope methodology for technicians, advanced students, and researchers. Practical experiments are included. Choppin (226) has published a sign%cant text and a series of good experi-
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ments on experimental nuclear chemistry. Garrett (368) gives an excellent discussion on the place of nuclear radiochemistry in the curriculum in general chemistry, and Radin (964, 965) has recently published a group of radioisotope experiments for use in the chemistry curriculum. Other articles containing laboratory experiments have also become available (211, 461, 564). The books by Emeleus and Sharpe (508) and Faires and Parks (321), and the revised edition of the National Research Council’s Subcommittee on Radiochemistry’s handbook (860) also provide excellent information on radiochemistry and radioisotope laboratory techniques.
RADIOISOTOPE SEPARATIONS
Much consideration continues to be given to radiochemical methods of analysis. General compilations by Fisher (332), Fletcher (338), Gerlit, Pavolotakaya, and Rodin (376), Harteck and Dondes (447), Healy (452), Krivokhatskii (631), Kovach (625), and Monk and Herrington (807) report on many of the radiochemical methods used to determine radioactive elements, The World Health Organization, Geneva (1228), also has recently issued a technical report on the methods of radiochemical analysis. Reviews on the methods of separation used in the analysis of mixtures of the fission products have been presented by Agrinier (15), Bar (82), Henry and Herczeg (467), Pi (934), and Thompson (1128). -4 revised collection of radiochemical procedures for most of the fission products and other radionuclides has been issued by Kleinberg (599). Schneider and Harmon (1028) also record procedures for the fission product elements. Supplemental radiochemical procedures to the Oak Ridge National Laboratory have also been recently issued (884). Methods for the quantitative analysis of radionuclides in process and environmental samples (113, 137, 1208), in urine (138, 1035), in biological science (113, 446, 1031), and in connection with nuclear reactor requirements (307, 930) have also been evaluated and reported. Other information on compilations of radiochemical analysis procedures appear in a recent revision to the booklet of the Subcommittee of Radiochemistry of the National Research Council entitled “Source Material for Radiochemistry” (860). Sharpatyi (1063) reports on the radiochemistry of aqueous solutions. Welford and others (1195) describe a method for the sequential analysis of ten nuclides occurring in long range fallout debris. Samsahl (1014) also describes a chemical eight-group separation method for routine use in radiochemistry. Strassman (1090) describes
methods for the separation and determination of short lived radionuclides. Wish and F r e i l i g (1226) report on the use of a carrier-free procedure in quantitative radiochemical analysis. Articles discussing factors affecting radioactive gas emanation ( l o g s ) , the precipitation of uranyl ferrocyanide from aqueous solutions (1082) have also been presented. Ziv and Sinitsyna (1243, 1244) report on the determination of the electrode potentials of radioactive elements. Applications of polarography in radiochemistry have been described by Ferenczy (327), Shinagawa and Nezu (1065), and by Love and Greendale (710, 711). Meinke (777) has previously described the interests of the Subcommittee OR Radiochemistry in compiling available information on the inorganic and radiochemistry of each individual element into a monograph to be issued as a part of a series. The following monographs have been issued and can be obtained from The Office of Technical Services, Washington, D. C., for a nominal cost: actinium (1105), aluminum (692), americium (927), arsenic ( l o g ) , astatine (62), barium (1115), beryllium (322), bromine (GOO), cadmium (275), calcium (1115), carbon (487), cesium (331), chromium (959), chlorine (600), cobalt (9S), copper (294, curium (927), fluorine (600), francium (500), gallium (692), germanium (761), gold (310), hafnium (1101), indium (1116), iodine (GOO), iridium (669), iron (869), lead (384),manganese (658), mercury (984), molybdenum (1019), niobium (1102), nitrogen (487), osmium (660), oxygen (487),.platinum (661), polonium (328), potassium (672), protoactinium (597), the rare earths (1105), the rare gases (806), rhenium (662), rhodium (R27), ruthenium (1229), scandium (1105), selenium (663), strontium (1115), tantalum (1102), technetium (61), tellurium (669) , thorium (601), tin (868), titanium (590), the transcurium elements (471), tungsten (838), vanadium (176), yttrium (1106), zinc (469), and zirconium (1101). Additional monographs in the series will be issued during 1962. Analytical techniques based upon precipitation, volatility, electrolysis, solvent extraction, ion exchange resins, paper chromatography, etc., have been used in either carrier or carrier-free separations for individual radionuclides or for the separation of groups of radionuclides. Publications during 196062 on these separation techniques can be categorized as follows: Precipitations. Pushkarev, Skrylev, and Bagretsov (961) report on the use of hydrosol and gelatin precipitations as a means of concentrating radionuclides. Spitsyn and Gromov (1087) report on the effect of radioactivity on the adsorption properties of a precipi-
tate. Radionuclide separations by precipitations from dilute solutions have been recorded by Sturzer (1114). Many articles show that specific radionuclide separations can be made either by direct precipitation or by coprecipitation as carbonyls (866), fluorides (855, 1152), hydroxides (612), mandelates (783), basic phosphates (21), sulfates ( I l B ) , sulfides (63S), phosphomolybdates (164), oxalates (165, 196, 411-413, 566), phenylarsonates (615),and polyuranates (614). Dipicrylamine (677) and other organic reagents (642) have been used in separating specific radionuclides. Active manganese has also been used as a coprecipitant in the separation of alkaline earths (300). Volatility. Wish (1625) reports on the use of a distillation method in the quantitative determination of fission ruthenium from mixtures of other fission products. Other reports and S35 by have been made on 1132 distillation methods (712, 951). A vacuum distillation technique has been used by-DeVoe (277) in the radiochemical separation of cadmium. Electrolysis. The rare earth elements (902, 1066-1068), the actinides (481, 798), radium (618, 619), and indium (994) have been separated by use of amalgam exchange reactions a t a mercury cathode. Electrolytic methods have also been used to separate uranium (993, l o l l ) , neptunium ( l o l l ) , Plutonium ( l o l l ) ,americium ( l o l l ) , cesium and strontium (179, 180, 912). An internal electrolysis method for use in carrier-free separations has also been described (505). Solvent Extraction. Freiser (349) has recently reported on the general use of solvent extraction in radiochemical separations. Moore (816) has written an excellent Nuclear Science Series Monograph, entitled “LiquidLiquid Extractions with High-Molecular Weight Amines.” Specific liquidliquid extractions of radionuclides from acid systems by use of TTA (586,1184), T B P (442, 514, 516, 521, 522, 749, 805, 874, 1071, 1167), tri-n-octylamine (572, 603, 1056), triisoactylaniine (814), and diisobutyl carbinol (717) have also been reported. Other systems, based on extractions with hexone (759), di(ethy1hexy1)phosphoric acid (856), dodecylbenzenesulfonic acid (513, 515, 858), n-benzoylphenylhydroxylamine (29), acid alkyl phosphates (219), dibutyl phosphate (295), alkylamines (503, 518, 520, 522), diisobutyl ketone (557), and phoshho-organic compounds (922, 928, 929) have been describrd. Other liquid-liquid extractions and methods have been reported by Kauffmann and Blank (664), hIcCown and Larsen (770), Boyd, Larson, and hIotta (162, 153), Butler and Ketchen ( 1 9 4 , Coleman, Kappelmann, and Weaver (239), Kimura (692), Knoch and Lindner (60S,
604), Kuznetsov and Blekhta (643)) Maeck and others (731), Nathans, Greenberg, and Feder (859), Nikol’skii (873), Palsheim and Zolotov (913), Panova and Levin (914), Pushkarev, Skrylev, and Bagretsov (962), Rimshaw and Malling (981),Ross and Hahn (989), Ryabchikov and Volynets (IOOd), Shevchenko and others (1055-1057), Stary (1097),Stary and Ruzicka (1O98), Ueno and Chang ( l l @ ) , and Warren and Suttle (1186). Chromatography. Ion exchange systems using organic and inorganic exchangers, ascending and descending paper chromatography techniques, electrophoresis and vapor phase chromatography continue to be used in methods of separating radioactive elements. Typical of the publications are the following: General reports on the use of ion exchangers in separating radionuclide mixtures, particularly the fission products, have been given by Seyb and Hermann (1047), Martinola and Wegner (754), Crouch and Swainbank (263), Dunkel (290), Ho (479), and Stronski (1112). Several reports on specific group separations by ion exchange resins have been made (125, 137, 965, 957, 958, 1014, 1046). Schumacher and Streiff’s (1040) method of ion-focusing exchange has been applied to fission product analysis by Shvedov, Ten, and Stepanov (1070), by Schumacher and Fried1 (1038,1039), and by Schumacher and Streiff (1041). Schumacher (1037) gives additional information on its use in radiochemical analysis. Anion exchange resins have been used to separate protoactinium (948), Th234 and/or U (115, 622-624), Ygo-SrgO and La140 (797), Sr90 (474), the rare earths (299), trivalent actinides and lanthanides (488), and Nbg5and Ta1E2 (1084). Cation exchange resins have been used to separate thorium (1109), zirconium (583), uranium (584, 585), scandium (593), ruthenium (450), and Pb, Ca, Sr, Ba, and Ra (320). Other anion and cation exchange resin applications have been reported by Akaishi (bo), Bogar and Lock (133), Choppin and ChethamStrode (2$8),Davis (264), Jackson and Short (528),Krawczyk (627),Llajumdar and De (738), lloeller, Leddicotte, and Reynolds (804),Roberts (982), Ryabchikov, Palei, and Alikhailova (IO&?), Stronski and Rybakow (1113), Tsubota and Kitano (1159), Wish (1223, 1224), and Dybczynski (293). Other types of ion exchangers used in analysis include silica gel (17 ) ,bentonite clays (214), beads impregnated with tri-n-octylphosphine oxide (281, 282), biotite and/or vermiculite (552, l o l a ) , activated charcoal (25), aminopolyacetic acids (363), cellulose (888),bis(Zethy1hexyl, orthophosphoric acid (121 7 ) , and humic acid (1222). The use of ion exchange films (319) and ion exchange
membranes (405) in radiochemical analysis have also been reported. General information on paper chromatography methods has been presented by Pocchiari and Rossi (949), and Levi and Danon (687). Paper chromatography separations of the fission products (377), of R a E from radiolead (244), and of uranium (441) have been reported. A method of focusing chromatography has been used by Shinagawa, Kiso, and Oyoshi (1064) to separate fission products. Adloff (10) reports on the separation of radioelements by use of zirconium-impregnated papers. Paper chromatography with liquid ion exchangers has also been used (615). Radiochromatography separations of organomercury compounds (976), uranium in soils and plant ash (960), and niobium and tantalum from titanium (134) have also been reported. Kawamura (668), Pucar and Jakovac (969), and Shvedov and Stepanov (1069) report on the use of continuous electrophoresis methods of analysis. A method of focusing electrophoresis has been reported by Maydan, Toicher, and Zeidenberg (765). General information on the techniques of gas chromatography and its applications to the determination of radioactive elements has been given by Adloff (11). Vapor phase chromatography techniques have been described for the analysis of C14-labeled (197, 198) and Ha-labeled organic compounds (198, 199, 283). Fission Products. This particular section is concerned with reported analysis methods used for separating and assaying the fission product radionuclides, either in groups or as single elements. Many of the papers, particularly the Radiochemistry Monographs, mentioned in the general information for this section could also be considered here. Group separations of the fission products are exemplified by the reports of Boni ( I % ) , Bub, Vie, and TS’ebb (179, 180), Dunkel (290), Getoff i377), Ishikashi and others (519), Kiba, Ohashi, and Maeda (588), and Kuroda and Menon (635). Boni (137) used an anion exchange method to separate a t least 20 of the fission products (and Kp239p C060, Fe59, Cr51, and Z n 9 in process and environmental samples. Bub and his coworkers (179,180) report on the use of electrodialysis methods using ” 0 3 , H F , and oxalic acid. H F gave the best transfer ratios for most of the fission products investigated. The other papers cited showed that cation exchange resin separations (290) paper chromatography (377), extractions of the cupferrates into chloroform (588), and coprecipitation of ferric hydroxide (519) were usable methods for the analysis of fission products. Of some genmal interest are the reports by Campbell, ~
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Ortner, and Anderson (207) on the thermogravimetric analysis of the fission product oxides and nitrates and by Mullins, Leary, and Maraman (835) on the removal of fission product elements by slagging. Nore specific separations for individual fission products can be considered in the following manner : BARIUhl-140 AND STROSTIUhI-89, -90. Eulitz (320) reports that Ballo (and Srsg*90and RaD) can be quantitatively separated in one process by gradient elutions from cation exchangers. U s umi and Taketatsu (797) have used anion exchange resins in the carbonate form to separate Ba140 and La140. Other methods for separating radiobarium have been reported by Hunter and Perkins, (492), by Lane (649).and by Reed, Myers, and Sabol (973). Groos ( @ I ) , Hardy and Klein (443), and Lieser and Hild (695) present brief surveys of the chemical properties of SrS9and Srgoand of the methods by which they can be separated from other radioactive species. Kolarik and Kourim (612) report on the use of iron and aluminum hydroxide to absorb Sr90YgOfrom solution. Srqohas also been separated from urine by coprecipitation with calcium oxalate (539); from barium and calcium with AhOz (300); from aqueous solutions of the fission products with aininonium phosphomolybdate (164); and with polyuranates (615). SrS04 precipitations have been used to separate it from calcium-45 (112). Other separations of Srg0 by precipitation have been described for its determination in bones (348. 473, 683), milk (473),and water (413). Goldin and Veltin (394) and Veltin and Goldin (1168) report on the use of tributyl phosphate as an extractant for Srgofrom water. Extractions and chemical separations have also been used to separate and determine SrgOin soils and plants (360), in waters (365), and from calcium-45 (173). Hinzpeter (414) reports on the use of ion exchange methods to determine SrgO. Anokhin (60) has used Sr90 tracer and both anion and cation resins, plus E D T d as a complexing agent, to separate strontium quantitatively from calcium and magnesium. Zeo-Karb225 resin and HSO3 eluents have been used by Davis (264) to separate Sr90 from radionuclide mixtures. Cation resins have also been used to separate SrS9,90from R a D and Ba140 (320) and from fission product radionuclides (973, 1103). The isolation and separation of Srgofrom other radioactives by use of vermiculite-biotite ion exchange columns and acid eluents has been studied by Frysinger and Thomas (352). l l o n t morillonite and kaolinite have been used by Gromov (420) to absorb Sr90 from solution. CaCl? and S a C l solutions were then used to desorb SrgOfrom 146 R
0
ANALYTICAL CHEMISTRY
these materials. SrgOhas been separated from radioactive barium and calcium (l323),yttrium-90 (797), alkaline earths (1013), and fission products (982,1013) by ion exchange. Ion exchange has also been used to separate SrgOfrom milk (952). Vermiculite columns have been used to separate Sr90 from aqueous solutions ( I O I d ) , and an ion-focusing exchange method ha5 been used (1040) to separate it from La140, Pr140,and other fission produck SrgOhas also becn srparatcd from YaOby papcr chromatography and electrophoresis methods (568,863). Other articles describe the wparation of Sr9O and/or Srg9i n corn. corn products, and human tissues anti iion(>>(35. '1?6,1235, 1236), milk (10S5)s animal bones (35, 110, 124, 926), and biological fluids (537. 1134. 1149, 1150). $0115 (QTc), waters (90.$-907.,950, 1022. 1126, 1153, 1246),vegetation (11 '8 11%). and from Y90 (284). CESIChf-l%. 137, ASDRCBIDIU~I-86. Fisher and Raggenbass (333) report that a greater decontamination of CsI37 from fission product mixtures, analyzed by the standard phosphotungstate method, can be obtained if a barium hydroxide metathesis of the cesium phosphotungstate precipitate is made. Barium phosphate and tungstate are formed while the cesium is obtained in solution as the hydroxide. Pushkarev and others (961) have used hydrosols and gelatin to concentrate Cs137 from radioactive mixtures. Reverse-phase partition chromatography has also been used in the determination of Cs137 (937). Dannecker, Kiefer, and Maushart (261) report a gamma spectrometric method to determine Cs'37. Gray (410) has shown that Cs137 can be separated from an aqueous solution of the fission products by a precipitation as CsBr. Hroadbank and others (164) report that cesium can be selectively removed from dilute nitric acid solutions by an ammonium 1Bmolybdophosphate precipitation and suggest that this can be used as a quantitative method for the determination of Cs137. Hunter (490), Kingsley, Cumming, and Finston (596),Krieger and Groche (628),and Lima, Abrao, and Pagano (697) also report on determining Cs137. Cs137has been separated from Rb*6 by an ion mchange method using Dowex 50 resin and elutions with 0.5N HC1 (512). Cation resins and ammonium phosphomolybdate reagents have been used by Arkell and Morgan (63) to separate Cs13' from urine. Quantities of from 5 pc. per 1 liter to 5 curies per liter have been separated from radioactive cerium and strontium by an adsorption of the Cs137on bentonite clays (314). Vermiculite (1013) and montmorillonite and kaolinite (420) columns have also been used to adsorb
CsI3' froin aqueous solutions. Cs134 has been separated from radioactive sodium by an acid elution of a cation resin column (1224). I o D I I ~ 132. E-~~ Kozyreva-Alkesan~, drova and Temnikova (626) review the chemical properties of and report methods for its separation. Maeck and Rein (734) describe a method of cation evchange and heterogeneous isotopic exchange to determine in fission product mixtures. StiennonBovj and Geladi (1106) have separated from ?'e132 by a chromatography method. Gas-cooled reactor effluents have bren analyzed by Reed, Myers, and Sabol (973) for several of the short-livcd iodine fission product isotopes. Brooks (169) and Eiland (302) report on distillation inethods for the deterniination of in urine. Alilk ( 6 R I ) , plasma (303), vegetation, thyroid glands, and natural waters (1155) have also been analyzed for Other methods for the determination of radioiodine have been reported by Hunter and Perkins (493), Jawakowski (536),and S a k a i and others (851). TECHSETICX-99A S D LIOLPBDENUM99. The solvent extraction behavior of septivalent technetium has been studied by Boyd and Larsen (152). Immiscible organic liquids, including alcohols, ketones, etherq, esters, nitro compounds, nitrites, amines, hydrocarbons, chlorohydrocarbons, and organophosphorus and organic-nitrogen compounds dissolved in nonpolar liquids, Jyere used in these studied. Boyd and others (163) separated Tcg9 from neutron-irradiated molybdenum by techniques involving either volatility, solvent extraction, reduction by metals in acid and alkaline solutions, or coprecipitation. Coleman and others (239) have used solvent extraction to separate Tcg9 from fluorination plant residues. Kuzina and Spits! n (641) have used a sulfonate cation exchanger (KU-2) to separate C060, W 3 7 , Zn6j, and Zrg5from Tc99 in an acid qolution a t p H 2. Pirs and Magee (9 $2) have used anion resins to separate Tc, Re, and N n . Love and Greendale (710, 711) report on a polarographic method of determining Tc and Ru fission product mixtures. Alckseev and Polevaya (26) and Maeck, Kussj-, and Rein (733) report on l f o g 9from fission product mixtures by solvent extraction methods. RU~HESICM-106. Brown and Kaylor ( 1 ? 1 ) , Saylor (862), and Aleadoms and others (776) have evaluated distillation methods for separating ruthenium radionuclides from reactor fuel solutions. Butler (193) reports on a number of sulfide preripitation methods for radioruthenium. Quantitative separations of radioruthenium from acid solutions of mixed fission products were accomplished by precipitating the sulfides either with thio-
acetamide, thiophenol, p-mercaptopropionic acid, or 2,3-dimercaptopropane. Mercuric sulfide precipitations have also been used to collect Ru106 from fission product mixtures (616). Cation exchange resins have also been used to separate Ru106 from other radioactive nuclides (450). Love and Greendale (710, 711) have made a polarographic determination of Ru106 (and Tcgg) in fission product mixtures. T E L L U R I U J IEakins, - ~ ~ ~ . Robson, and Stockley (297) have shown that H2Te is evolved when irradiated uranium is dissolved in HC1. Using this method, TeI3*has been separated from most of the fission products by continuously adding 6 X HC1 and telluric acid carrier to the solution and sweeping the evolved H2Te gas into a 5% FeCl-3M HC1 solution with nitrogen or helium. Metallic tellurium and the Te132 are precipitated from this solution with dnC12 solution and then converted into the desired chemical form. Stronski and Rybakow (1113) report on the use of an ion exchange method to separate radioactive tellurium, tin, and antimony. Nariko (760) has used a solvent extraction of an HC1 solution with 20% tributyl phosphate in kerosine to separate Te(1V) from Te(V1). ARSENIC-78. Kjelberg and Pappas (698) have isolated fission product arsenic-’it; by distillation and determined its yield from the thermal neutron fission of uranium. Z I R C O I i I U ~ I - 9 5AND KIOBIUM-95. AIilner and Edwards (793) have recently reviewed the analytical chemistry of zirconium. Zrg6 has been separated from citrate solutions of fission product mixtures by elutions of anion resin columns of Dowex 21K with either HK03, HC1, HC104, or IYH4C1 solutions (583). Hardwick and Bedford (442) report on the tributyl phosphate extraction of Zrg5 (and plutonium) from 4 to 6LV “03 solutions. Zrgj (and Nbgj) have been recovered from acid solutions by extractions with flavanol in diisobutyl ketone (667) and with tributyl phosphate (986, 1145). Low and Andersson (115) describe a method for the determination of Zrg5(and Kb99 in soils, and Meadows and hlatlock (775) report on a method of determining radiozirconium in fission product solutions of irradiated plutonium. Other methods of determining radiozirconium have been suggested by Hunter (491), by Hunter and Perkins ( 4 9 4 , by Leaf (656), and by JTallace (1180, 1181). Kb95 has been electrochemically separated from Zrg5 (79) and from Tals2 (407). The adsorption-electrochemical method of Balashova and Merkulova (79) employed platinum and steel electrodes to separate pure niobium from dilute H I 0 3 and HF solutions. Methods for the determination of Kbg5 in eXluent plant solutions (1159) and in
vegetation, seaweed, fish-flesh, and natural waters (1162) have also been reported. Removal of S b g 6from solutions containing Zrgj by adsorption upon Vycor glass has also been reported (817). I n studies using Nbg5 and Talg2 tracers, Aleksondrova and Chmutov (25) have separated Nbg6from Tals2 by eluting activated charcoal columns, saturated with phenylarsonium acid, with 4y0ammonium oxalate and 0.65M HC1. Citric and sulfuric acid solutions have also been used as eluents in separating NbgSand Tala2by an ion exchange method (1084). Alimarin and Borzenkova (28) have also used Nb96 tracer in ion exchange chromatography studies on the separation of K b and Ta. I n another tracer study, Kbg6has been separated from Tala2 by an extraction of a 370 tartaric acid solution with a 10% alcoholic solution of n-benzoylphenylhydroxylamine (29). Niobium can be rapidly separated from tantalum a t a p H of 4 to 6 in ratios of Pl‘b:Ta of 1OO:l and 1:100. RAREE.4RTHS AIiD YTTRIUM. Several articles giving a general description of radiochemical methods for separating the rare earth group from other elements have been published. Llironov and Odnosevtsev (796) report on extractions of the rare earth elements from slurry. Other articles (290, 293, 755, 766, 956, 1046) describe chromatography separation methods for the rare earths. Lindner and Johnson (700) have adsorbed radioactive rare earths from nitrate melts on alumina and Pyrex glass. Zimmerman and Ingles (1,941) have isolated some of the rare earths by a chlorination and volatilization procedure. Broadbank and others (164) have shown that Ce144(and Cs137and Sr90) can be removed from solution by a preformed precipitate of ammonium 12molybdophosphate. Uranium oxalate has been used by Bykhovskii and Grinberg (196) to separate Ce144from other fission product radionuclides. Ce144 (and YQO)have been separated by Butler and Ketchen (194) by a solvent extraction method. Hunter and Perkins (496) and 11Ieadows and others (776) describe other methods of determining Ce144 (and/or Kd147 or Prnl4’). Specific methods for separating Ce144(and Nd, Zr, and Th) from aluminum (1180, 1181),Ce144from effluent plant solutions (1156),and Ce144in vegetation, seaweed, fish-flesh, and natural waters (1154) have also been described. Lanthanum-140 (and other lanthanides) have been separated from fission product mixtures by a method of isotopic and nonisotopic carrying and ion exchange (36). Inactive lanthanum n-as used as a carrier for fluoride and hydroxide precipitations of all the lanthanides formed. Clanet (%%?), Edge (399), and Hulet and others (488)
have reported on anion exchange studies of the rare earth elements. Trioctylamine-treated paper has been used in a chromatographic separation of lanthanum and other rare earth elements from thorium and uranium (215). La140 (and Sm’53 and YW) have been separated from other radio-activities by oxalate precipitations (165). Iofa (506) has used a method of internal electrolysis to separate La1@from ThC and RaE. Stary (1097) has extracted lanthanum from acid solutions nith benzoylacetone. Promethium-147 has been separated from other fission products (Zr”-Xbg5, Ru106-Rh106, Sr90-Yg0,Cs137 and I3l) and from Co6O and Np23gin urine by coprecipitations on basic phosphate precipitates (21). Another method of separating Pm147 from fission products has been reported by Britt (163). Nd147 has been separated from Pn1l4’by use of ion exchange chromatography and EDTA complexing agents (664). tracer to Braier (167) has used develop a separation method for microquantities of europium and other rare earths in uranium. By use of cation exchange resin and elutions with 6-11 HCl, it was s h o m that the rare earths would adsorb and that they could be separated rapidly from uranium which did not adsorb on the column. Eula4 (and have also been separated from fission products by a coprecipitation on lanthanum oxalate (411). Lanthanum oxalate has also been used to separate Y90 from fission product mixtures (412). Xore specific methods for separating these lanthanide elements and yttrium in seaweed, vegi>tation, fish-flesh. and natural r a t e r s have been described elsewhere (1160). FISSION GASES. Rapid methods of separating radioactive fission gases have been described by Koch and Grandy (608) and by Townley and others (1132). A gas chromatographic method of analysis for radioactive gases has bf.en described by Kritz (630). Prakash (954) has recovered Xe13’and KrgOfrom fission gas mixtures, and Rider and Peterson (979) describe a method of recovering Kr95 from nuclear reactor discharges. Lenis (693) reports on a method of analyzing natural gas for Kr8j and H3. URASIUJI. Kuznetsov, Savvin, and Mikhailov (644) review the more recent advances that have been made in the analytical chemistry of uranium (and of T h and Pa). Xotojami, Onishi, and Hashitani (834), Markov and others (752), and Soister and Conklin (1085) also have published bibliographies on analltical methods for uranium and/or thorium. Bauthier, Sontag, and Chesne (100) have separated from solutions of irradiated thorium by a solvent extraction with 307’ triaurylamine-HC1 mixture. Trioctylphosphine oxide in toluene has also been used to extract U233 VOL 34, NO. 5, APRIL 1962
0
147 R
from HC1 solutions of irradiated thorium (522). Ishimori and Sammour (617) and Pushlenkov, Komarov, and Shrivalov (965) have also used solvent extraction methods in separating and studying the behavior of U233. Burger and Roake (185) report on the extraction behavior of uranium as UOz(N03)2. Methyl ethyl ketone and carbon tetrachloride have been used to extract uranyl nitrate (645). Codding, Vondra, and Zebroski (854) report on the decontamination of irradiated U235 from fission products and plutonium by solvent extraction. Uranium in fluorination plant wastes (859), in urine (169), in thorium, cerium, phosphate, copper, and nickel mixtures (586), in plutonium, ruthenium, and zirconium mixtures (605, 604), and in thorium and protoactinium mixtures (505) has been separated by solvent extraction. U+4 and U+6 have been separated in HCl solutions by extracting with a diisoamyl ether-methylphosphoric acid mixture (104). The anion exchange behavior of U+6 in sulfate and carbonate systems has been studied by Khopkar and De (584). HCl, HzS04, Hxoa, HC104, NaC1, NHdC1, NaN03, and Xa2S04were used to elute the uranium from a Dowex 21K column. I n the sulfate system, U is separated from cerium, vanadium, cesium, silver, cadmium, and zirconium. In the carbonate system, it is separated from phosphate and molybdate. Khopkar and De (585) have also used the cation exchange resin, Amberlite IR120, to separate milligram amounts of uranium from thorium, zirconium, cerium, copper, nickel, and phosphate. H2S04, acetic acid, and HC1, ” 0 3 , citric acid were used as eluents. Sodium carbonate and bicarbonate solutions have been used as eluents to recover uranium from an anion exchange resin (624). Amberlite IRCdO resin with EDTA solutions as eluents has been used by Krawczyk (687) to separate uranium from rare earths. Dietrich, Caylor, and Johnson (881, 282) in their analyses of urine report that uranium can be adsorbed upon a glass-bead column impregnated with tri-n-acetylphosphine oxide. Uranium in H N 0 3 solution has been separated by a method of reversed phase-partition chromatography (441). Samartseva (1011) and Khlebnikov and Dergunov (582) have separated uranium (and Np, Pu, and Am) by electrolysis. Microquantities of uranium have been determined in urine by precipitation with tannic acid and hexamine (1183). Other articles that have been published describe methods to determine submicrogram amounts of uranium in mixtures of milligram amounts of iron, aluminum, and plutonium ( I S O ) , in aqueous solutions (1182), as contamination on completed reactor fuel as148 R
ANALYTICAL CHEMISTRY
semblies (790), in U-Pu fission element alloys (651), in low enriched, nonirradiated UOn pellets (779), in “burnup” analyses of irradiated natural uranium (723), and in vegetation, soil, and water (570).
mend a simple radiochemical method for the production of Pa234 from Th234. Anion resins-HC1 exchange systems have been developed by Starik Sheidina, and Il’menkova (1095) and by Pluchet and Muxart (948) to determine protoTHORIUM AND PROTOACTINIUM. actinium in aqueous solutions. Solvent Motojami, Onishi, and Hashitani (854), extraction methods of determining PaZ3l Kuznetsov and others (644), and in water and sediments (1009) and of Ryabchikov and Balbraikh (1002) have separating Pa232from irradiated thorecently reviewed the analytical chemisrium (743, 769, 1086) have also been try of thorium. The article by Kuznetreported. SOY and his coworkers (644) also reviews NEPTUNIUM, PLUTONIUM, AKERICIUM, the chemistry of protoactinium. CURIUM,AND CALIFORNUM.A survey Matsumoto (‘758)describes radioof the different methods used in preparchemical methods that are useful in deing and analyzing the transuranic eletermining thorium isotope ratios. Artiments has been given by Thompson cles describing specific separations of (1188). Ion exchange and solvent exthorium from uranium process streams traction methods have been most fre(953) and from aluminum (1180, 1181) quently used in separating the transuranics either as a group or singly. have also been published. Quantities of thorium as small as 2 pg. have been Choppin and Chetham-Strode (228) determined in urine by initially prehave used anion resins to study their cipitating the thorium with ammonium behavior in hydrochloric acid. A group hydroxide and then dissolving the preseparation from the lanthanide elements cipitate in HC1 (at pH 4.2) and extracthas been reported by Hulet, Gutmacher, ing the thorium from the acid solution and Coops (488). In this study, the with chloroform (658). Thorium has mixture was adsorbed on either 2, 8, or been separated from uranium by ex10% DVB resin and the separation tracting thorium phenylacetate from made by elutions with 10M LiC1. the mixture with diethyl ether (1158). Moore (815) has effected a separation Azine extractions have been used to of the actinide and lanthanide elements separate thorium from the rare earths by use of trioctylamine extractions of (1118). Ichikawa and Uruno (505) hydrochloric acid solutions. Tributyl have shown that thorium cannot be phosphate extractions have been used to extracted from a HC1 solution with separate and isolate neptunium, pluan Amberlite LA-1-kerosine mixture. tonium, and americium (and Th, Pa, However, extraction coefficients of 200 and U) from HNO, solutions (578). for uranium and 60 for protoactinium Mitchell (798)reports on an electrodepohave been obtained for this system, and sition of the actinide elements in tracer they propose, that this is a usable concentrations. Khlebnikov and Dermethod for separating uranium and gunov (586),Samartseva ( l o l l ) , and protoactinium from thorium. Buddery, Yakovlev and others (1235) also report Jamrack, and Wells (186) also report on separation of neptunium, plutonium, solvent extraction systems for thorium. and americium by electrodeposition. Berman, McKinney, and Bednoc Akaishi (21) reports on the separation (115) report on the separation of ThZa4 of Np239 from urine by a method of from uranium by an ion exchange coprecipitation upon calcium or magmethod. The uranium complex in nesium phosphates. Other fission prod9.6M HCl is adsorbed upon the column ucts and Cow were separated in the same and the Th234washed through the resin manner. Lanthanum fluoride (855) has bed. Strongly basic anion exchangers also been used as a coprecipitant for have been used to determine the distrir y ’ ~ 2 3 7 * ~ 3 ~Kondratov . and Gelman (614, bution of thorium chlorides in alcoholic 615) have used oxalate and phenylHC1 solutions (625). Dowex 1 resin arsonate precipitations to separate Np and elutions with 90% methanol-10% (IV) and Sp(V1) from other radioactive 5N “ 0 3 have also been used to sepaelements. Bagnall and others (77) rate thorium from mixtures of uranium report on the separation of neptunium (622). Cation exchange resins and (and plutonium) by acetamide complexing of tetrachlorides. EDTA have been used to separate Buchanan and others (181) report thorium from solutions of low grade that 1 p.p.m. of neptunium can be ores (1109). Cerrai and Testa (215) report on the separated from pure plutonium by exuse of a chromatographic separation of tracting Np(1V) from 12M HC1 soluthorium from uranium by means of tion with 0.5F mono (2ethylhexyl) orthophosphoric acid-toluene mixture. paper treated with tri-wactylamine. An addition of 0.lM hydroquinone and Khlebnikov and Dergunov (582) have 0.1M K I were made before extracting used electrodeposition methods to sepato keep neptunium in the quadrivalent rate and produce thick layers of thostate and the plutonium in the trivalent rium (and u, Np, Pu, and Am) upon metallic plates. state. Di(ethylhexy1)phosphoric acid Carswell and Lawrence (911) recom(856) and dodecylbenzenesulfonic acid
(858) have been used to extract h'p237J39 from mineral acid solutions. XpZ3' and/or Np239 have been separated from plutonium metal (1079),from irradiated uranium (857, 91S), from fluorination plant residues (239), and from transuranic element mixtures (31) by solvent extraction. Akaishi (20) has also used an ion exchange method and a basic precipitation to separate ?Xp239from aqueous solutions of the actinide elements. Laggis and Schmitt (646) report on a similar method of separating Kp237. Plutonium has been separated from fission product mixtures by coprecipitations with lanthanum fluoride (11621, lanthanum oxalate ( 4 l S ) , and as tetrachloride acetamide complexes (77). Tributyl phosphate has been used to extract plutonium (and zirconium) from 4 to 6 S "03 solutions (442, 521). Tri-n-octylamine (1056), TTA ( l l 8 4 ) , and dibutyl phosphate (101) have also been used in isolating and separating plutonium by solvent extraction. Anion exchange methods of separating P u + have ~ been reported by Buchanan and others (181) and by Jackson and Short (628). Ahrland (17) describes a method of separating plutonium and fission products from irradiated uranium by means of silica gel columns. Other articles report on the separation and determination of plutonium in urine (169, 1194), in irradiated UOz (594), in uranium pitch ore (1094),in uranium fission product mixtures (130, 1187), in radioactive effluent solutions (1021), and from nickel-bearing samples (341). Plutonium has also been determined in radioactive mixtures by a spontaneous fission method (200) and by gamma spectrometry (1156). Americium-241 (and Eu1j4)have been separated from other radioactive materials by a lanthanum oxalate precipitation (411). Liquid-liquid extractions, with such extractants as dibutyl phosphate in different organic solvents, have been used to effectively separate Amz4' from fission product mixtures (101,296). Twenty-five (25) micrograms of Am241 has been separated from large amounts of plutonium by use of an anion resin column (181). The Am241and the plutonium were adsorbed upon the column solutions from a 12N HC1-0.114' "03 and Pu separated by elutions with 1N HCl. Other ion exchange methods for separating Am241have been reported by Lebedev and Yakovlev (667) and Starik and Ginzburg (1092). Holst and Barrick (481) have used a mercury cathode electrolysis method to purify americium chloride solutions. Americium (and P u and Kp) have also been electrochemically separated by Khlebnikov and Dergunov (582) and Samartseva (1011 ) . Gamma spectrometry has been used by Maly and others (744) to determine Am241in plutonium solutions.
Curium(II1) has been separated from americium(II1) by an anion exchange method involving the insolubility of their lactate complexes (667). Issac, Wilkins, and Fields (626) have separated californium from large quantities of curium in 12M HC1 by a n extraction with 100% TBP. Californium has also been separated from the lanthanide fission products by use of Dowex 50 cation resin and EDTA complexing in aminopolyacetic acids (363). RADIUM AND RADON. Fourniguet, Jeanmaire, and Jamnet (346) have quantitatively coprecipitated micromicrocuries of radium from urine on a BaS04 precipitate. After mixing the precipitate with zinc sulfide, the radioactivity mas measured by scintillation counting. Goldin (393) has separated dissolved radium in public water supplies by coprecipitations with barium and lead sulfates. EDTA was used as a precipitant to recover Bas04 from a nitric acid solution of the sulfates. R a E has been separated and purified from HCl solutions of RaD, its daughters, and Pb, by an electrolysis-paper chromatographic technique by Conte and Muxart (244). A nickel strip absorbs the RaE, Po, RaD, and P b from the solution. After dissolving the absorbed materials from the nickel n-ith H N 0 3 and placing the solution on a paper chromatogram, descending and ascending chromatography is used to separate R a E from the mixture. Klumpar, Majerova, and Jirousek (602) report on a method of electrodepositing 6.3 X gram of radium from water and measuring its concentration by counting the decay products of radon by a scintillation counter. Radium has been separated from barium by electrolysis with a mercury cathode (618, 619). Radium isotopes have been determined by quaternary amine extractions from aqueous solutions (608). Other methods of determining RaZz2and Razz8 in various materials have been reported by Baratta and Herrington (89), Brooks (169), Higgins and others (470),Weiss and Lai (1192),and Zharov (1239). Petrom and his associates (931, 932) radiochemically separate and determine the isotopic composition of radium in uranium melting process samples. Radon has been separated from radiomesothorium by Ziv and Volkova (1246) and has been determined in liquids and slurries by Greig (416). LEAD, POLONIUM, ASTATINE, AND BISMUTH. Lead412 has been separated from thorium by absorbing a slightly acid solution of the mixture upon a n ion exchange resin and eluting with distilled water (402). Ancarani and Riva (60) and Ziv and Sinitsyna (1244) report on a rapid electrodeposition of Poz10 from radioactive minerals.
Moore (813) has used trioctylamine extractions to separate P o w from mineral acid solutions of bismuth targets. Matsuura and others (769) have extracted Po(1V) from acid solutions with hexone. Other articles report on the separation of Pozla from urine (169), efRuent treatment plant solutions (1167), and acid solutions of thorium (872). Belyaev and others (109) report on a solvent extraction method of separating astatine from lead, bismuth and thorium targets irradiated by 660m.e.v. protons. Lima and Abrao (696) have shown that bismuth-210 could be separated from radiolead by a precipitation method using E D T A as a complexing agent. ACTINIUM. Foster and Fauble (346) have prepared milligram amounts of AcZz7from purified salts by a lithium reduction of actinium fluoride and a volatilization of the actinium. Farabee (323) has separated actinium from inactive lanthanum carrier by use of a cation eschange resin column and eluting the lanthanum from the column with citric acid a t p H 3.2. Lavrukhina, Kourzhim, and Filatona (664) have separated and determined AcZz3 in natural minerals by measuring the radioactivity of its Fr223 daughters. Actinium isotopes have also been determined in uranium mill effluent (88) and in the presence of actinium X (1096).
RADIOCHEMICAL ANALYSIS OF OTHER RADIONUCUDES
Tritium. Foskett ( 3 4 4 , Okano (899), and Trusov and Aladzhalova (1137) generally describe the methods used to detect, separate, and measure H3. Peets, Florini, and Buyske (924) have described a method involving a rapid dry combustion technique for the determination of tritium in biological materials. H3 has been separated from C14 by processing neutronirradiated phenylalanine by a paper chromatographic method (90). Osinski (903) has reported on the use of paper chromatography in the assay of H3labeled compounds. Lewis (693) reports on the use of a gas chromatography method to determine tritiated methane and Kr6 in natural gas. Methods describing the analysis of urine (169, 194, 1144, 1151) and water (194) for H3 have also been reported. The reports cited elsewhere for the radioactivity measurement of HS also contain information on radiochemical separations of tritium. Carbon-14. Cacace and others (197-199) report on a chromatographicradiometric analysis of determining C'4.labeled substances. The method is based on the continuous combustion of radioactive compounds flowing from VOL. 34, NO. 5, APRIL 1962
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the column as water and Con. The radioactivity of each compound separated is measured by an ionization chamber. Karmen and Tritch (560) and most of the other articles cited in the section of this review concerned with CL4 radioactivity measurements have described radiochemical separations of radiocarbon by gas chromatographic methods.
Sodium-24, Magnesium-27, Potassium-42. Typical of
and
the methods of separation used in individually determining r\TaZ4, Mg27, and K 4 2in mixtures are those ion exchange methods of Cerrai and Gadda (213) and Heyn and Finston (468). K42 (and Rba6and C S ' ~ have ~ ) been used to determine the analytical behavior of sodium tetraphenylborate in the precipitation of the alkali metals (373).
Sulfur-35
and
Phosphorus-32.
Chernyak and Navtanovich (219) have reported on the use of acid alkyl phosphates to determine S35and P32. Other radiochemical analysis methods for these radioisotopes are cited in the section of this review concerned with "carrier-free" separations. Calcium-45, -47 and Scandium-46. Pasternak and Zelenay (920)have used a focusing ion exchange method to separate Ca4Sand Sc46in trace quantities. Sc46 has been separated from fission products and rare earths by an acid elution of a cation resin column (693) and from thorium by a chlorinationvolatilization method (1241). Other articles report on the determination of Ca45 and/or Cad7 in bones (935) and neutron-irradiated carbonates (546) and on the determination of Sc46in radioactive fallout samples (628).
Iron-55, -59, Manganese-54, Cobalt-60, and Zinc-65. Hallberg and Brise (433) describe a precipitation and solvent extraction method used to determine Fe55and Fe5g in blood. Hahn and Smith (430) have used a p-nitroso, P-naphthol precipitation to determine Co60in radionuclide mixtures. C060 has been separated from )Ins4, Z i P , and Fe59 by a reversed-phase chromatography method (789). Other methods, involving anion exchange resins and HCl elutions, have been used to separate Cow from nickel (792, 1164, 1175). Krieger, Gilchrist, and Gold (629) also report on a method of concentrating and determining Co60(and Z n 9 in rainwater. Maeck (732) used diisobutyl carbinol extractions to determine ZnO5 in radioactive mixtures.
Silver-llOm and Cadmium-115, -115m. Kudo (633) uses cupric sulfide to coprecipitate Agllom from its waste solutions. DeVoe (B77) reports that radioactive cadmium can be separated with chemical yields of 78% or more from 20 different elements by solvent extraction with dithizone in basic media or by ion exchange from hydro-
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ANALYTICAL CHEMISTRY
chloric acid solutions. I n this study, Cd115 was also separated from varying amounts of radioactive silver and zinc by a vacuum distillation of elemental cadmium. DeVoe, Kim, and Meinke (278) and DeVoe, Nass, and Meinke (279) report on the radiochemical separation of cadmium by amalgam exchange.
Hafnium-182, Tantalum-182, and Tungsten-187. Vobecky and Mastalka (1174) have used a solvent extraction method in the isolation of radioactive hafnium and tungsten as the spallation products of tantalum. Kuznetsov and Titov (646) also report on a solvent extraction method for radiotungsten. Tal82 has been isolated and quantitatively separated from deuteron-irradiated tungsten by a series of radiochemical steps involving either coprecipitations upon ferric hydroxide, anion exchange resins, or solvent extraction (270). Separations of Ta1*2 from niobium (as Nb95) have been described in articles cited elsewhere in this review.
CARRIER-FREE SEPARATIONS
During 1960-61 , carrier-free separations of many radionuclides continued to be of importance. Henry (456),Jol, Jones, and Lawson chine ( 5 4 ~ 9Kahn, (552),LIayer and Anderson (766),Rowland (991), and Wish and Freiling (1226) report on the preparation of carrier-free tracers and their chemical behavior. Ifunze and Baraniak (844) hare described a method for the production of carrier-free n'aF18. Carbon disulfide and bromoform in dilute ammonia have been used as extractants of P32from sulfur targets (595). An ion exchange method is then used to adsorb P32 as the orthophosphate. The P32is eluted from the column with 0.05N HCl and then extracted from the acidified eluent with butyl acetate in the presence of ammonium molybdate. Carrier-free P32has also been separated from irradiated sulfur by passing an acid solution through a silica gel column (535). Ignited BaS04has been used by Kar and Bhutani (558) to concentrate from Cu, Zn, and Cd. The P32 was desorbed from the sulfate precipitate by small amounts of 0.1N HCl. Similar techniques have been used to obtain enriched P32 from irradiated triphenylphosphine oxide (864). Kucharski and Plejewski (632) have described a method of preparing S3%beled sulfuric acid. Burtseva and others (190) have separated in carrier-free form from deuteron-irradiated chromium by a coprecipitation upon ferric hydroxide. After the mixture had been dissolved in HCl, the iron was removed by an ether extraction. Ether extractions of acid
solutions of neutron-irradiated iron have also been used to separate Fe59 from (689). Matuszek and carrier-free Sugihara (762) have described a microchemical method of obtaining small amounts of LInS4from radioactive solutions of iron. Cos8 has been separated in carrier-free amounts from nickel by a solvent extraction method (688). Toropova (1151) has used hexacarbonyl extractions of acid to obtain carrier-free chromium radioisotopes. Carrier-free CrS1has also been prepared by de Soete, Host?, and Leliaeret (274). The preparation of arsenic radioactivities froin proton-irradiated germanium has been described by Saito, Ikeda, and Saito (1010). Baraboshkin (85)has reported on a distillation radiochemical method to prepare carrier-free amounts of the germanium radioisotopes. Tcg9, produced by proton bombardment of molybdenum, was isolated and purified chemically from Sr9O-Yg0,CsI3'Ba13', Ce144-Pr144, and If0 by an H2S04 distillation method using either HNOs or HClOa as an oxidizing agent (611). I n this same study, pyridine extractions were applied before the distillation to give a preliminary separation of Tcg9 from molybdenum and/or the fission products. Tc99m (and Kbg5 and Zrg5) has been prepared also by an electrochemical method (995). The preparation of carrier-free A 1 0 9 9 has also been reported by Ebihara and Yoshihara (298) and by Tucker, Greene, and Nurrenhoff (1140). Cd109 in carrier-free amounts has been separated from cyclotron-irradiated silver targets by a precipitation as AgI from an acid solution of the target (408). I n the same study, radiocopper has been separated from Cd1°9 by a precipitation as Cu212. Carrier-free has been prepared from irradiated palladium by Taylor (1125). The preparation of carrier-free Pd'OO, PdlOl, and Pd103from a ruthenium target and Pd103 from a rhodium target has been described by Shimojima (1062, 1063). Carrier-free indium radiotracers (either 1n1l1,In115m, or In116) have been prepared by ion exchange (919),electrolysis (921), reversephase partition techniques (937), and extraction (996). Carrier-free In1167n has been prepared by Ebihara and Yoshihara (298). Carrier-free Rhlo2 has been isolated from ruthenium targets by Kurbalov and Townley (634) and by Shimojima (1060, 1061). Munze (843) has described a method for the production of carrier-free from Te132. Carrier-free 1 1 3 2 and Te132 have been separated from neutronirradiated uranium by a fractional adsorption on aluminum oxide (1140). Duyckaerts and Lejeune (292) have shown that carrier-free separations of Ba-Sr-Y-La, Ca-Sr-Ba-Ra, and Ra2*8--Th can be obtained by passing solutions of
these mixtures through a Dowex 50 column and eluting with E D T A solutions. Ion exchange columns have also been used to separate carrier-free from Ce14* (722). Ion exchange membranes have been used to separate and concentrate carrier-free P o from SrgO-Yg0 niiltures (405). Kefedov and Toropoi a (865) have produced Re188 in a carrier-free system. Parker (917) has used a vacuum eraporation system for separating carrierfree gold radioactil itp from irradiated mercury. Carrier-free PbZl2has been prepared by Kahn and Langhorst (553) by releasing thoron from a boiling thorium nitrate solution refluwd in a Soxhlet extractor. Subbeqncntly, the thoron decays to Pb2I2n hich is washed out and retained by an ion elchange column. Ph212is purified and remoied from the reiin column by eluting n i t h 1JI HC1. RADIOACTIVITY MEASUREMENT TECHNIQUES
Iluring the past 2 y a r s many improvements have b t m brought about in the methods and equipmwt used for the detection of radioactivity. Of particular interest has been the issuance of the Proceedings of the International ;Itomic Energy ilgcncy’s Symposium on the “l\letrology of Radionuclides.” Held in Vienna In October 1959, it v a s attended by many researchers who had prime interests in radionuclide measurement methods. Typical of the metrology methods used by each participating country are those that were described by hglintsev and his colleagues (14), Baptista ( S I ) , Bochkarev and Razhenov (131), Campion (,?OR), and Grinberg (419). -4dditional information on radionuclide metrology n as presented elsenhere by h g l i n t w and his colleagues (13). Gadda (358) also reports on general techniques. the apparatus, and the experimental data obtained for radioactil ity nieayurements. LeGallic (675) ha. made siniilar obseri ations for measuring IOLT-le\ el radioactivity. Repoi tq on more spwialized radionuclide measurements include one by Bek-Uzarob and his associates (106) on the absolute measurements of Aul98. Chabre and Drponiniier (216) report a conversion factor for use in the interpretation of the beta spectra from Au198, Cllenbogen (304) I eports on counting csfficiencies for determining Coj6, COB, m d Co60by the use of a t least two different counters and three different countiiig techniques. Hull (489) describes tlvtection and measurement methods l m e d upon scintillation counting to trace water flow patterns by radioactive tracers. Ralkova (969) also reports on similar studies. Blanchard, Kahn, and Hirkhoff (128) describe a technique for the preparation of thin uniform radioactive source5 by surface absorption and
electrodeposition. Other articles of special interest include those by Herberg (459) and Jaffey (529) on statistical tests for counting. Herberg ( 4 9 ) specifically reviews methods of obtaining statistical data from liquid scintillation counting methods. Of considerable significance in the detection and measurement of radioactive species is the report by DeVoe (276). Working in conjunction n i t h the Subcommittee on Radiochemistry of the National Research Council. he has been able to provide a compilation of information about the radioactive contamination of materials used in scientific research. Besides giving information on the levels of radioactive contamination in materials used in or as a shield for radioactivity detection systems, this report also gircs data obtained in the analysis of chcmical reagents for radioactivity. Much of the information appearing in this report is of great value to those scientists interested in low-level radioactivity analysis and measurement requirements. Although the above reviews and reports and other publications mostly report on the use of Geiger and proportional counting methods, considerable emphasis has been given to scintillation counting methods in other reports published during this review period. Liquid and solid scintillators and silicon and germanium diode counters have been used in both gross scintillation counting and spectrometry determinations, I n addition, more new reports have been made on methods coordinating radioactivity measurements with automatic data processing systems. Since a great number of publications on radioactivity measurement techniques, apparatus, etc., have appeared during 1960-61, the sections t h a t follow will list only those publications of particular interest. Equipment. Counters, scintillation mechanisms, and their construction have been described by Blanc (127). Julliot (551), RIanagan (745), Silar (1073), and Strauss (1108) describe the apparatus used in scintillation counting. Whalen, Meadows, and Kelson (1,905) describe a time analyzer using a multichannel pulse height analyzer, and Parker (926) reports on the use of a n improved anticoincidence shield in low background counting. Other ideas and apparatus for automatic analysis in nuclear techniques have been described b y Desneiger (272,273),and Ludn-ig and others (718). il transistorized alpha-particle detector has been described by Ananiades and Dewdney (48). The operation and maintenance of an alpha-energy analyzing system have beendescribed by Brauer and Connally (160). An alpha counter has been constructed and its operation described by Byrne and Rost (196) for
use in the direct determination of plutonium in solution. Gonshor, Green, and lJ700d (398) have constructed a n adapter for use with a low-level beta counter to measure alpha radioactivity. Beta-gamma coincidence methods using high efficiency detectors for the measurement of radioactivity have been described by Beller (107) and Gandy (366). Gutmann and Gilat (427) report on the use of a low background beta counter equipped with a plastic scintillator as an anticoincidence shield. Parker (916) also reports on a n improved anticoincidence shield for use in low-level counting. Bradley (165) has constructed a demonstration beta spectrometer and reports on its operation. Tanaka (1124) has reported on the construction and use of a low-background beta-ray scintillation spectrometer using a coincidence method with a Geiger counter, Schneider and Liridqvist (1029) explain the equipment and techniques used in the automatic analysis of beta-ray spectra. Similar information has been given by Elliott (306) in his description of the use of standard units in automatic counting systems. Fonler and W a t t (847) report on the preparation of Geiger-Xuller tubes. A method of predetermining the deadtime of a Geiger-Muller counter has been given by Lamotte and LeBaud (648). Gas-filled Geiger counters for use in the measurement of S35(782,782), H3, and C14 (547, 780) and windowless gas-flow counters (647, 800,801) have also been described. il dipping counter has been used by Braunstein and Young (161) to measure the half life of
ux*.
Long and Mason (650) describe a scintillation counter for measuring solid H3-labeled samples. Jones, Rlallard, and Peachey (547) also describe a counter for use in the routine assay of tritium-containing samples. Equipment described for use in liquid scintillation counting include a n inexpensive disposable sample container (591), a large volume 4~ liquid scintillation detector (289).a n automatic scan device for determining H3 on paper chromatograms (209),protective strips for paper chromatograms (350), and other accessories (970). JTenzel (1191) reports on the use of a radioactive hollow cylinder in a simple standard measurement of a liquid counter tube. Lohmann and Perkins (709) report on the use of ultraviolet light irradiations to stabilize the counting rates of liquid solutes. The construction and use of liquid scintillation radiation rate meters for gamma measurements have been described by Williams and others (2212). Kelley (574) described multichannel analyzer construction. Triulzi (1135) describes scintillation counter systems using T a I scintillators in variable or 4n geometries t o measure gamma VOL. 34, NO. 5, APRIL 1962
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spectra quantitatively. Ellett and Brownell (305) describe a total absorption gamma-ray spectrometer containing NaI and plastic scintillators. Tests made on the linearity of photomultipliers (463) and on photopeak counting efficiencies for 3 X 3 inch NaI crystals (426) have been reported. Schmidt (1025) reports on the use of CsI scintillators in gamma spectrometry. Large volume detectors have been used by Anderson and Van Dilla (57) in the absolute measurement of Cs'". Large organic scintillators (184) and plastic phosphors (581) have also been used in gamma-ray spectrometry. The principles of use, construction, and applications of silicon diode counters in radioactivity measurements have been reviewed by Ryvkin and others (1008). Germanium and silicon diode counters have also been used by Engler (314) to detect beta radiations. A stack effluent radioisotope monitor has been used by Harvey (4.48). The apparatus and the techniques employed are described and some of the experimental data obtained are also reported in that article, Alpha Radioactivity Measurements. Methods of measuring alpha-emitting sources have been described by Engelmann and Capgras f312), by Halden and Harley (4S1), and by Pingel (9.41). A report (1158) has been made on a method of determining total alpha radioactivity in feed solutions. Gerardi (374) reports on the manufacture and calibration of primary standards for alpha counting. Adams and Richardson (6) have analyzed bauxite for thorium and uranium by alpha counting. Aleksandrov (24) has determined small amounts of thorium in tungsten and molybdenum by alpha counting on ZnS-silver-activated screens. Similar techniques were used by Isabaev, Asylobaev, and Cherdytsev (524) in determining actinium in minerals. Low specific alpha activities have been determined by Hill (472) by means of alpha spectroscopy. Bernhard and others (116) and Olkowsky and Cohen (901) have used alpha spectroscopy to determine U236enrichments in various materials. Bertrand (117) also reports on the use of an alpha spectrometer to determine Pu239in irradiated natural uranium. Silicon diode detectors have been used by Chetham-Strode, Tarrant, and Silva (221) in alpha particle spectroscopy of the transuranic elements. Fleury and others (839) report on the use of CsI(T1) scintillation crystals in alpha particle spectroscopy. Beta Radioactivity Measurements. GEIGER-AfULLCR Ah'D PROPORTIONAL COUNTERS.Christman ( Z a g ) , Radosewski (966), and Steinberg (1100) discuss
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beta radioactivity measurements in their reports on counting methods for the assay of radioactive samples. Christman (229), in particular, reports on methods of detecting and measuring low-energy beta radiations. Abecasis (S), Baptista (81), Sanchez del Rio, Reynoldo, and Radriguez (1015), and Vasilev, Petrzhak, and Sushchovskii (1166) report on the determination of absolute beta radioactivity by GeigerMuller counters. Corompt and Bouchez (247) use 4n scintillation spectrometry for absolute beta measurements. Cross (262) uses thin scintillation crystals for low-level beta counting. Rapid methods for identifying 8-ray emitters and beta-radioactive impurity dosage have been described by LeGallic, Legrand, and Grinberg (676). Experiments on the determination of the attenuation of beta radiations in thick radioactive sources have been described by Anokhin (60, 61), by Fedorov (326), and by Lerch and Vogel-Ludin (684). Graphs and tables currently used for the measurement of beta-emitters by Geiger counting methods have been presented by Scaroni and Triulzi (10.90). Geiger-Muller counters have been used speciiically for the determination of C1402by Boyce and Cameron (150) and by Kalab and Broda (555). Adamski, Bouzhyk, and Jozefowicz (8) report on the determination of Na and K by beta measurement. Beta counters have been used by Behounek and Zelnkova (105) to analyze liquids for radioactivity, The radioactivity of tritiated water vapors has been determined in a GeigerMuller counter by Cameron and Puckett (205) and by Fry (351). Other tritium-labeled substances have been rapidly assayed by Rorrland, Lee, and White (992) and by Tykva (1142) by use of a Geiger-Muller counter. The use of a Geiger-Muller counter to measure beta radioactive gases has also been described by Bochkarev and Bazhenov (131) and by Grinberg (417, 418). Cicorone, Thomas, and Verly (252), Garnett, Hannan, and Law (367), Ohno and Morimitsu (887),and Rowland, Lee, and White (992) have used a proportional counter to measure gaseous H3. A proportional flow counter has also been used to measure S35 radioactivity (504, 542) and to measure CI4 and H 3 in films (523). LIQUID SCINTILLATIONCOUKTERS. The principles of scintillation counting and the counting equipment used have been reviewed by Bush (191), Hamada (43S), Koechlin (609), Loveridge and Thomas (71S), Nisnevich (875), Ott (Q08),Owen (Q11), Ryves (loo?'), and Upson and Brown (1147). Basic considerations for the use of liquid scintillation counters in the determination of low-energy beta particles have been presented recently by Kawai and
Nishiwaki (567). Jozefowiez (550) and Shahani (1050) report on the use of liquid scintillators in determining absolute beta radioactivity. A liquid scintillation counting method to identify beta-emitting isotopes has been described by Hutchinson (499). Organic solutes such as ethane (78), butane mixtures (285), 2,5-diarylsubstituted thiazoles (579), dialkylamines (580), l-octadiene (846),paraoligo phenylene (861), trirnethyl bromide (1030), benzene (1122), and phenylethylamine (1227) have been used as scintillators in liquid scintillation counting. Bray (162) suggests the use of various liquid scintillators in liquid scintillation counters to measure the radioactivity of aqueous solutions. Scintillating gels (465, 1051) and ion exchange resins (4.54)have also been used as scintillators. Quenching corrections within liquid scintillators can be estimated by the method proposed by Bruno and Christian (177). General information on the use of a liquid scintillation spectrometer to determine the absolute disintegration rates of low-energy beta radiations has been given by Horrocks and Studier (484). Werbin, Chaikoff, and Imada (1199) and Whkman, Eccleston, and Armstrong (1206) also report on the use of a liquid scintillation spectrometer in radioassays. Recent developments in the use of liquid scintillation counters in counting biochemical samples have been described by Davidson (263) and in the analysis of labeled organic compounds by Korchunov and Xovotorov (620). Scintillation counters equipped with coincidence circuits have been used by Kohegyi, Csanyi, and Levay (6101, Sandalls (1016), and by Sigmond and Schjetne (1072). Methods for the scintillation counting of paper chromatograms have been reported (371, 708, 1121, 1198). The automatic recording of paper chromatography radioactivity data has been described by Martalogu, Nascutiu, and Scintere (753). Liquid scintillation counters for use in assaying H3-containing substances have been described by Sedei and Higashimura (1044). H3-labeled organic compounds have been separated by vapor phase chromatography (198, 199, 283) and the tritium radioactivity measured by liquid scintillation counting. The liquid scintillation counting of tritiated water has been described by Cameron and Boyce (204). Sandalls (1016) and Sigmond and Schjetne (1072) describe coincidence liquid scintillation counters for use in the determination of H3 in urine and mater. A liquid scintillation counting method for determining H3 a t 22' C. has been described by Hutchinson (496). Kaufman and his associates (571) report on the low-level determination of
tritium in various substances by liquid scintillation counting. Foskett (34.4) and Okano (899) also describe methods for detecting and measuring Ha. Liquid scintillation counting has also been used to determine small amounts of Ha in biological samples (676, 924), in urine (199, 383, 498, 1199), in labeled organic compounds (330, 1,906, 1a07), in water (199, 662), and on paper chromatograms (209,903,1198). A method, using scintillation radioautography of H3-labeled compounds on paper chromatograms, has been described by Parups and others (918). Bousquet and Christian (146), Jenkinson (643), Kasida and others (666), Jeffay and Alvarez (541) Maimind, kerman, and Rfeiman (7371, Nygaard (889), Tamers (1122), and Tamers, Stipp, and Collier (1123) describe liquid scintillation methods for the determination of C14. C14 has been determined by liquid scintillation counting (540) and methods in the presence of in the presence of P32in tissues and blood (76). A liquid scintillation method has also been used to measure natural CI4 in a radiocarbon dating system (265, 1091, 1124, 1123). C14-labeled salicylic acid has been separated by paper chromatography and by vapor phase chromatography (197, 199) and the CI4 radioactivity of the separated compound measured by a liquid scintillation method (145). AqueQUS solutions of C14-labeled bicarbonate, obtained in the analysis of biological materials, have also been assayed by liquid scintillation techniques (178). Blood and tissue (390, 458), other biological samples (676), paper chromatograms (288, 1121), and low-boiling fluids (330, containing C14 have been analyzed by liquid scintillation methods. 0402 has been determined by Moss (933) and by Roeller (1227) by liquid scintillatioii counting methods. Moss (835) also reports on a rapid mechanism for the routine liberation and trapping of the P40,. Labeled-carbon dioxide has also been determined in aqueous carbonate solutions (444,. Ludwicli (718) reports on liquid scintillation spectrometry to determine Zrg5-Kbg5and a method of coincidence standardization of these isotopes. Pm147 in fission product mixtures has been determined by Britt (163) by use Qf a liquid scintillation count method. Gleit and Dumot (591) have used a liquid scintillation counter to measure the beta radiations of N P . Liquid scintillation counters also have been used to detect and mcasure the beta radioactivity of radioactive metallic elements (315),or radioautograms (371), and of aqueous samples (399). Liquid scintillation techniques have also been applied by Ludwick and Perkins (719) to counting phosphoresence emissions t o
determine trace quantities of zinc sulfide. COUNTING WITH PLASTIC OR ORGANIC SCINTILLATORS. Andruszkiewicz, Kuzama, and Polacki (69), Basile (91), and Brownell (172) describe applications of plastic scintillators in the analysis of radionuclide mixtures. Boyce, Cameron, and Taylor (161) have measured tritiated hydrogen in a simple plastic counter. The beta radioactivity collected on filter papers has been determined by a scintillation count by means of organic phosphors (366, 357). OTHER COUNTERS. Silicon (314, 1008) and germanium diode counters (314) have been used to detect and measure beta radiations. Takahashi (1119) reports on the use of ionization chambers to measure tritiated water. G a m m a Radioactivity Measurements. Although gross gamma counting methods continue to be used, many more reports have been published on the use of gamma spectrometry in analysis. For instance, a bibliography on applications of radiospectroscopy has been made available (118). Crouthamel(254), Gatrouis and Crouthamel (369), and Sweitzer (1117) very aptly present the techniques of applied gamma-ray spectrometry and give gamma-ray spectra for most of the radionuclides. Anders (54) and Kamemoto and others (556) have also issued reports showing the gamma-ray spectra of some neutron-activated elements. Descriptions of the techniques and apparatus, and reports of some of the experimental data obtained in the use of a gamma spectrometer and a multichannel analyzer in analysis h a r e been made by Brooke (168), Cianflane and Triulzi (231), Engelmann and Vagner ( S I S ) , Gadda (958), Harris, Hamblen, and Francis (445), Leveque (685), Lima (698), Ljunggren (702, 7039), Managan (746), May (7631, and Samsahl (1014). Novakora and Silar (8799) report on the detection of extremely low gamma activities with scintillation detectors. Gunnink and Stoner (426) report on the photopeak counting efficiencies: for 3 x 3 inch solid and well-type NaI crystals. Anderson and Van Dilla (57) report on the calibration of scintillation detectors for the absolute measurement of Csl*’. Special gamma-counting methods involving the counting of annihilation radiations (243), the continuous analysis of gamma radiations from hot radioactive liquids (416), the resolution of gamma spectra from fission product mixtures (938), and the use of large organic scintillators (184) have also been reported. Bate and Leddicotte (94) describe a complement-subtraction method of gamma-ray spectrometry for use in resolving complex mixtures of gamma-emitting radionuclides. Watanabe (1188) gives special information
about the effects of large amounts of beta radioactivity in the measurement of gamma radioactivity by means of a gamma spectrometer. Gamma spectrometric methods, usually as nondestructive techniques, have been applied to the determination of uranium and thorium by Adams and Richardson (6), Avan and Keller (73, 74), DeLange (266, 267), and Iokhelson and Shitov (506). Delvin, Palmer, and Upson (268) used similar techniques in determining total uranium and U235in aluminum-uranium fuel elements. Alkire (32) has also used gamma spectrometry in the continuous analysis of irradiated uranium process systems. UZ3& enrichment in various substances has also been determined by a nondestructive gamma spectrometric method (250). The gamma spectra of plutonium-242 (f136),of americium-241 (7.44), and of fission products (761) have also been determined by nondestructive analysis. Cartwright and Robbins (212 ) report on sources of error in the determination of U235 by gamma spectrometry. The radium, thorium, and potassium content of rocks have been measured from an aircraft by means of a gamma spectrometer (80). Kaul and Muth (566) report on the determination of radium by scintillation spectrometry. Gamma spectrometry has also been used to determine radioactive contaminants in foods (361). Milk has been analyzed for 1131, Cs13’, and J3aI4O by gamma spectrometry (429). Cs13’ in KM-Cs137 mixtures (900) and in rain water (1126) has been measured by a method of nondestructive gamma spectrometry. Counting methods for determining the total gamma radioactivity in sand, sea silt, mud, seaweed, vegetation, fish-flesh, and Faters have also been described (1161). Gamma spectrometry methods, emplo>-ing 3 X 3 inch NaI(T1) crystals, have b w n used in determining neutroninduced radionuclides in radioactive rocks (I), silicon (236), and beryllium (166). Sodium and potassium radionuclides in neutron-activated materials (8) and gold in blood (280) have been determined by nondestructive gamma spectrometric methods. Mahmoud and El-Kesr (736)have measured the gamma spectra of Co60 and XaZ4 through cadmium. Radioactivity Data Processing systems. Computation process systems for resolving the spectra obtained in gamma-ray spectrometry of irradiated materials also has been seriously considered during the period of this review. Many investigations offer information on computer data processing. For instance, Rosholt and Dooley (987) report on automatic measurements and computations for the radiochemical analysis of alpha-emitting radionuclides. VOL 34. NO. 5. APRIL 1962
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Anders and Beamer (56) have used a digital computer to resolve timedependent gamma spectra of neutroninduced radionuclide mixtures. Borgholthaus (14O), Chester and Burrus (220),Henveld and Borgholthaus (467), Fite and his associates (334-336), Kuykendall and others (638-640), and West and Johnston (1200)also report on computer techniques for gamma spectral analyses. Gilbert (386) has presented a mathematical analysis system for the simultaneous estimation of several radioactive elements in a mixture. Nostrand, Favale, and Winton (877)), Nostrand and others (8781, and Rolf (985) report on computer analysis of complex gamma-ray spectra. Nostrand and others (878) report on the use of a least squares computer program. Rolf (985) and West and Johnston (1200) have used an IBM-650 computer in their work. Kuykendall and his associates (658440) and Strickfaden and Kloepper (1110) have used an IBM-704 digital computer in their work. Harvey (448) used analog computer techniques in processing his counting data and for solving the simultaneous equations derived for his I\ ork. USE
OF RADIOISOTOPES I N ANALYTICAL CHEMISTRY
Considerable interest has continued to be expressed in creating and employing analytical techniques based on the production of a radioisotope, or the phenomena associated with its decay, in analysis problems. These applications include activation analysis and radiometric analysis methods based on radioactive reagents, isotope dilution, and the use of radioactive tracers in developing analytical methods. The remainder of this review is concerned with a general summary of these radioisotope applications. Activation Analysis. T h e interest in the use of activation analysis as a technique to solve many analytical problems concerned with the determination of most of t h e elements in submicrogram or microgram quantities continues to increase. Most technical meetings concerned with analysis problems usually include a number of papers on activation analysis applications in their programs. Likewise, many new articles on its uses-at least 345-have appeared in print during 1960-61. With regard to technical meetings, i t should be noted that the International litomic Energy Agency sponsored Conference on the Use of Radioiostopes in the Physical Science and Industry, Copenhagen, September 1960, devoted a large part of its program to activation analysis. The proceedings of this meeting report the determination of sulfur
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in high neutron absorption materials by fast neutron activation analysis (381), autoradiographic determination of inclusions and segregrations in metals ( 7 8 9 , the analysis of ancient silver coins (19), the analysis of high-purity metals (23), the determination of silicon (502), and the determination of the Re-Os ages of iron meteorites (464). Special topics about the use of coincidence gamma-ray spectrometry (rod), a system of automated activation analysis (639),fast radiochemical separations (178), portable neutron generators (778), beryllium determinations with a photoneutron source of SbIz4 gammas (432), and nuclear geophysics in prospecting for ore and coal deposits (183) are also included in the proceedings of this Conference. Probably the most outstanding meeting on activation analysis held during the period cited was the 1961 International Conference on Modern Trends in Activation Analysis. This Conference was cosponsored by the International Atomic Energy Agency, The Division of Isotopes Development, United States Atomic Energy Commission, and the Activation Analysis Research Laboratory of the Agricultural and Nechanical College of Texas, and it was held at College Station, Tex. in December 1961. Papers concerned with activation techniques, gamma-ray spectrometry, computer data processing, and general and specific activation analysis applications were presented. At least 250 representatives from 16 foreign countries, Canada, Mexico, and the United States were present for the Conference. The proceedings will be issued early in 1962. With regard to published literature, it should be noted that the proceedings of the Activation Analysis Symposium sponsored by the International Atomic Energy Agency in June 1959, have now been published. Papers reporting on radioactivation analysis with nuclear reactors and particle accelerators (245, 668) in geochemistry (465),in industrial applications (686), and in biochemistry and medicine (682) appear as part of these proceedings. In addition, general applications on its use in determining minor constituents in steels (486) and in aluminum and iron (22) have also been reported. Reports on its use in specific applications for tantalum in high tantalum-ferro alloys (382), for mercury in and a variety of sample materials (104), for intermetallic diffusion in gold-lead systems are also included in these proceedings. A special report on the use of a gammaray spectrometer to determine positron and gamma-ray cascade-emitting nuclides also appears in the proceedings (703). K i t h regard to more general informa-
tion on activation analysis, i t must Le noted that many more review articles on applications have appeared during 196061. Bock-Werthmann and Schulse (132) report on the literature available through mid-1961. Gibbons and his colleagues (380) have issued a first supplement to their bibliography which was first reported by Neinke (777). Other reviewtype articles on activation analysis include those by Aten (67, 68),as well as those by Born (141), Brandt (269), Broda (166), Cornuet (246),Daabek (255j, Duyckaerts (291), Gibbons (378), Girardi (389), Hearle (453), Herforth and Koch (4629, Ionescu (507), Kauer (663), Laverlochere and Martinelli (663), Mapper (747). hlesler (784), Morris (819), Morzek (82B), Mullins and Leddicotte (841), X e s e (871), Okada (890, 691, 896), Rakovic (967), Schmitt (1026), Schulze (1036), and Vorres ( 1 1 7 7 ) . Broda (166) reviews some of the uses of activation analysis in biochemistry. Similar articles revien-ing biochemical applications have also been presented by Ogburn and his coworkers (886) and Stephens (1104). Shibuya and &higaki (1058) report on the method's use in agriculture and biology. Reiser and Schneider (974) specifically review the prospects for the use of activation analysis in the steel industry, and Baranov and his coworkers (87) emphasize its use in the analysis of pure materials. Additional reviews of its potentials in solving analytical problems for trace elements in semiconductor materials (2022) and metals (611, 828) have also been published. Erwall ( S I S ) , Klofutar (601), and Leveque (686) describe how it can be used in specific industrial problems. Revien-s on the use of activation analysis in geochemistry have been published by Napper (748), Moorbath (812), Rassoul, Langhoff, and Herr (911), Simon (8077j , Smales and Wager (IOSO),and TKnchester (1218). General and specific information on its use in petroleum exploration and research has been presented by Caldwell and hlills (201) and by Guinn and his colleagues (422-425). Burrill and associates (287, 188) and Kagner, Campanile, and Guinn (1178) discuss the use of a Van de Graaff neutron source in various applications and in materials testing and research. Colenian (237) has recently revieived the potentials of fast neutron activation analysis. Activation analysis applications by use of a source of 14-m.e.v. nuetrons have also been cited by Lbov and Kaumova (655). The use of sources of 1.5-m,e.v. protons (?68) and other charged particles (760, 1078, 1220) in analysis problems have also been discussed. General information about the use of short-lived isotopes in activation
analyses has recently been presented by Anders (53), Kamemoto and his coworkers (556), Monnier (808-81 1), S a k a i and others (852-864),Okada (896), and Pierce (936). Anders (55) also has reported on the sensitivities obtained from a Van de Graaff accelerator neutron source. Additional sensitivity data for thermal neutrons have been presented by Laverlochere (652). The activation analysis handbook prepared by Koch (BOT), first reported by Neinke ( Y E ) , has now been issued by Academic Press, Kew York, as a bound publication. It contains a large amount of information about neutron particle reactions and thcrmal neutron sensitivities. NUCLEAR PARTICLE SOURCES.Meinke's recent review on nucleonic applications (777) gave excellent summary information on the availability of neutron sources-reactors, accelerators, and low cost laboratory generators. A large number of the 1015 cost generators have been put into operation. Typical of the evaluations of the potentials of these sources in routine applications are those that have been made by Anders (53,55), Kuykendall and Wainerdi (633)) and 1Ieinke (778). Radioisotope - beryllium sources (RaBe) are still used in some activation analysis applications (636, 637). The uschfulness of Van de Graaff accelerators as neutron sources (187, 188, 237, 422425) has already been cited. Lima and his coworkers (698) report on the use of a swimming pool reactor as a source of neutrons for activation analysis applications. More recently, a series of studies has been inade by Lukens, Otvos, Wagner, a n d Guinn (721, 910) on the use of photoexcitation processes in activation analysis. Some of the radionuclides produced as metastable isomers of these processes become very specific means for determining a n element. RADIOCHEhlICAL S F P l R A r I O N S FOR Acr~va~A r oP ~ A L Y ~ I SI\Iost . of the A-uclear Science Series Jf onographs mentioned in t h e earlier portions of this article contain radiochemical procedures t h a t have been used in specific activation analysis applications. Many of the other articles cited in this review give detailed radiochemical separation procedures for the activation analysis of interest. Other sources of information on radiochemical procedures used in activation analysis include the Oak Ridge Yational Laboistory Master Analytical Manual (884). Typical of the procedures appearing in this Manual are those for antimony (664) and nickel (839). Special information about the us(' of radiochemical sciparation procedures in activation analysis (666, 667, 726, 778, 1014) and the subsequent nst' of information obtained from a radiochemical analysis in the calculation
of activation analysis data (665) also appear in this Manual. Additional information on radiochemical procedures used in the activation analysis program at Oak Ridge National Laboratory has also been presented by Mullins (837). Benson (111) has completed additional studies on the use of neutron activation chromatography to determine small amounts of phosphorus in biochemical specimens. Strickland and Benson (1111) report on the paper chromatography analysis of phosphatides in mammalian cell fractions. Goto, Ikeda, and Amano (404) report on the use of organic agents in activation analysis. Ferenczy (327) and Hainaguchi and cou-orkers (436) have used polarography in activation analysis applications. RADIOACTIVITY JIEASUREMESTS IX ACTIVATIOS AKALPSIS. hIany of the radioactivity measurements used to complete an activation analysis employ the use of a gamma spectrometer with a multichannel pulse height analyzer. Such measurements are made either as a direct analysis of the irradiated material or following the radiochemical processing of the sample. The gamma spectrometry reports by Crouthamel (254, Gatrouis and Crouthamel (369), Anders (54), and Kamemot0 and others (556) give much usable information for activation analysis applications. More specific reports on the use of gamma spectrometry in activation analysis have been given by Abdullaev ( l ) ,Adamski and others (8), Bate and Leddicotte (94), Cojocaru and others (235), Diebel and Garrett (280), Leveque (685),Lima and others (698), Ljunggren (7'02, 703),May (763), and Westermark and Sjoestrand (1203). The reports by Fite and others (334-336) and Kuykendall and others (638-640) exemplify the possibilities of using computers to process the gamma spectrometry data obtained from activation analyses. hlateosin and XcKeown (157) have provided an up-todate tabulation of the gamma-rays emitted by radioactive nuclides arranged in order of increasing energy. Dzhelepov and Peker (296) tabulate many of the decay schemes of radioactive nuclei. All of these reports are useful referencm for activation analysis applications. Although considerable intcrests exist for gamma spectrometry uscs in analysis, many of the applications cited below continue to use gross gamma counting and beta radioactivity determinations. Each of the reports cited should be consulted for the particular radioactivity measurement method used. Activation Analysis Applications. The determinations of trace elements in metals and alloys have been t h e prerequisite for a large number of activation analysis applications. Many
of the geochemical and biochemical interests in trace element distributions also are being attacked by activation analysis methods. Articles from each of these areas are specifically cited below. I n addition, articles on miscellaneous applications and specialized uses of activation analysis are cited. LIIETALS AKD h L L O Y S . Adamski and others (7-9) describe a method for the simultaneous determination of small amounts of sodium and potassium in steel and aluminum used as reactor structural materials. Ion exchange and gamma spectrometry techniques were used in these determinations. Cast iron and steel have also been analyzed for parts per million of manganese by Bouten and Hoste (146), Hoste ( 4 8 9 , Hoste, Bouten, and Adams (486), and Mori and Umezawa (818). Hoste and his associates (146, 485,486) have used an internal standard in their analyses for manganese. The results obtained in the determinations of tantalum in ferro alloys (382) and copper in steel (679)have also been reported. Parts per million or less of iron, zinc, copper, gallium, manganese, chromium, scandium, and hafnium have been determined in high purity aluminum and iron by activation analysis. Albert (22), Albert and Gaittet (23), Chaudron (218), and Gaittet (366) describe the systematic chemical analysis scheme and the gamma spectrometry methods used in these investigations. Brune (176) and Lewis (691) also analyzed high purity aluminum for the same elements; Chinaglia and Malvano (222) determined microgram amounts of copper, gallium, and manganese in aluminum; Ricci and Mackintosh (978) have analyzed aluminum for trace cadmium. Aluminum for use in reactors has been analyzed by activation analysis (1237), and hlackintosh (724) reports on the use of activation analysis to study the effectiveness of zone-refining techniques in the purification of aluminum. Sondestructive activation analyses for microquantities of Cu and M n in silicon are described by Erokhina and his associates (317). Semiconductor silicon, after a reactor irradiation, has also been analyzed by llakoskewa, JIaslov, and Obukhov (741), Rychkov and Glukhareva (1005), and Williams (1211) by gamma spectrometry. Silicon has been analyzed by Amano (44) for parts per billion of Cu, Ga, and Sb. Trace amounts of the halide ekments have also been found in the activation analysis method used by Ichimiyi, Baba, and Kozaki associates (502) and by Sozaki and others (880, 881). Silicon has also been analyzed for trace antimony, copper, strontium (235), arsenic and silver (403,569), phosphorus (530), and oxygen (882) by activation analysis. VOL. 34, NO. 5, APRIL 1962
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Germanium has been analyzed for trace selenium (396), antimony (396), and arsenic (534). Trace impurities in the parts per million range have also been determined in the activation analysis of antimony (968), selenium (893, 1052, 1211, 1232, 1248-1250), and tellurium (1052, 1232, 1248-1250). Negina and Zamyatmina (867) have determined parts per million of barium, nickel, copper, antimony, molybdenum, manganese, cadmium, tin, gold, and arsenic in beryllium. Mullins and Leddicotte (840) have found parts per million of U2a5, and Th232 in beryllium by an activation analysis method. Seyfang and Todd (1049) and Todd (1129) also found similar amounts of these elements in beryllium. Bradshaw, Johnson, and Beard (156) have used activation analysis and gamma spectrometry to analyze beryllium for trace carbon, oxygen, and nitrogen. Coleman (238) and Gilman and Isserow (388) have used a flux of tritons to determine oxygen in beryllium. Coleman and Perkin (240) describe an apparatus that can be used in this activation analysis application, Parts per million of iridium in platinum (549),palladium in platinum (589), platinum and palladium in gold (799), gold in platinum (825), osmium and iridium in palladium and platinum (824, iridium in rhodium (827), and gold and platinum in refined silver (898, 1247) have all been determined by activation analysis. Ancfent silver coins (19) and gold and silver metals (1281) have been qualitatively analyzed following a nuclear reactor irradiation. Aubry, Flechon and May (72) have shown that activation analysis is capable of use in investigating the role of microgram amounts of palladium in forming chemical deposits on nickel. Leddicotte and others (673, 674) summarize the results obtained for many of the trace elements determined in metals and alloys analyzed in the Oak Ridge National Laboratory activation analysis program. Other articles specifically describe activation analysis applications used to determine cadmium in zinc (379), tantalum in niobium (434, cobalt in Inconel (428), gold and arsenic in high purity lead (476), molybdenum in tungsten (8@), gold and other trace elements in copper (477, 478, 1230), indium and gallium in metals (510, 533), zinc and calcium in gallium ( 6 8 3 , hafnium in zirconium (898), lanthanum, samarium, and europium in manganese nodules (570), rare earths in thorium metal and thorium oxide (850), manganese, copper, zinc, arsenic, and antimony in thallium (30), holmium in rare earth oxides (436), and vanadium in various metal alloys (17 4 ) . A fast neutron activation analysis method of determining trace sulfur in 156 R
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metals has also been described (381). The intermetallic diffusion of gold in gold-lead systems (65) and the diffusion of trace elements into quartz and germanium crystals (678) have also been studied through the use of activation analysis techniques. GEOCHEMICAL APPLICATIONS.Abrao (4, 5 ) has measured the gold, copper, and uranium content of ores and minerals at the parts per million level by neutron activation analysis. Uranium238 has also been determined in ores and minerals by activation coupled with a beta-gamma delayed coincidence countr ing method (107). Fechtjg, Gentner, and Zahringer (324) describe an activation analysis method for determining argon in potassium minerals. An activation analysis method employing ion exchange after the sample irradiation has been used to determine trace rare earth elements in monazite, fergusonite, euxenite, allanite, gadolinite, and yttriolite ores (354, 366). The determinations of trace scandium (577), tungsten (945), gold and cadmium (1176-1172), potassium (1216), and copper and manganese (707) in minerals and ores have also been reported. Hamaguchi and his associates (438, 439) report on the determinations of trace copper, molybdenum, tin, tantalum, and tungsten in silicates. Rubidium has also been determined in silicate rocks (186). I-Iamaguchi and his associates (440) also reported values obtained for trace Sc, Cu, As, Sb, La, Sm, Eu, Au, and U in standard samples G-1 and M7-l. Kemp and Smales (578) reported on the Sc and V content of G-1 and W-I. Limestones have been analyzed by Haskin, Fearing, and Rowland (449) for trace U233by measuring the gaseous Xe133produced in the neutron irradiation. The chromium, cobalt, and strontium content of Bureau of Standards’ rock reference samples have been determined by Turekian and Carr (1141). Ahrens and Edge (16) have measured the K/Cs ratios of some basic rocks by an activation analysis method. Other articles have reported activation analysis determinations of microquantities of cobalt (210), strontium ( 7 1 4 , gallium (820), rhenium (821), scandium (577), silver (822, 823), thallium (822, 823), tantalum (826), and gold and cadmium (11701172) in rocks. Abdullaev ( I ) , Fedorov, Sokolov, and Ochkur (325),and Iokhelson and Shitov (606) have described nondestructive activation analysis methods for the determination of trace element impurities in rocks by means of a gamma-ray spectrometer. Rocks and meteorites have been analyzed both by gamma-ray spectrometry and radiochemical methods for microgram and submicrogram quantities of tantalum (69),tungsten (69),scandium (96, 577),
chromium (96), europium (96), cadmium (119), and vanadium (576). Abdullaev and his coworkers (2) have analyzed sphalerites for microgram amounts of iridium. Ehmann (301) has analyzed tekites for trace nickel. The geochemical characteristics of iodine in meteorites have been studied by Goles and Anders (395) by use of an activation analysis method. Trace amounts of lanthanum and other rare earth elements have been determined in chondritic, achondritic, and iron meteorites by Mosen, Schmitt, and Vasilevskis (830) and others (1027). The osmium and rhenium contents of iron meteorites have been determined by Herr and his colleagues (464-466, 480). Reports on the determination of silver, rhodium, and indium (1024) and heavy elements (972) in chondritic meteorites have also been made. Stone meteorites have been analyzed for scandium, chromium, and iron (96), selenium and tellurium (1023) and UZ3j (617). Konig and Wanke (617) have used the neutroninduced Xe’33 and Xe135 isotopes in their determination of U235. The age of stone meteorites have also been analyzed by the potassium-argon age determination method (1185). Other activation analysis applications in geochemistry have been cited by Leddicotte and his colTorkers (670). Many different trace elements have been analyzed for in water by Leddicotte and Lloeller (611). and the activation determination of trace uranium in sea Eater has been reported (1214). Hamaguchi, Kuroda, and Hosohara (437) have determined parts per billion of mercury, copper, and arsenic in marine sediments. BIOCHEMISTRY APPLICATIO~-S. Borg and his coworkers (139) have described a method of selective radioactivation and multiple coincidence spectrometry to measure parts per billion of manganese in various body tissues. Tissue has also been analyzed for trace manganese by Papavasiliou and Cotzias (916). Stable cobalt has also been determined in body tissue by use of the neutron-induced radioisotope 10.5 rn C o m m (654). Iodine in the thyroid (1179), phosphatides in mammalian cells (1111), cadmium in biopsy specimens (1608), and chlorine in muscle tissue (114) have also been determined by activation analysis. Parts per billion of gold in blood have been determined by Diebel and Garrett (680) by the use of neutron activation and scintillation spectrometry. Trace manganese, iron, and chromium have been determined in blood by Hutchinson (497). Pijck, Gillis, and Hoste (940) have determined microgram amounts of copper, chromium, cobalt, and zinc in blood. The arsenic content of Sapoleon’s hair was measured by an activation
analysis method (342). Trace arsenic has also been determined in similar biological specimens by Mackintosh and Jervis (765). Parts per million of chlorine, bromine, and iodine ha.ve been determined by Bowen (147) in a variety of biological materials. Bowen (148) has also determined tungsten in these same materials and Bowen and Cawse (149) extended this work to the determination of trace sodium, potassium, and phosphorus in the same materials. Other articles describing activation analysis methods for the determination of strontium in milk (803), gold in pharmaceuticals (1163), and trace elements in plants and soils (1130,123,$), have been published. MISCELLANEOUS APPLICATIONS. Anders (52) has used gamma spectrometry to measure nondestructively the F2” (10.2 s) radioactivity produced in the F19 (n, y) F20 reaction in order to determine the fluorine content of a number of different sample materials. Anders (63) also reports on the use of other very short-lived isotopes in activation analysis. Born and Riehl (142144) and Anbar, Peisah, and Rafaeloff and others (49) report on the determination of microquantities of oxygen in various solid materials by use of the neutron reactions, Li6 (n, a ) t and OIG(t, n ) F1*. The use of LiG reactions to determine beryllium has also been reported (680). Trace bromine, copper, manganese, and sodium in KCl and trace chlorine, manganese, copper, and sodium in K B r have been determined bj, an activation analysis method (58). Baumgartner (97,98) has determined trace chlorine in zinc sulfide. He also has reported the results of his activation analysis work on determining chlorine and other trace elements in strong neutron-absorbing materials (99). Samples of lithium hydroxide and lithium carbonate have been analyzed for trace mercury contamination (251). ‘The nondestructive assays of ancient potsherds (S09), parts per million of aluminum in reactor cooling waters ( S l l ) , trace selenium in sulfur (316), manganese in wood pulp (329), trace elements in sodium triphosphates ( 3 4 3 , trace elements in commercial grade toluene (582), trace elements in silicon carbide (716), aluminum in polyethylene (849), vanadium and aluminum in graphite (853), manganese and arsenic ingraphite (870),rare earths in graphite (988), mercury in cellulose and other materials (704, 1201, 1204)~copper in rubber latex (258), and sodium in telluric acid (742) have also been reported. Okada and others (889, 893895,897) report on the determination of erbium, ytterbium, scandium, and dysprosium in rare earth rich materials. Stable isotopes have been incorporated into textile materials andprocesses,
and their characteristic behavior as trace elements in these materials have been studied by activation analysis and nondestructive gamma-ray spectrometry (64, 876). SPECIAL APPLICATIONS.Aidarkin and his colleagues (18) and Iredale (509) have reported on the use of y, n reactions to determine beryllium in ores. This photoneutronic method has also been used t o determine deuterium concentrations in natural waters (84, 392). Bisby, Hale, and their associates (121-123, 136, 431) have described gamma and alpha irradiation techniques and instrumentation for the detection and assaying of beryllium minerals. Bojin (135),Brownell (173),Bulashevich and others (183), Dakhnov (257), Mezhiborskaya (786-788), Milner and Edwards (794), Posik, Babichenko, Grodko (963),and Smirnov and Starchik (1081) also have described similar techniques for the determination of the beryllium and boron content of ores. Alpha-induced radioactivity methods for use in the control of products containing aluminum and boron (943, 947) and beryllium, aluminum, and fluorine (944, 946) have also been described. Boron has been determined in minerals also by detecting the alpha particles from the reaction B1o (n, (Y) Li7 (33‘7). Other ideas on the use of the same reaction for boron analysis have been reported by Ivanova and Kirznozov (526)and Khristianov, Panov, and Chernova (587). PoZ10-Be neutron sources have been used to determine quantities of boron in concentrations as small as 0.005% in profiling deposits of boron-containing ores and minerals (85, 86). Boron concentrations in gaseous mixtures have also been determined by means of neutron beams from radioisotopic-beryllium sources (230). Shimelevich (1059) and Wiesner (1209, 1210) report on a procedure of activation analysis of rocks under borehold conditions. The isotopic composition of lithiumbearing materials has been determined by a neutron activation method involving the production of a source of tritons by the Li6(n,a)H3 reaction (120). Coleman (2%) also reports on a similar method for the determination of lithium isotopic concentrations. Similar techniques have been used in determining the lithium content of aqueous solutions (1619) and of ores (1238); such techniques have also been used in determining oxide film thicknesses (1221). The isotopic composition of U235in uranium oxide has been determined by May and Leveque (764). Seyfang (1048) has reported a method of obtaining increased precision in the isotopic abundance of U2% by activation analysis. Beller (107) has described a method of deter-
mining the isotopic concentration of U2a by neutron activation. The particle size distribution in samples of thorium oxide have been studied (92, 95, 1120) by use of the neutron P-’reactions Th232(72, -i)Th233?&Pa233
(27.1 d ) . The gamma radiations (0.320 m.e.v.) of Pa223 are measured by means of a small NaI crystal as the thorium oxide particles settle by sedimentation. Particle sizes as small as 0.7 micron have been determined by this method. One of these reports (92) also generally describes a centrifugation method used to measure particle sizes as small as 0.02 micron in the same sample system. An activation analysis method used to determine particle-size distributions in samples of UOz has bsen described by Iwamoto (5%’). Amiel (46) reports on the use of a n activation analysis method involving a measurement of delayed-neutron emission to determine parts per million of uranium and thorium in a variety of sample materials. Amiel and Peisach (47) have also used reactor neutrons to determine t’he deuterium concentrations of heavy water by the reaction 0’6 (H2,n) FI7. Other articles have described activation analysis methods of determining stable barium in SrQ0solutions ( 8 3 3 , carbon in iron by proton bombardment (1076), carbon, oxygen, and silicon in solids by 15-1n.e.v. deuterons (12,?0), oxide film thickness by proton activation (1127), and sulfur by iast neutron activation (381). Neutron activation analysis has also been used to measure diffusion coefficients (1006) and to calibrate fast neutron flux areas in a nuclear reactor (266). Tracers a n d Natural Activities in Analysis. The introduction of a radioactive-labeled material into a sample system or a mezisurenient of the natural radioactivity of a system become very useful techniques for rapid a n d economical methods of analyses for elements or materials. I n this reviewer’s opinion, radiometric analysis methods,“ involving either isotope dilution n-ith radioactive tracers, labeled reagents for use in chemical techniques such as titrations, or the use of radioactive tracers for procedure development have much use ill analytical chemistry. Preformed radioactive For the purpose of this review the term “radiometric’’is used in the following broad context: “An analytical technique involviiig a radioactivity measurement in which the measurement itself is the controlling factor.” K e understand that this word, and also the self-defining “radioreagent,” mill be considered by several nomenclature committees within the next year. Our policy as to the use of these and other radiochemical terms may be modified accordingly. (1
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sources, either as alpha, beta, or gamma radiation sources, or radioisotopic-beryllium neutron sources, also can be useful in meeting many analysis requirements. Driscoll (286, 287) and Vlasova and others (1173) have presented a general discussion on techniques that can be used in radiometric analysis. More specific reports on the use of radiometric analysis techniques can be categorized: ISOTOPE DILUTIOK ANALYSES. Since this technique ineasures the yield of a nonquantitative process, only simple equipment is required. Glassware and mechanical equipment common to an analysis laboratory are adequate. Inexpensive counting systems for measuring radioactivity are readily obtained from electronic equipment suppliers. Alimarin and Bilinovitch (27) review the principles of isotope dilution and discuss its applications to the analysis of inorganic substances. Weiler (1191) reports on the accuracy of the isotope dilution method. Stary and Ruzicka (1099) have used a n ion exchange technique in an isotope dilution method for iron using Fej9. Solvent extraction (1001) and microcoulometry (998-1000) have also been used in isotope dilution methods. Other isotope dilution applications reported have used ZnE5and CoEoto determine zinc and cobalt in metals (241); Tals2 to determine tantalum in metals (40); Hf181 to determine hafnium in zirconium (42, 376); C136to determine microgram amounts of chloride (644); Se7j to determine selenium in organics (573); Ag1l0m to determine small amounts of silver (998-1000) ; Zrgj, Xbg5,and Ta1R2to determine zirconium, niobium, and tantalum in steels (38, 39); thorium isotopes in dating of marine sediments (54); and C060 to determine cobalt in steels (.47jl 1089). Kebster and others (1189, 1190) report on the use of U2” and Paz4*in isotope dilutions by mass spectrometry. ANALYSES WITII L.4BELED REAGENTS. Radiometric methods employing reagent solutions or solids tagged with a radioactive species hare been used to determine the solubility of barium tungstate (1240), ruthenium hydroxide (I&?), phosphotungstates (1088), and neodymium oxalate (15.4). Polythionates (1032), lead (1166), fluoride ( 8 4 4 , and organic precipitants (1193) have also been analyzed by radiometric methods using radioreagents. Co60-labeled hexamine trichloride has been used to determine beryllium (269) and thallium (606). Tagged Co(CH3COO)^ solutions have been used to determine fatty acids on paper chroTritium-labeled matograms (909). lithium-aluminum hydride has been used to determine hydrogen (224, 387). Other authors report on the synthesis and use of H3- (198,199,460,1216) and C14- (197, 198) labeled compounds in 158 R
ANALYTICAL CHEMISTRY
analysis. PS2 reagents have been used either with isotopic exchange (925,1074, to determine zirconium (559). Nagase, 1075), a pyrolysis-ion exchange system Baba, and Suzuki (848) have used for fluoride (729), separation of colloidal tagged phenylmercuric acetate comparticles (701),adsorption of surfactants pounds in drug research. Dern (271) on copper phthalocyamine (1043),deporeports on the use of double-labeled iron sition of Zn6j and P32on metallic and (Fej5 and Fej9) compounds in research. nonmetallic surfaces (461), the dilute Gilat (385) has employed a Sr8j-labeled solution chemistry of antimony (648), carrier for Srw determinations. Ca4jor chromatographic separations by the tagged cation exchangers have been adsorption of complexes (401, 699). used to determine aluminum ( 4 1 ) . KATURALRADIOACTIVITY APPLICAThe use of Agllo radioreagents to TIONS. A number of reports on the use titrate zinc and copper with EDTA of radiometric analyses involving only a has also been reported (103, 363). measurement of the natural radioreagents have been used to estimate activity of an element h a r e been made. monosaccharide and poly01 concentraNondestructive alpha, beta, and gamma tions of compounds separated by chrocounting methods have been employed. matography (104). Ha-labeled anthraConcentrations of uranium-235 in uranilic acid has been used to determine nium isotope mixtures (118) and of Pu239 copper by an amperometric titration in irradiated uranium (117) have been method (37). determined by alpha spectroscopy. KrBs-labeled gas has been used in Low-level beta counting methods have surface area measurements (76). Other been used to determine K40 in meteorites tagged reagents have been used to (483) and in rocks (990), and NaZ2in measure the surface area of UOz powders meteorites (1169). (400) and surface contaminants of Low-level natural gamma radiometals (45). Burton (189) has deactivities can be measured with scintillascribed the use of long-lived radon tion detectors (875, 879). Gamma-ray products as natural atmospheric tracers. spectrometry has been applied to the McFarling and others (771, 772) determination of U and T h in granitic report on the use of radioactive species rocks (606, 561, 977, 1017). It has as intrinsic tracers for industrial process also been used to determine U and T h control, and radiometric methods for in ores (267); K in rocks (108,259,661, automated process control have been 923); Ra in rocks (606); uranium in described by Scott and Driscoll (1033). aqueous and organic solutions (137, Magnesium and calcium have been 161); uranium in the presence of ionium determined in portland cement by (1064); Pa231in water and sea sediments has radiometric methods (170). (1009); Pa233 in irradiated thorium been used by Moser (831, 832) in hynitrate (1086); and in the determination drology applications. of uranium isotopic enrichments (1018). CHEMICALSYSTEMAND PROCEDURECartmight and Robbins (212) have disEVALUATIONS. The use of radioactive cussed the sources of errors that are tracers as a means of determining the possible in determining uranium isotopes behavior of an element in a separation by this radiometric analysis method. RADIOACTIVE SOURCES.hleinke (717) system or in evaluating chemical separation procedures continues with much in his review has pointed out that success. Ziv and Ishina (1949) have radioactive clathrate sources are interstudied the electrochemical separation esting applications of radioactive of bismuth from dilute solutions by use tracers, Additional information on the of Biz1O tracer. and Sb95 tracers properties and applications of rare gas have also been used to study the electroclathrate compounds have been given by chemical behavior of T a and K b (409). Chleck and his associates (223, P2@, Lloyd and Morris (705) have used Ir1g2 by hlock, Trabant, and l l y e r s (802) in studying chemical separations of the and by Kilson and Hughes (1213). platinum metals. As76, SblZ4,and Sn1I3 Hommel, Chleck, and Brousaides (482) tracers have been used to study methods have reported that parts per billion of of separating arsenic, antimony, and tin ozone can be determined in nonradiofrom pig iron (397). Gorshtein (401) active gases by use of quinol-kryptonhas investigated the errors that can 85 clathrate sources. occur in cocrystallization and coprecipiReports on the use of sources of a tation with radiotracers. Other presingle radionuclide with characteristic cipitation reactions have been studied radiation energies (such as C136 and by Geilmann and others by Lieser (691), Tl204) to serve as detectors in x-ray (373), and by Koch (605). Radiospectrometry have also been made tracers have been used by Blasius and (206, 841). Beta-ray sources have Beccu (129) to study the contact ion been used in particle size analyzers exchange properties of ion exchangers. (690). The characteristics of SrN beta ilmano (46) has used radioisotopes to particle detectors for use in gas-liquid study solvent extraction methods for chromatography have been described tungsten, molybdenum, and vanadium. by Upham, Lindgren, and Nichols Other reports on the use of radioactive (1146). An Am241 gamma source has tracers have included those concerned
been used in a laboratory analyzer to measure the concentration of heavy elements in process solutions and flowing streams (242, 727). Sm1*5,SmljaJGdlS3,
and Tm”O sources have been used for radiography (414). Radioactive sources have been used in dose measurements (767) and to determine the distribution of iron on recording tape by radiographic methods (740). The uses of radioisotopic-beryllium sources of the Po2l0 and RaZ26type in activation analysis have already been cited elsen-here in this review. In another application, Segatto (lO46) has analyzed boron silicate glasses for boron by neutron transmission. ACKNOWLEDGMENT
The preparation of this paper has been greatly assisted by the interests of the Division of Isotopes Development, E.s.Atomic Energy Commission. The writer is grateful for the assistance of L. hl. Guinn, N. B. Tuck, V. C. Leddicotte, D. L. Willson, and A. P. Grimanis in preparing the manuscript and bibliography. LITERATURE CITED
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