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International Conference

ACTIVATION ANALYSIS

October 15—19,1990 Beijing, China

ABSTRACTS

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Division of Activation Analysis and Radioanalysis, China

1990 Beijing

International Conference ACTIVATION ANALYSIS AND ITS APPLICATIONS

(ICAAA) October 15—19,1990 Beijing, China

ABSTRACTS

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Organized by Division of Activation Analysis and Radioanalysis

Sponsored by National Natural Science Foundation of China (NSFC)

Chinese Nuclear Society (CNS)

Chinese Chemical Society (CCS)

Chinese Academy of Sciences (CAS)

Nuclear Physics Society, CNS (NPSC)

Nuclear and Radiochemical Society, CNS (NRSC)

Beijing Nuclear Society (BNS)

Chinese Association for Science and Technology (CAST)

International Centre for Theoretical Physics (ICTP)

International Advisory Committee

Chatt,A (Halifax) Das.H.A. (Petten)

Iyengar,V. (Gaithersburg) Lennihan,J. (Glasgow)

Liu,Y. F. (Beijing) Moauro,A. (Rome)

Ni'ese,S. (Dresden) Park.K.S. (Seoul)

Sabbioni,E. (Ispra) Suzuki,N. (Sendai)

Yakovlev,Y.V. (Moscow) Yeh.S.J. (Hsinchu)

National Committee

Chai Chifang (Beijing)—Chairman Feng Xichang (Beijing, Publication)

Li Shounan (Beijing) Liu Desao (Beijing)

Sun Jingxin (Beijing) Tian Weizhi (Beijing, Publication)

Tong Chunhan (Chendu) Wang Yongxian (Shanghai)

Wu Zhihua (Shanghai) Xiao Lun (Beijing)

Xu Honggui (Beijing) Zhang Zhiyao (Beijing)

Zhao Pengji (Chendu) Zhong Honghai (Guangzhou)

Zhou Ruiying (Beijing) Zhou Yunlu (Beijing)

Organizing Committee

Chai Chifang—chairman Ju Kefei

Qiu Xibai Sun Jingxin

Tian Weizhi Wang Yongxian

Zhang Zhiyao

CONTENTS

AL-Joboori, S.M., AL-Bedri, M.B.H. and Hassan, H.A.A. TRACE AND TOXIC ELEMENT DETERMINATION IN DRINKING WATER OF IRAQ BY NEUTRON ACTIVATION ANALYSIS ICAAA-001 1

Aarnio, Pertti, Hakulinen, Timo and Routti, Jorma EXPERT SYSTEMS FOR NUCLIDE IDENTIFICATION AND INTERPRETATION OF GAMMA SPECTRUM ANALYSIS ICAAA-002 4

Adams, Bruce, Gihwala, Dherendra, Peisach, Max and Dent, D. THE DETERMINATION OF TRACE AND MINOR ELEMENTS IN BREAST CANCER TISSUE ICAAA-003 6

Alexandrova, G.I., Shmanenkova, G.I. and Pugatcheva, O.P. CHARGED PARTICLES ACTIVATION IN ANALYSIS OF PURE MATERIALS ICAAA-004 8

Andreev, A.V., Varich, O.M. and Makarov S.A. PRECISE 14 MeV NEUTRON ACTIVATION ANALYSIS ICAAA-005 9

Anikiev, V.V., Prasad, S.K., Polyanova, T.Yu.and Kolesov, G.M. STUDIES OF DISTRIBUTION OF CHEMICAL ELEMENTS IN SUSPENDED MATTER AND BOTTOM DEPOSITS OF CONTINENTAL SHELF OF EASTERN CHINA SEA USING NEUTRON ACTIVATION ANALYSIS ICAAA-006 11

Asubiojo, O.I., Obioh, I.B., Oluyemi, E.A., Oluwole, A.F. and Spyrou, N.M. ELEMENTAL CHARACTERISATION OF AIRBORNE PARTICULATES AT TWO NIGERIA LOCATIONS DURING THE HARMATTAN SEASON ICAAA-007 1 3

Bao Weidong, Zhou Manfang and Yuan Genie DETERMINATION OF 12 RARE-EARTH ELEMENTS IN HiGH-PURE Sc203 BY PRETREATMENT NEUTRON ACTIVATION ANALYSIS ICAAA-008 . 16

Berzina, I.G., Gusev, E.B., Lukin, V.I. and Rilnikov, V.S. STUDY OF BRAZED AND WELDED JOINTS BY METHODS OF RADIOGRAPHIC ACTIVATION ANALYSIS ICAAA-009 l 8

I

Capannesi, G., Sedda, A.F. and Cecchi, A. OAK LEAVES FEASIBILITY AS GASEOUS POLLUTION MONITOR ICAAA-010 20

Capannesi, G. Renzi, L., Sedda, F. and Jin, Li-Yun STUDY OF TRACE ELEMENT IN HAIR SAMPLES FROM TWO CHILDREN AT DIFFERENT DATE BY USING INAA ICAAA-011 22

Chai Chifang, Ma Shulan, Zhao Zhenhua, Zhao Huilan, Mao Xueying, Ma Jianguo and Zhou Yaoqi DETERMINATION OF REE ABUNDANCES IN MINUTE BIOGENIC APATITE BY NAA AND ITS GEOCHEMICAL SIGNIFICANCE ICAAA-12 M

Chatt, A. and Jayawickreme, C.K. STUDIES ON SPECIATION OF TRACE ELEMENTS IN BIOLOGICAL MICROMOLECULES ICAAA-013 * 26

Chen Yinliang and Wang Xiaoling NEUTRON ACTIVATION ANALYSIS OF RHENIUM IN ROCKS ICAAA-014 28

Cheng Yuandi, Wang Xuepeng, Qian Yine, Zhang Yuanxun and Tan Mingguang PREPARATION AND CERTIFICATION OF THE HUMAN HAIR REFERENCE MATERIAL ICAAA-015 29

Ciftcu, Em. and Popa-Nemoiu, Al. UNCERTAINTIES IN THE CHARGED-PARTICLE ACTIVATION ANALYSIS AT CYCLOTRON ICAAA-016 31

Constantinescu, B.,.Pascovici, G. and Plostinaru, D. LIGHT ELEMENTS DETERMINATION USING ACTIVATION METHOD AT THE INPE CYCLOTRON ICAAA-017 33

De Nadai Fernandes, Elisabete A., Ferraz, Epaminondas S.B., Martinelli, Luiz A. and de Oliveira, Helder AMAZON BASIN: TRACE ELEMENTS IN VARZEA SEDIMENTS ICAAA-018 35

I

Deng Hongmin and Li Jianming STUDY OF BORON IN LEGUME FORRAGES USING SOLID STATE NUCLEAR TRACK DETECTOR ICAAA-019 37

Dighe, P.M., Pansare, G.R. and Bhoraskar, V.N. MEASUREMENT OF FILM THICKNESS BY 14 MeV NEUTRON ACTIVATION ANALYSIS ICAAA-020 39

Dighe, P.M., Panasare, G.R., Kulkarni, S.G. and Bhoraskar, V.N. USE OF 14 MeV NEUTRON IN ANALYSIS OF EXPLOSIVE CLASS MATERIALS ICAAA-021 41

Dim, L A , Adetunji, J. and Okujeni, CD. INAA OF VEINED PYROCLASTIC ROCKS FROM ABAKALIKI, LOWER BENUE TROUGH NIGERIA ICAAA-022 43

Ding Zuguo, Chai Chifang, Fu Jiamo and Sheng Guoying INVESTIGATION ON TRACE ELEMENTS IN THE CRUDE OILS AND ORGANIC MATERIALS EXTRACTED FROM SOURCE ROCKS FROM CHINA WITH INAA ICAAA-023 44

El-Amri, F.A. and El-Saltani, H.E. DETERMINATION OF TRACE ELEMENTS IN NORMAL AND DIABETIC WHOLE BLOOD BY NEUTRON ACTIVATION ANALYSIS ICAAA-024 46

Elteren, J.T. van and Das, H.A. SPECIATION OF ARSENIC IN WATER SAMPLES ICAAA-025 48

Englert, Peter A.J., Castaneda, Carlos M., Sanii, Behzad, Drake, Darrel M., Reedy, Robert C and Young, John C. PLANETARY GAMMA-RAY SPECTROSCOPY: METHODICAL IMPROVEMENTS THROUGH NEUTRON INELASTIC SCATTERING CROSS SECTIONS BETWEEN 20 AND 70 MeV ICAAA-026 51

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Esposito, M., Collecchi, P., Oddone, M., Martines, H., Aste, H., Merlo, F., Meloni, S., Caramella-Crespi, V. and Genova, M. PLASMA AND TISSUE LEVELS OF SOME LANTHANIDE ELEMENTS IN THE HUMAN COLORECTAL LESIONS ICAAA-027 53

Fang Hong, Feng Xizhang and Chai Chifang A STUDY OF THE NINQIANG CARBONACEOUS CHONDRITE MATRIX BY INAA ICAAA-028 55

Feng Songlin, Zhong Ming, Ren Minqin and Liu Nianqin PROGRESS IN MEASURING THE IMPURITY CONTENTS IN A BaF2 CRYSTAL USING THE PIXE ANALYSIS ICAAA-029 57

Flitsiyan, E.S. USE THE METHOD OF ACTIVATION RADIOGRAPHY FOR GEOLOGICAL AND GEOCHEMICAL INVESTIGATION ICAAA-030 59

Genova, N. PROVENANCE STUDIES OF ANCIENT ETRUSCAN MARBLES BY NEUTRON ACTIVATION ANALYSIS AND DATA REDUCTION ICAAA-031 61

Ghafourian, H., Ali, Sameh A. and Ache, H.J, SEPARATION OF TECHNETIUM FROM DISSOLVED RESIDUES OF IRRADIATED NUCLEAR FUEL ICAAA-032 63

Gihwala, Dherendra, Lackay, Lotter Geoffrey and Peisach, Max MEASUREMENT OF PROTON INDUCED PROMPT LOW ENERGY PHOTONS BY RESOLUTION SPECTROMETRY: THE ANALYSIS OF NOBLE METALS LANTHANIDES ICAAA-033 64

Hien, P.Z., Mai, T.K., Quang T.X., Loc, N.V. and Thuy T.N. DETERMINATION OF Ko-FACTORS OF SHORT-LIVED NUCLIDES ( T l / 2 < 1 MIN, ) BY THERMAL NEUTRON ACTIVATION TECHNIQUE ICAAA-034 66

Holzbecher, J. and Ryan, D.E. ANALYSIS OF IRON METEORITES BY INSTRUMENTAL NEUTRON ACTIVATION WITH A SLOWPOKE REACTOR ICAAA-035 68

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Ha, P. MULTIELEMENT ANALYSES OF BLOOD AND SERUM SAMPLES OF DIABETIC PERSONS BY INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS ICAAA-036 70

Izak-Biran, T., Mantel, M., Lavy, N., Even, 0 . and Shenberg, C. DETERMINATION OF SELENIUM AND OTHER ELEMENTS IN HUMAN COLON TISSUE BY INAA; COMPARISON WITH RESULTS OBTAINED BY XRF METHOD ICAAA-037 72

Jin Li-Yun, Li Yun and Yang Ming RNAA OF ULTRA-TRACE Ir IN PRECAMBRIAN-CAMBRIAN BORDER SAMPLE BY THIOUREA-TYPE CHELATE RESIN SEPARATION ICAAA-038 n

Kanias, George D. NUTRIENT AND OTHER TRACE ELEMENTS IN INSTANT SOUPS ICAAA-039 76

Karandashev, V.K. and Grazhulene, S.S. APPLICATION OF EXTRACTION CHROMATOGRAPHY IN NEUTRON ACTIVATION ANALYSIS ICAAA-040 78

Karpov, Yu.A., Kudinov, B.S. and Murashov, M.V. GAS EXTRACTION IN ACTIVATION ANALYSIS ICAAA-041 8 °

Kennedy, G. and Hobeika, S. PSEUDOCYCLIC ACTIVATION OF GEOLOGICAL MATERIAL ICAAA-042 82

Kennedy, G. and Bergeron, S. TREE RINGS AS MONITORS OF HEAVY METAL AIR POLLUTION HISTORIES ICAAA-043 84

Khrbish, Y.S. and Spyrou, N.M. PROMPT GAMMA-RAY NEUTRON ACTIVATION ANALYSIS BY THE ABSOLUTE

METHOD ICAAA-044 8 6

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Knaus, Ronald M. INSTRUMENTAL NEUTRON ACTIVATION METHODS TO MEASURE SHORT-TERM ACCREATION AND EROSION IN WETLANDS WITH RARE EARTH SOIL HORIZON MARKERS ICAAA-045 88

Knorr, J., Schiekel, M., Franke, W. and Focke, F. PROTEIN DETERMINATION IN SINGLE GRAINS BY INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS ICAAA-046 90

Kolesov, G.M. NEUTRON ACTIVATION ANALYSIS IN SOLVING UNIQUE GEOCHEMICAL AND COSMOCHEMICAL PROBLEMS ICAAA-047 92

Kolesov, G.M., Barsukova, L.D., Miklishansky, A.Z., Nazarov, M.A. and Sapozhnikov, D.Yu NEUTRON ACTIVATION DETERMINATION OF IRIDIUM AND SOME NOBLE METALS IN ROCKS, IMPACTITES AND OTHER GEOCHEMICAL SAMPLES ICAAA-048 94

Kolesov, G:M., Kudryashova, A.F., Mashtalka, A., Tarasov, L.S., Frana, Ya. and Shubina, N.A. SPECIAL FEATURES OF COMPOSITION OF LUNAR BASALTIC ROCKS BY NEUTRON ACTIVATION ANALYSIS ICAAA-049 96

Kolotov, V.P., Atrashkevich, Vajda I., Nagy, P., Brech, F., Kadar, A. and Vasarhely, F. ASPRO : A SOFTWARE PACKAGE FOR AUTOMATIC PROCESSING OF GAMMA RAY SPECTRA ICAAA-050 97

Kolotov, V.P., Mua, Le Tat and Nekrasova, N.N. SIMPLE RADIOCHEMICAL PROCRDURE FOR DETERMINATION OF SOME ESSENTIAL AND TOXIC ELEMENTS IN BIOLOGICAL SAMPLES BY NAA ICAAA-051 "

Kong Ping, Chai Chifang, Mao Xueying, Ma Jianguo c-nd Ma Shulan STUDY OF CHEMICAL SPECIES OF ANOMALOUS IRIDIUM IN CRETACEOUS TERTIARY (K-T) BOUNDARY CLAY WITH RNAA AND CHEMICAL STEPWISE DISSOLUTION PROCEDURE

.ICAAA-052 1 0 1

VI

Lackay, L.G., Gihwala, D. and Peisach, M. MEASUREMENT OF PROTON-INDUCED PROMPT LOW ENERGY PHOTONS BY HIGH RESOLUTION SPECTROMETRY: THE ANALYSIS OF NOBLE METALS ICAAA-053 103

Levine, Louis D. MICROPROVENANCE STUDIES OF ARCHAEOLOGICAL CERAMICS: A CASE STUDY FROM THE KANGAVAR AND MAHIDASHT VALLEYS, CENTRAL WESTERN IRAN ICAAA-054 105

Li Guodong and Tong Chunhan APPLICATION OF NAA IN ANALYSIS OF SEDIMENTARY ENVIRONMENTS IN SHALLOW SEA ICAAA-055 107

Li Yinming, Ding Yuzheng and Sun Xiaozhong SOME ASPECTS OF RADIOANALYTICAL CHEMISTRY OF 196, 198Au, 192lr, 186Re, AND 96Tc ICAAA-056 109

Lin Xilei and Heydorn, K. EFFECT OF CASCADE COINCIDENCES ON THE EFFICIENCY CALIBRATION OF A GAMMA-X DETECTOR ICAAA-057 11°

Lin, Xilei, Speziali, M. and Orvini, E. A PREIRRADIATION SEPARATION PROCEDURE FOR GALLIUM DETERMINATION IN BIOLOGICAL AND ENVIRONMENTAL MATERIALS BY NEUTRON ACTIVATION ANALYSIS ICAAA-058 112

Liu NianQing, Zhang, Xiaofeng, Feng Songlin and Zhong Ming THE METABOLISM OF TITANIUM AND OTHER ELEMENTS IN WISTER RAT ICAAA-059 H-1

Liu Yuren and Seymour, R.S. AN ON-LINE THERMAL NEUTRON PROMPT GAMMA MEASUREMENT SYSTEM FOR BULK DETERMINATION OF AL AND FE IN METAL ORES ICAAA-060 1 1 6

Lo Jem-Mau, Lin Yeu-Ping and Cheng Chia-Cheng SOLVENT EXTRACTION OF DITHIOCARBAMATES COMPLEXES AND BACKEXTRACTION WITH PALLADIUM(II) FOR DETERMINATION OF TRACE METALS IN SEAWATER BY NEUTRON ACTIVATION ANALYSIS ICAAA-061 1 1 8

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Loureiro, A.L.M., Vasconcellos, M.B.A. and Pereira, E.B. TRACE ELEMENT DETERMINATION IN AEROSOLS FROM THE ANTARCTIC PENINSULA BY NEUTRON ACTIVATION ANALYSIS ICAAA-062 121

Lu HuiJuan and Zhou YunLu DETERMINATION OF RARE-EARTH ELEMENTS IN HIGH-PURE YTTRIUM OXIDE BY NEUTRON ACTIVATION ANALYSIS ICAAA-063 1 2 3

Lu Zhaoda, Li Yinming, Qian Ruisheng, Chen Da and Chang Yongfu THE SYSTEMATIC SEPARATION AND RADIOCHEMICAL DETERMINATION METHOD FOR NEUTRON ACTIVATED NUCLIDES AND SOME ACTINIDES ICAAA-064 125

Ma Jianguo and Sun Jianguo AN EXPERT SYSTEM FOR NEUTRON ACTIVATION ANALYSIS ICAAA-065 126

Mao Zhixiang, Yan Peilan, Huang Jianwei, Dai Xiankai, Chai Chifang, Qian Qingfang and Ma Jianguo A STUDY OF THE SEDIMENT MOVEMENT WITH THE METHOD OF NEUTRON ACTIVATION ANALYSIS ICAAA-066 128

Moauro, A. and Carconi, P.L. NEUTRON IRRADIATION OF LiAL02 AS CANDIDATE CERAMIC BREEDER MATERIAL OF THE FUSION REACTORS;r-SPECTROMETRY OF THE ACTI-VATION NUCLIDES & EVALUATION OF THE TRITIUM PRODUCED BY(n, r) ICAAA-067 1 3 0

Moauro, A. and Carconi, P.L. AN EUROPEAN INTERCOMPARISON OF VEGETAL STANDARD REFERENCE MATERIALS, BASED ON INAA AND SOME NON NUCLEAR SPECTRO-CHEMICAL TECHNIQUES ICAAA-068 132

Ni Bang-Fa and Tian Wei-Zhi NAA OF IAEA LAKE SEDIMENT RM SL-3 FOR 45 ELEMENTS ICAAA-069 1 3 3

Ni Bang-Fa, Wang Pingsheng, Luo Yingjun and Yu Shouyan STUDY OF THE BIOAVAILABILITY OF ZINC USING ACTIVABLE ISOTOPE TRACER 70-ZN BY NEUTRON ACTIVATION ANALYSIS

ICAAA-070 I 3 5

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Niedergesaess, R., Schnier, C. and Pepelnik, R. ANALYSIS OF FERTILIZER PHOSPHATES USING REACTOR NEUTRONS AND 14 MeV NEUTRONS ICAAA-071 137

Niese, S., Krogner, K., Gleisberg, B., Werner, CD., Pfeiffer, L. and Kramer, W. INVESTIGATION OF MANTLE-DERIVED MAGMATITLES BY NEUTRON ACTIVATION ANALYSIS ICAAA-072 138

Niese, S. and Helbig, W. LOW RADIOACTIVITY MEASUREMENT OF ACTIVATED NUCLIDES IN AN UNDERGROUND LABORATORY ICAAA-073 1 4°

Nikolaenko, O.K., Mirotin, I.V. and Goldshtein, M.M. NEUTRON ACTIVATION DETERMINATION OF OXYGEN COEFFICIENT FOR HIGH-TEMPERATURE SUPERCONDUCTING MATERIALS ICAAA-074 U2

Nodar, Shonia, Liguri, Mosulishvili and Nana, Kharabadze ON THE POSSIBILITY OF EXPERIMENTAL DETERMINATION OF MICROELEMENT BIOVARIABIUTY IN BIOLOGICAL SYSTEMS ICAAA-075 l u

Nonie, S.E., Randle K. and Blackband, A.G. DEVELOPMENT OF A COMPUTER-BASED SYSTEM FOR FAST NEUTRON CYCLIC ACTIVATION ANALYSIS ICAAA-076 146

Nonie, S.E. and Randle, K. MULTI-ELEMENT DETERMINATIONS OF ROCK SAMPLES USING FAST NEUTRON CYCLIC ACTIVATION ANALYSIS ICAAA-077 1«

Olivier, C. and Morland, H.J. THE ELIMINATION OF MATRIX EFFECTS IN THE DETERMINATION OF FLUORINE BY PROTON-INDUCED PROMPT GAMMA SPECTROMETRY ICAAA-078 150

Pantelica, Ana, Salagean, Maria and Nicolae, Marieta IMPURITY CONTENT DETERMINATION !N HIGH PURITY CERAMIC POWDERS BY NEUTRON ACTIVATION METHOD ICAAA-079 152

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Papadopoulos, Neophytos l\l. and Synetos, Sotiris RECENT DEVELOPMENTS IN SHORT-LIVED NUCLIDE ACTIVATION ANALYSIS AND ANALYTICAL EFFICIENCY ICAAA-080 m

Patil, S. F., Rajurkar, N.S.(nee Adhyapak) and KANADE, K.G. THERMAL NEUTRON ACTIVATION ANALYSIS OF MINERAL NUTRIENTS IN DIFFERENT VARIETIES OF RICE IN INDIA ICAAA-081 156

Peisach, Max, Pineda, Carlos A., Jacobson, Leon and Loubser, Jan H.N. NUCLEAR ANALYTICAL STUDY OF ROCK PAINTINGS ICAAA-082 158

Peisach, Max, Pineda, Carlos A., Jacobson, Leon and Loubser, Jan H.N. ANALYTICAL STUDY OF NAMIBIAN POTTERY FROM SOUTPANSBERG ICAAA-083 160

Peisach, Max and pineda, C.A. DETERMINATION OF ALUMINIUM AND SILICON IN ZEOLITES BY PIXE ICAAA-084 162

Peng Lixin and Tian Weizhi INAA OF IAEA-155 WHEY POWDER FOR PHOSPHORUS AND OTHER 24 ELEMENTS ICAAA-085 m

Pillay, E.A. and Peisach, Max A SENSITIVE BORON PROBE USING THE REACTION 10B(3He, n)12N ICAAA-086 166

Pineda, Carlos A. and Peisach, Max PROMPT ANALYSIS OF RARE EARTHS BY HIGH ENERGY-INDUCED (p, x) REACTION ICAAA-087 168

Preoteasa, E.A., Salagean, M., Pantelica, A., Berceanu, St., Plostinaru, D., Constantinescu, B., Lungu, V. and Vilcu, Al. INAA AND PIXESTUDY ON THE COMPLEX MODIFICATIONS OF HUMAN BLOOD SERUM MINERAL COMPOSITION IN SEVERAL HEMOPATHIES ICAAA-088 I 7 0

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Qian Qinfang, Wu Suiqin, Tian Jibin and Chen Shiqing MULTI-ELEMENT DETERMINATION OF SOIL SOLUTION BY INAA ICAAA-089 172

Qian Xingzhen, Li Xiuxia A NEUTRON ACTIVATION ANALYSIS STUDY OF THE BACKGROUND VALUES AND STATES OF ELEMENTS IN NATURAL WATER ICAAA-090 174

Rajurkar, N.S. (nee Adhyapak), Patil, S.F., and Ballari, P.R. ELEMENTAL ANALYSIS OF AGRICULTURAL SOILS IN MAHARASHTRA (INDIA) BY INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS ICAAA-091 176

Rao, R.R., McDowell, L.S., Jayawickreme, C.K. and Chatt, A. EVALUATION OF HOMOGENEITY OF SELECTED REFERENCE MATERIALS FOR SELENIUM BY CYCLIC NEUTRON ACTIVATION ANALYSIS ICAAA-092 178

Rastikerdar, Samad A SOPHISTICATED IRRADIATION FACILITY FOR THE STRONGEST Am-Be NEUTRON SOURCE OF THE WORLD ICAAA-093 180

Rommel, M., Gehrbish, Sh. and Langrock, E.-J. THE POSSIBILITY OF AGGREGATE IDENTIFICATION IN CONCRETE BY PHOTON-ACTIVATION-ANALYSIS (PAA) ICAAA-094 182

Rossbach, M. and Stoeppler, M. FACILITY FOR PROMPT GAMMA ACTIVATION ANALYSIS OF BIOLOGICAL SAMPLES WITH COLD NEUTRONS AT THE KFA-Julich ICAAA-095 183

Rossbach, M. and Byrne, A.R. RADIOCHEMICAL NAA OF PLATINUM GROUP ELEMENTS IN BIOLOGICAL AND ENVIRONMENTAL SAMPLES ICAAA-096 186

Saiki, M., Vasconcellos, M.B.A. and Rogero, J.R. ANALYSIS OF BRAZILIAN SNAKE VENOMS BY NEUTRON ACTIVATION ANALYSIS ICAAA-097 188

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Salagean, Maria, Pantelica, Ana and Brad, I. MICROELEMENT CONTENT IN LEAVES AND FRUITS OF HIPPOPHAE RHAMNOIDES (L) PLANT DETERMINED BY NEUTRON ACTIVATION ANALYSIS ICAAA-098 190

Sarmani. Sukiman, Wood, Abdul Khalik and Hamzah, Zaini THE DETERMINATION OF ARSENIC, MERCURY AND SELENIUM IN MALAYSIAN SEA FOODS BY INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS ICAAA-099 132

Shmanenkova, G.I., Schelkova, V.P., Uritskaya T.P. and Volkova, L.V. DETERMINATION OF RARE EARTH ELEMENTS IN MINERAL RAW MATERIALS AND RARE EARTH INDUSTRY PRODUCTS BY NEUTRON ACTIVATION ANALYSIS ICAAA-100 194

Shtangeeva, Irina SHORT AND LONG PERIOD VARIATIONS OF THE ELEMENT COMPOSITION PLANTS AND SOIL IN LENINGRAD ICAAA-101' 196

Shulepnikov, M.N., Firsov, V.I., Kiseliova T.T., Rabinovich, B. Sysoeva, N.S. and Kondratieva, G.I. HIGH-FLUX NUCLEAR REACTOR IN ANALYZING SUPER-PURE METALS AND SEMI-CONDUCTORS ICAAA-102 198

Sima Octavian NEUTRON FLUX FLUCTUATION AND THE PRECISION OF NEUTRON ' ACTIVATION ANALYSIS ICAAA-103 200

Smakhtin, L.A. and Shevaldin, O.A. STUDIES ON THE NON-UNIFORMITY AND REPRESENTATIVE SAMPLING BY NAA ICAAA-104 203

Smakhtin, L.A., Filippova, N.V., Miglina, N.V., Shokel E.S. an Shutova, I.N. THE USE OF UNIVERSAL COMPARATOR METHOD IN LARGE-SCALE NAA • ICAAA-105 205

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Smakhtin, L.A., Mekhryusheva', L.I., Filippova, N.V., Miglina, IM.V. and Sinitsyna, T.S. THE DETERMINATION OF RARE-EARTH ELEMENTS IN ENVIRONMENTAL OBJECTS ICAAA-106 207

Solodukhin, V.P. COMPLEX OF PHYSICAL METHODS OF ANALYSIS TO INVESTIGATE ELEMENTAL COMPOSITION OF NATURAL HYDROCARBONS ICAAA-107 209

Song Quanxun AN AUTOMATED SYSTEM FOR INAA ICAAA-108 210

Spiridon, Stefania and Spiridon, Gheorghe NEUTRON ACTIVATION ANALYSIS OF CONSTITUENT MINERAL ELEMENTS CONTENT OF FEEDS-AND BIOLOGICAL SAMPLES ICAAA-109 212

Sun Jingxin and Wang Yuqi > INVESTIGATION ON BACKGROUND VALUES OF TRACE ELEMENTS IN SOILS OF CHINA WITH INAA I. THE BACKGROUND VALUES OF U, Th AND REE IN SOIL ICAAA-110 214

Sun Laiyan, Lu Fengying, Su Rongwei and Zhen Houxi DETERMINATION & EVALUATION OF TOXIC AND TRACE ELEMENTS IN CHINESE FOODSTUFFS ICAAA-111 216

Szabo, A.S. POSSIBILITIES OF APPLICABILITY OF PROMPT ACTIVATION TECHNIQUE IN THE FOOD CHEMISTRY ICAAA-112 218

Thakur, A.N. ISOTOPICALLY ANOMALOUS MERCURY IN METEORITES BY NEUTRON ACTIVATION ANALYSIS; A COSMOCHEMICAL APPLICATION ICAAA-113 220

Tian Jibing, Qian Qingfang and Chai Chifang STUDY ON THE DISTRIBUTION OF SELENIUM AND OTHER ELEMENTS BY NAA AND BIOCHEMICAL TECHNIQUE ICAAA-114 222

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Tian Junliang, Liu Puling and Li Yaqi A STUDY ON ELEMENTAL PEDOGEOCHEMISTRY OF LOESS PLATEAU, CHINA, BY INAA ICAAA-115 225

Tian Wei-Zhi and Ni Bang-Fa FURTHER STUDY ON PARAMETERIZATION OF REACTOR NAA ICAAA-116 227

Tian Weizhi and Peng Lixin A STUDY OF SAMPLING REPRESENTATIVENESS OF IAEA RM SD-M/TM MARINE SEDIMENT BY INAA ICAAA-117 229

Tluchor, D., Stverak, B. and Ciganek, L. TRACE ELEMENTS IN THE HUMAN EYE TISSUE ICAAA-118 231

Tong Chunhan and Li Guodong A NEW METHOD FOR CLASSIFYING PARENT TYPE OF ROCKS CONTAINING DISSOLVED ORGANIC MATTERS ICAAA-119 232

Tong Chunhan, Liang Xingzhong, Li Guodong and Li Juchu NEUTRON ACTIVATION STUDIES ON THE GEOGAS FROM A HIDDEN GOLDEN ORE DEPOSIT ' ICAAA-120 .234

Trukhov, A.V., Naumov, A.P. and Ganzha, A.P. THE COMPTON RANGE SIMULATION OF A SPECTROMETER RESPONSE FUNCTION FOR THE ESTIMATION OF ACTIVATION METRELOGICAL CHARACTERISTICS ICAAA-121 236

Tsukada Masamichi, Yamamoto Daijiro, Endo Kazutoyo and Nakahara Hiromichi PRE-CONCENTRATION METHOD USING AN ACTIVABLE YIELD TRACER FOR NEUTRON ACTIVATION ANALYSIS ICAAA-122 239

Vaganov, P.A. and Chou Rongsheng NEUTRON ACTIVATION STUDY OF MONOMINERAL FRACTIONS OF DEEP-WATER OCEANIC SULPHIDES ICAAA-123 241

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Vaganov, P.A. IRIDIUM AMONALY IN THE UPPER VENDIAN ICAAA-124 243

Vajda, I. and Toth, L. A BRIEF SUMMARY OF EMG'S MULTICHANNEL ANALYZER PRODUCT RANGE ICAAA-125 245

Vitali, Vanda AN APPLICATION OF DATA ANALYSIS AND EXPERT SYSTEMS TO INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS RESULTS: AN ANCIENT MATERIAL'S PERSPECTIVE ICAAA-126 247

Wang, Haiying DETERMINATION OF WHOLE-BODY PROTEIN IN SMALL ANIMALS BY IVNAA ICAAA-127 2^

Wang, Haiying BACKGROUND INVESTIGATION ON THE DETERMINATION OF NITROGEN BY IVNAA ICAAA-128 251

Wang Jun, Chen Da and Qian Shaojun NEUTRON ACTIVATION ANALYSIS OF GEOLOGICAL ROCK MATERIALS ICAAA-129 253

Wang Xinfu, Zhu Guanghua, Shen Xinyin, Xiong Duanggui, Wu Xueqin and Sun Youping A P1XE STUDY OF THE EFFECTS OF THE ZINC-SMELTING WITH AN INDIGENOUS METHOD ON SURROUNDING ATOMSPHERIC ENVIRONMENT ICAAA-130 255

Wang Yinson, Tan Mingguang, Zhi Min, Zhuang Guisun and Cheng Yuandi DISTRIBUTION OF SOME ELEMENTS IN HUMAN HAIR AND INTERNAL ORGANS DETERMINED BY NAA ICAAA-131 257

Wang YunLiang THE DIAGNOSTIC PRINCIPLES AND PROGRAM OF TRACE ELEMENT ABUNDANCES ON THE PETROGENESIS AND MANTLE EVOLUTION ICAAA-132 259

XV

Weginwar, R.G. and Garg, A.N. MULTIELEMEIMTAL NEUTRON ACTIVATION ANALYSIS OF DUST PARTICULATES FROM A CEMENT FACTORY IN CENTRAL INDIA ICAAA-133 261

Wei Lun-cun, Bao Shanglian, Yang Qixiang and Yang Xihong QUANTITATIVE CALCULATION OF THE CHARGED PARTICLE ACTIVATION ANALYSIS WITH CHANNELING ICAAA-134 263

Wu Yuguang and Zhao Junlin DETERMINATION OF TRACE ELEMENTS IN SAMPLES OF ANTARCTICA BY NEUTRON ACTIVATION ANALYSIS ICAAA-135 265

Wu Zhiqiang SEPARATION AND PURIFICATION OF 99-Tc FROM SIMULTING HIGH-LEVEL RADIOACTIVE LIQUID WASTES ICAAA-136 267

Xiao Jiazhu DETERMINATION OF 14 TYPES OF CHINESE TEA BY INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS ICAAA-137 269

Xiao Jiazhu SIMULTANEOUS DETERMINATION OF N, P, K, IN PLANTS BY 14MEV NEUTRON ACTIVATION ANALYSIS (FNAA) ICAAA-138 271

Yang Huazhong DETERMINATION OF SOME TRACE ELEMENTS IN HAIR OF DIABETICS BY ENERGY DISPERSIVE FLUORESCENCE METHOD ICAAA-139 273

Yang Huazhong and Song Shizhan ANALYSIS OF ELEMENT CONTENTS IN FOSSILS OF THE ANCIENT VERTEBRATES USING 241-Am XRF METHOD ICAAA-140 275

Yang Ruiying A PRELIMINARY STUDY ON THE TRACE ELEMENT GEOCHEMISTRY OF BASALTIC ROCKS FROM THE TANGBALE IN THE WESTERN JUNGGAR, XINJIANG, CHINA ICAAA-141 277

XVI

Yang Shao jin and Zhang Yi Ming IDENTIFICATION OF MARINE AEROSOL COMPONENT BY COMBINED NEUTRON ACTIVATION ANALYSIS AND SCANNING ELECTRON MICROSCOPY WITH X-RAY ANALYSIS ICAAA-142 2 7 9

Ye Zongyuan, Li Yubing, Ding Shengyao, Bao Zongyu, Yang Yiaoyun and Rong Chaofan AN INVESTIGATION OF METHOD FOR DETECTING EXPLOSIVES ICAAA-143 281

Yeh, S.J., Tseng, C.L. and Wei, J.C. PRECONCENTRATION FOR NEUTRON ACTIVATION ANALYSIS ICAAA-144 282

Zhang Weicheng, Zhang Tianmei, Zeng Wenbing and Lei Xiangguo DETERMINATION OF 13-C IN BREATH SAMPLE BY PIGE ICAAA-145 285

Zhang Xiaofeng, Ma Jianguo, Qin Junfa and Xiao Lun MULTIVARIATE STATISTICAL TREATMENT OF PIXE ANALYSIS OF TRADITIONAL CHINESE MEDICINE ICAAA-146 287

Zheng Jian and Zhang Guisun DETERMINATION OF TRACE ELEMENTS IN SUBCELLULAR FRACTIONS OF HUMAN LIVER BY INAA ICAAA-147 289

Zhong Ming, Feng Songlin, Liu Nianqing, Ren Minqin, Zhang Xiaofeng and Yan Linna PIX ANALYSIS OF CHEMICAL COMPOSITION OF GRAPHITE PHASE IN CAST IRON ICAAA-148 2 9 1

Zhou Dehai RADIOCHEMICAL SEPARATION OF 199-TL FROM THE AU TARGET BOMBARDED WITH a-PARTICLES ICAAA-149 293

Zhuang Guisun, Wang Yinson, Tan Mingguang, Zhi Min, Wang Yongjia and Zhuang Fulin PRELIMINARY STUDY OF TRACE ELEMENTS IN HUMAN BRAIN TUMOUR TISSUES BY INAA ICAAA-150 295

xvn

LATE CONTRIBUTIONS

Ding Xixiang, Chen Baoguan and Yang Yueqing

STUDY ON EVOLUTION OF GRANITE-PEGMATITES IN PEGMATITIC PROCESS BY MEANS OF NAA ICAAA -151 297

Fisher, E. M. and Dong Naisheng SAMPO 90 : AN ACCURATE AND VERSATILE TOOL FOR THE GAMMA SPECTROSCOPIST ICAAA -152 299

Peisach,M. , Pineda, C. A. ,Pil lay,A. E. and Themistocleous ,T. DETERMINATION OF ALUMINIUM AND SILICON IN ZEOLILES BY PIXE ICAAA -153 301

Soltanieh,A. A. ,Pazirandeh,A. ,Rahimian,N. and Salehi, M. PROMPT GAMMA NEUTRON ACTIVATION ANALYSIS OF COAL AND COPPER

ORE SAMPLES ICAAA -154 303

Wang Ke and Li shenzhi

NEUTRON ACTIVATION ANALYSIS IN MNSR ICAAA-155 305

Zhang Weihua and Cao Chuanru

DETERMINATION OF 30 ELEMENTS IN SEDIMENTARY SAMPLES BY INAA WITH MNSR REACTOR ICAAA -156 307

Park,K. S. ,K im,N. B. ,Woo,H. J.,Kim,D. K. ,K im,J . K. and Choi,H. W. DETERMINATION OF IMPURITIES IN HIGH PURITY SILICON BY INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS ICAAA -157 308

Park,K. S. ,K im,N. B. ,Woo,H. J. ,Hong,W. and Chun ,S. K. A STUDY ON KOREAN ANTHRACITE BY INSTRUMENTAL NEUTRON ACTIVATION

ANALYSIS

ICAAA -158 310

Seymour,R. and Cox,J. USING LIBRARY —DIRECTED ANALYSIS FOR SINGLET AND MULTIPLET PEAKS ICAAA -159 312

XVB1

TRACE AND TOXIC ELEMENT DETERMINATION IN DRINKING WATER OF IRAQ BY NEUTRON ACTIVATION ANALYSIS

S.M.AL- JOBOORI Nuclear Resarch Ceentre, Tuwaitha, Baghdad, IRAQ. M.B.H. AL- BEDRI,H.A.A.HASSAN. Physics Department, College of Science, Baghdad University, Baghdad, IRAQ.

This paper is a part of a research project on foodstuff analysis,using

Instrumental Neutron Activation technique for the determination of

the concentration of trace and toxic elements . This technique has

been applied for determination of the concntration of 23 elements in

drinking water collected from 30 locations across Iraq. Several

authors [1-3] have used the preconcentration technique of the water

by evaporation and freeze drying,followed by neutron activation analy-

sis for determination of multielement con centration levels in water.

The samples were collected using polyethylene bottle of 2 liter, pre-

viously cleaned with concentrated nitric acid and rinsed with double

distilled water. 5ml of nitric acid was added to the drinking water in

order to prevent loss of trace elements by adsorption on the container

wall,and the sample was concentrated by evaporation at 70-75 C using

ther mostaically hot plate to reduce the volume from 1L to(15-20) mL.

The concentrated sample was carefully bransferred from the beaker and

placed in a quartz bottle of 50ml under infrared lamp at low heat and

then kept at an oven at 70 C to be dried .

1

A bout 50 mq of each samples and standard were irradiated in IRT-5000 11 - 2 - 1 13

Reactor Cor 5 win and 6h. at a duxes of: 7x10" n.crn S and 2.3x10 -2 -1

n. cm S respectively. The samples and standards were counted

using Ge(Li)and Hp Ge detectors with a resolution (FWHM ) of 2.5 and

2.0 Kev at 1332 Key of 60Co respectively. The counting system was

linked to on- line computer for instant analysis of the gamma-rays.

The interferences from other radionuclides and other nuclear reac-

tions have been corrected in the present work. The accuracy of our

method was assessed by the analysis of AGV-1,SL-1 standard reference

materials. A good agcament has baen achieved between the present

values and the recommended values Table-1 . The range concentration of

23 elements in Iraqi drinking water has been determined Table-1 .

[1]. HABIB, S., MINSKI,M.J.,J.Radioanal. chem. 63(1981)379.

[21. NDIOKWERE,Ch.L.,GUINN, V.P., J. Radioanal. chem. 79(1983)147.

[3]. MILLEY,J.E, CHATT,A.,J. Radioanal.chem. 110 (1987)345.

2

Table 4 anges and mean concentrations or trace elements in Iraqi

drinking water (ug/M

~" "ELEMENT RANGE MEAN±S7D7

Na*

Mg*

A l *

S i *

CI

Ca*

Sc

V

Cr

Mn

Fe

Co

Zn

As

Br

Rb

S r

Mo

Sb

I

Ba

Ce

U

2 . 4 0 _235.4

0 . 5 5 _ 1 0 . 1 3

0 . 0 7 _ 1 . 6 8

1.10 _18.04

0 . d 3 ? _ 1 5 . 9 6

1 9 . 1 0 _ 2 3 6 . 9

0 . 0 1 3 _ 0 . 5 3

0 . 7 6 6 _ 4 . 0 2

0 . 3 6 3 _ 5 . 2 9

0 . 1 6 _ 1 6 . 5

3 5 . 0 _1425.

0 . 0 4 5 _ 0 . 6 9

7 . 9 3 _1615 .

1.03 _6 .24

0 . 1 0 J 2 9 . 8

0 . 9 5 _ 4 . 1 1

0 . 4 1 J 2 . 6 5

0 . 1 8 3 _ 1 6 . 1

0 . 1 8 _1 .99

0 . 6 3 _ 6 . 4 5

J 2 . 1 2 _ 3 1 5 . 6

0 . 1 4 5 _ 2 . 1 8

0 . 2 1 8 _ 4 . 3 1 6

5 7 . 4 + 5 0 . 3

4 .82i2 .3fa

0 . 4 7 ± 0 . 3 8

3 . 2 1 1 3 . 7 8

5 . 4 5 1 7 . 1 8

8 5 . 4 + 5 7 . 9

0 .08+0 .124

1.66 +0.78

1 .65+1.42

8 . 1 4 1 6 . 7

2 3 8 . 1 3 7 8 .

0 .27+0 .24

2 4 8 . 1 3 4 3 .

2 . 8 5 1 1 . 6 3

4 . 8 2 1 7 . 6 5

2 . 6 1 + 1 . 2 9

1 .1810 .703

5 .0913 .84

0 . 4 9 1 0 . 4 7

3 . 5 4 1 4 . 1 1

8 8 . 1 1 8 6 . 4

0 . 8 1 1 0 . 7 4

1 .3510.94

* rhg/1 3

EXPERT SYSTEMS FOR NUCLIDE IDENTIFICATION AND INTERPRETATION

OF GAMMA SPECTRUM ANALYSIS

Pertti Aarnio, Timo Hakulinen, Joima Routti

Helsinki University of Technology Nuclear Engineering Laboratory

SF-02150 Espoo, Finland

Gamma spectrum analysis is currently a widely used tool in many fields. Correct quantitative identification of radionuclides in a sample is often vital when making decisions for further actions. For example, finding fission products in a sample may suggest a radioactive release from the nearby nuclear power plant. Careful analysis, however, may prove that the fission products are due to nuclear weapons test or from a nuclear reactor of different type. In this case shutdown of the neighbouring reactor would be a costly mistake. The decisions must be correct and done quickly. This requires a substantial amount of expertise on the part of the laboratory personnel. Full quantitative identification of a complex spectrum takes many hours.

There are several good computer codes available for the automated analysis of gamma spectra. These include program MicroSAMPO [1] developed in our laboratory. The nuclide identification is an iterative process where the analyst aims to find correct nuclides by decreasing the amount of possibilities by trial and error. Although the process of identification is quite complex, it can be formulated using "rules of thumb" combined with exact mathematical analysis. Thus, it is feasible to build an expert system where the knowledge of a human expert" concerning the problem is converted into explicit rules. These rules can be processed by using an inference engine, a specialized program for reasoning.

There are two main strategies of inference in an expert system, for-ward chaining and backward chaining. In forward chained reasoning

4

initial data are brought into system after which the inference engine checks validity of rules in the system and fires every rule it can. If the fired rules cause further rules to become valid, the process continues until no more valid rules exist and one has, hopefully, reached a solu-tion. In backward chaining the user may ask a question, that is, state an assertion, which the inference engine tries to validate. Rules on which the truth value of the question depends are checked backwards if they can be validated until the answer is found. Standard approach to the identification problem is forward chaining, with which thor-ough analysis of a spectrum can be performed. Backward chaining comes in handy when one wants to know, for example, whether some specific isotopes are present in a sample.

We are currently developing an expert system that will carry out the quantitative nuclide identification with minimum of user interven-tion. Reasoning process is performed in a LlSP-based expert system development environment, Gold Works, where rules and data struc-tures are represented as LlSP-objects. The system uses a database containing over 2000 radionuclides with about 48000 gamma transi-tions [2] together with a dedicated database manager. Spectra are provided in preprocessed format, where peak energies, intensities and backgrounds with corresponding error estimates have been calculated using MicroSAMPO. In the first phase the expert system should be able to identify with good accuracy gamma spectra of arbitrary com-plexity and to compute corresponding activities, but the possibilities for system development extend further. When the amount of radionu-clides in a sample is known it is possible to use this knowledge in a more general level in a decision support system. This system should help to make decisions concerning the origin and future development of the measured radioactivity as well as give recommendations for appropriate measures to be taken.

[1] P.A. Aarnio, J.T. Routti, J.V. Sandberg, Journal of Radioanalyt-ical and Nuclear Chemistry, 124 2 (1988) 457-466.

[2] G. Erdtmann, W. Soyka, The- Gamma Rays of the Radionuclides. Verlag Chemie GmbH, Weinheim 1979.

5

THE DETERMINATION OF TRACE AND MINOR ELEMENTS IN BREAST CANCER TISSUE

Bruce Adams Department of Nuclear Medicine, Groote Schuur Hospital and UCT Observatory, 7925, South Africa.

Dherendra Gihwala School of Science, Peninsula Technikon, P.O.Box 1906, Belville, 7535, South Africa.

Max Peisach National Accelerator Centre P.O.Box 72, Faure, 7131, South Africa.

David Dent Department of Surgery, Groote Schuur Hospital and UCT Observatory, 7925, South Africa.

Essential trace elements play an important role in regulating biological processes as agents which inhibit or activate various enzyme systems. Experimental data has impli-cated trace metals as playing a possible role in the aetiology of cancer. An elemental analysis of breast cancer tissue was made in an attempt to acquire information regard-ing the possible causes of the disorder. Certain studies showed an increase in the con-centrations of specific trace metals in breast cancer tissue.[l,2] Other investigators found a deficiency in certain trace metals in certain malignancies including renal adenocarcinoma and melanoma, and patients with these disorders have been treated with some success by replacing these elements as part of the therapeutic regime. [3]

Prompt Gamma-ray and X-ray spectrometry - PIPPS and PIXE were used to deter-mine the relative concentrations of trace and minor elements in breast cancer tissue. These concentrations were compared with those obtained for tissue from benign breast disease and normal breast tissue. Other analytical methods to which these tissues were subjected include: X-Ray Fluorescence; Voltametry-Polarography; Emission Spectrometry; UV/Visible Spectrophotometry and Atomic Absorption Spectrometry. PIXE and PIPPS are compared with these other analytical processes.

Multivariate statistical methods were applied in attempts to determine the inter-relationships of the various elements and to define the relative importance of single or groups of elements. Cluster analysis, multi-dimensional scaling and correspondence

R

analysis techniques were used to determine the relationships of the different elements.

Specific attention was given to the following elements: vanadium, tungten, molyb-denum, selenium, tin, chromium, zinc, copper and iron.

These techniques were also used to determine the concentrations of the elements in the serum of these patients in an attempt to identify a marker which might allow for the early diagnosis of breast cancer.

[1] Risk S.L. and Sky-Peck H.H. Cancer Research, 44 (1984) 5390-5394. [2] Ehud J., Margolioth M.D., Schenker J.G., and Chevion M. Cancer 52K(1983) 868-872. [3] TallbergT., Mahlberg K., Kalima T., Present Status of Non-Toxic Concepts in Can-cer, Kargar, Basel (1987).

7

CHARGED PARTICLES ACTIVATION IN ANALYSIS OP PURE MATERIALS

Alexandrova G.I., Shmanenkova G.I., Pugatcheva O.P.

State Institute for the Rare Metals "GIREIMET",

Moscow, USSR

Charged particles activation with nHe, p, d as the basis

for sensitive methods of oxygen, carbon and nitrogen deter-

mination (I0~ -10" %) is used for high purity materials in-

vestigation as well as mass-spectrometry, neutron-activa-

tion and some other techniques. To estimate purity of tho-

se semiconductor materials, in which gas-forming impurities

are limited, the techniques have been developed.

For oxygen, carbon and nitrogen determination in silicon,

germanium, gallium arsenide, gallium phosphide and other

bulk crystals and structures, as well as in a large group

of metals. According to the developed techniques oxygen is

determined with 13 MeV He ions, carbon with 13 MeV 'He

ions or with 3-5 MeV deutrons and nitrogen with 6-10 MeV

protons. Having accelerated flows of these particles one

may choose optimum conditions for the analysis and reduce

or even completely eliminate interferences on the adjacent

light element nuclei. Thus, boron presence as a dopant in

some silicon grades makes the helium-3 ions usage for car-

bon determination impossible. This is also typical for the

gallium arsenyde prepared by the Czochralski technique un-

der a molten layer of BpO*. In this case the accelerated

deutrons are used for carbon determination.

The best experimental detection limites for these methods

which takes into account the etching and the matrix acti-

vity is 10 - 10"'% weight.

8

PRECISE 14 MEV NEUTRON ACTIVATION ANALYSIS

Andreev A.V., Varich O.M., Makarov S.A.

State Institute of Rare Metals

109017* Moscow J-17, U.S.S.R.

Besides of traditional domain of activation analysis appli-

cation, trace element analysis, this method now is success-

fully applied for precise (with accuracy better than 1 %

rel.) determination of element macroconcentration. In the

most extend it is valid for 14 MeV activation analysis.

Development of precise analysis techniques is much more dif-

ficult and time-consuming problem than development of just

high-sensitive ones. That is resulting from necessity

to take into account a number of sources of systematic and

random errors with make contribution to total accuracy

more than 0.1} rel.

Investigations of the error sources of 14 MeV activation

analysis made in the present work shown that the value of

all random error sources except of counting statistics can

be made as low as 0.1% rel. Because of trie spectroscopy sys-

tem count rate capability, it is complicated to lower the

value of statistical error to 0.1% rel. especially when

short-lived nuclides are used.

The most probable sources of systematic errors, making con-

siderable contribution to the overall accuracy are:

1. Certificated element content in the standard.

2. The difference of neutron flux self-shield effect and

]f-ray self-absorption in the samples and standards.

9

3. The certificated value of half-life period of the

nuclide analysed.

4. The affect of the total counting rate of spectroscopy

system during analysis of samples and standards.

The results of our study and developed techniques make it

possible to decrease the total contribution of different

sources of systematic errors to the value of 0.3 - 0.5

% rel. With the total accuracy of the large variety of

materials and elements determined is 0.2 - 0.8 % rel. The

results are given in Table 1.

Table 1. Precision determination of main components in some

compounds and compositions (confidence probability P=0.95)

Sample Mas3,mg Element Concentration S-

determinned % mass

Ru

0

Ru

Pb

Nd

0

0

0

V

Al

Nb

0

V

Nb

Zr

25.3 +

75.1 +

29.8 +

32.9 +

20.7 +

16.14+

20.28+

25.90+

79.5 +

23.3 ±

65.3 +

31.3 +

62.4 +

33.8 +

4.1 +

0.4

0.7

0.5

0.5

0.2

0.09

0.13

0.22

1.5

0.2

0.4

0.2

1.4

0.6

0.2

0.0057

0.0045

0.0076

0.0077

0.0055

0.0080

0.0080

0.0080

0.0080

0.0034

0.0030

. 0.00(46

0.0081

0.0051

0.015

S- - relative standard deviation of mean.

RuO, 193-8

Pb2Ru206(Nd) 521.7

YBa2Cu30?_x 6235.5

Ce02

Pr205

V-Al

LiNbO-

V-Nb-Zr

2584.1

2175.8

1234.6

150.5

4131«6

531-3

10

STUDIES OF DISTRIBUTION OF CHEMICAL ELEMENTS IN SUSPENDED MATTER AND BOTTOM DEPOSITS OF CONTINENTAL SHELF OF EASTERN CHINA SEA USING NEUTRON ACTIVATION ANALYSIS

V.V.Anikiev+, S.K.Prasad, T.Yu.Polyanova, G.M.Kolesov. V.I.Vernadsky Institute of Geochemistry & Analytical Chemistry, USSR Academy of Sciences, Kosygin Street 19, 117975, Moscow V-334, USSR; +Institute of Pacific Oceanography, USSR Academy of Sciences (DVO),Radio Street 7,690052,Vladivostok,USSR.

Recently activation analysis is considered to be one of the most modern mechods of analyses. This tool is used in carrying out wide range of investigations between dry and ocean currents to understand'formation of new sedi-ments and to undertake basic measures to protect sea and its surroundings from pollution. Keeping in view these two problems a small portion of the upper layer of the bottom sediment of Eastern China sea-shelf was chosen. This layer is formed by the direct influence of solid waste which was carried into the sea by the rivers Yunzi and Huanke.

Determination of chemical elements in the samples was undertaken with the help of Neutron Activation Analysis. Two types of irradiation were made for this purpose. In the first case samples were irradiated with^fast and _2 thermal neutrons under a flux of 1,2 X 10 ^neutrons cm s for 20 hours, and in the second case the samples were irradiated in cadmium filter for period of 80-100 hours. The sediment samples collected weighing in the range 15-20 mg and 50-60 mg, respectively, were analysed.

Irradiated samples were analysed at different time inter-vals to avoid interferences of radionuclides. So after lapse of 5 days and 3 weeks measurements were carried out with the help of a Ge(Li) semiconductor detector, multichannel analyser coupled with a microprocessor. The gamma-spectra and elemental concentrations were evaluated using a special computer programme.

The following groups of elements were used as indicators for different natural processes:

Alkali metals (Na,K,Rb,Cs) determine change in composi-tion of clay particles. Distribution pattern of lithophilic elements (Fe,Sc,Co, Cr) finds out the possibility of judging the relationship between surface sedimentary minerals and deep sedimen-tary minerals.

11

Carbonaceous materials can be compared by knowing the composition of Oa and Ir.

Distribution pattern of rare-earth elements (La,Ge,Sm, Eu,Tb,Yb,Lu) provides information of the influence of the processes like hydrolysis, oxidation, recovery, biological concentrations, complexation and sorption on the fractionation of chemical composition of sedimen-tary materials.

Rare elements (Th,Hf,Ia) give supplementary information necessary to have precise knowlege of assumptions and hypotheses.

Distribution of highly toxic elements like Sb and Gr decides the important link of these elements with waste disposal and river drainage.

Distribution characteristics and composition of macro and micro elements provide evidence for the movement of sedimentary material between land and ocean that takes place with fractional composition of this material under the influence of different geochemical processes.

12

Elemental Characterisation of Airborne Particulates at

two Nigeria locations during the Harmattaa season.

0.1. Asubiojo*, I.B. Obion**, E.A. Oluyemi*, A.P. Oluwole** and N.M. Spyrou***,

•Department of Chemistry, Obafemi Awolowo University, Ile-lfe, Nigeria.

••Department of Physics, Obafemi Awolowo University, Ile-lfe, Nigeria.

•••Department of Physics, University of Survey, Guilford, Survey, U.K.

ABSTRACT

Air Particulate samples collected during the harmattan season at two different locations - Kano in the Northern part, and Ile-lfe in the Southern part of Kigeria, were analyzed for up to 30 elements using a combination of Instrumental Neutron Activation Analysis and X-3ay Fluorescence Spectrometry.

The total suspended particulate in Kano i3 much higher than Ife, resulting in much higher elemental concentrations in the former than the latter, in some cases by as much as one order of magnitude (Table 1). For example, the^mean concentrations of Si and Pe in Kano are 270ug/m3 and 21ug/m-5

respectively compared to 73 #/E3 and 2 g/m3 respectively in Ile-lfe, However, the mean concentrations in Ile-lfe are ,^\ comparable to those of Summer/Early Vinter in Toronto, Canada^ \ for most of the elements determined.

Enrichment factors were calculated for elements in the airborne particulates at the two locations, using Titanium as the reference element. At both locations, the elements Ka, Mg, Al, I, K, Ca, V, Cr, Kn, Pe, Zn and Rb exhibited low enrichment factors (E.P. 3) which Co, Ni, Cu, pb and As exhibited high enrichment factors (E.P. 10). With the exception of V, which usually has significant anthropogenic contributions, most of the elements with low enrichment factors are generally of natural origin while those with high enrichment factors are conventionally associated with anthropogenic sources. Enrichment factors of about 100 and 10 were obtained for Fb and As respectively at both locations, which should give cause for concern because of the toxicity potentials of these elements. However, it is noted that the Nigerian samples are still less enriched in Pb than Toronto samples.

13

In Kano, most of the elements are concentrated in the medium particle-size range of 3-1,5 m, with the exception of Si which peaks at 3 m and 0.1*9 in» representing a mixture of medium and fine-sized particles, and S which has a clear bias for fine particles, understandably arising from fuel combustion. These results are not exactly in agreement with the results of KcTainsh and Walker (2) who found that Kano harmattan dust in 1^82 was mainly distributed between fine ( 2. m) and coarse particles ( 7*6 m ) .

For the Ile-Ife samples, we have a progressive increase in concentration of virtually all the elements, from coarse to fine particles. Here, it is evident that most of the elements are derived from a common source of fine particles, an indication of dust from the Sahara desert whose coarse components have been deposited along the way before reaching Ile-Ife, a Southern town some 200kra away from the source of the Sahara dust. Like Cawse and Beavington (3) observed earlier for Bagauda in the Northern part of the country, contribution of local entrained soil is minimal. It is also in agreement with Adedokun _et _al (k) who found that Ife harmattan dust is mainly composed of fine particles with a mode of 2,5 m. In line with the results of these previous workers, there is a higher concentration of most elements in the fine particle range in Ile-Ife than in Kano.

Table 1» Elemental Concentrations in Airborne Particulates.(ns/nr)

SleKent Ile-Ife Kano Al 18298 71360 As 1.96 Ca 5036 21*111* Co 90 230 Cr 17 131 Cu 219 U76 Fe 2072 21203 K 2995 69U1 Mg 2360 7959 Kn 93 655 Ha 13U9 6998 Mi 96 . 298 P 119 6I46 Pb 106 883 Rb 26 1*09 S 729 1723 Si 73363 269590 Ti • i+68 361*6 V 2.23 11 Zn * 90. '

14

REFERENCES

T.G. Pringle and R.E. Jervis, J. Radioanal. Nucl. Chem. 112 (1987) 210. "

G.H. McArinsh and P,H. Walker, Z. Geomorph. N.F., Vol. 26, No.J4: (1982) U17.

F. Beavington and P.A. Cawse, Sci. Tot. Environ. 10, (1978) 239.

J.A. Adedokun, V.O. Qnofurieta, O.A. A.dedeji, J. Theor. Appl. Clim. (in press).

15

Determination of 12 Rare-Earth Elements In High-Pure Sc 20 3 By Prctreatment

Neutron Activation Analysis

Bao Wei Dong Zhou Man Fang Yuan Ge.n Le

Beijing General Research Institute Of Non ferrous Metals

A method for the determination of 12 rare-earth elements in high-pure Sc,03

by pretreatment neutron activation analysis has been described in this

paper.The pre treatment proress of samples is that the scandium is extracted

by PMBP and butyl acetate at dilute acid. The Scandium is separeted from

rare-earth elements.The results of radioisotope tracer experiment proved

that the decontamination factor of scandium is over 4.5X10" and the

chemical yield of rare-earth elements is over 96%.The method can meet the

needs of neutron activation analysis.

After pretreatraent the sample is quantitatively transferred to 12 layers

12 x 12mm XIN HUA quantitative filter paper and is dried at GO'C/ then is

wrapped in a pure aluminium foil. Samples and corresponding standards are

packed together and irradiated in low temperature channels of the heavy

water reflective layer.The samples are irradiated for 5 hours and are

cooled for 2 days for the determination of La,Pr, Sm,Ho and the others are

irradiated for 20 hours and are cooled for 20 days for the determination of

Ce,Nd, Eu,Gd,Tb, Tin, Yb, Lu. After irradiation and cooling, the samples are

dissolved. The chloride solution of the sample is pr.ssed through a

preequilibrated P204 column at a definite flow rate.The column is washed

with different concentration HCL.Measuring soure is made. The gamma-ray

spectra of the samples is measured by S-9fl multichannel y -spectrum system.

The measuring time is 300-600 seconds for standards and 1800-3600 seconds

for samples.The experimental results and the detection limits are shown in

following table.

16

Table,The experimental results and the detection limits(PFm)

I 1 1 1 1

name/element ] La | Ce | Pr j

99.991) S c a 0 , | 0 . 9 5 + 0 . 0 2 5 | 2 . 4 3 + 0 . 3 8 | 0 . 3 6 + 0 . 0 5 7 |

this p u r i f i e d Sc.O, I 0 . 0 7 6 ± 0 . 0 0 9 4 | < 0 . 0 5 3 | < 0 . 1 3 | ' The d e t e n t i o n l i m i t s | 3 . 7 X 1 0 " 1 5 . 3 X 1 0 " I 0 .11 I

1 1 i j

( 1 f ] [ Nd | Sra | En | Gd | Th |

0.96 + 0.042 (0.14+0.0028 I 0.21 + 0.0017 |

STUDY 01' BRAZED iiZTD \ffiLDEC JOIBTO BY I'.iSTHODS OF

RADIOGRAPHIC ACTIVATION ANALYSIS

^orzina I. G. , Gusev .i. 3., Lukin V. I., Rilniko'v V. S.

L'ioscoiv Railway Transport Institute

1014-75 USSR, Moscow, GSP, A-55, Obraztsova, 15

Plash (n,°0 - radiograph was applied to study distribu-

tion of boron in both refractory nickel alloy joints bra-

zed by boron braze and parent material. Joints braaos of

different composition containing boron as the principal

component in charge of lowering of temperature in seam

area were investigated.

The effect of surface treatment prior to brazing on boron

distribution was studied. Depth of boron penetration into

parent material and nature of its distribution in seam

area were shown to depend on the kind of surface treat-

ment applied prior to brazing. Boron distribution in bra-

zed seam area depending on the shape of joint clearance

was also studied.

Structure of zones of boron distribution in brazed soam

area was investigated. Diagram of boron distribution in

brazed joints studied was drawn up. Principal zones of

seam area differing in boron distribution nature were

distinguished. Diffusion zones were found on both sides of

brazed seam which are not to be found by metallographical

tests. Faulty operating conditions were detected under

which sections lacking braze occur in seam clearance.

18

file:///ffiLDEC

It was found that boron penetrates parent material by both

diffusion of molt containing boron and diffusion of single

atoms.

Isothermal annealing after brazing was found to cause boron

re-distribution in all samples examined and its transition

from seam area to parent material accompanied by widening

of diffusion zone. Specific boron re-distribution among

brazed joint zones was observed in samples subjected to

isothermal annealing after brazing.

3oron distribution among zones of brazed joint was corre-

lated with its strength properties. Certain minimum width

of brazed joint clearance which determines absence of sec-

tions with minimum boron content and corresponds to high

strength properties' of joint was shown to exist.

(n,o£) - radiography tests, (p,o0 - microanalysis and x-ray

microspectrum analysis were used to find out distribution

of aluminium, magnesium and lithium (Al,Ivig,Li) in welded

joints of aliKiiinium-magnosium alloys. Distribution of Li,

Al and Mg in weld area was found to be uneven. Effect of

heat treatment on re-destribution of the above elements was

studied. Regimes of heat treatment which cause decrease in

Li and other elements concentration gradients in welded jo-

int area were determined. It was shown that there exists

certain correlation between distributions of Mg and Li, Al

and Li. Oxygen concentrations were found to rise in welded

joint area which occur at fatigne cracks. It was shewn that

lithium may serve as indicating element (both in positive

and negative aspects) to determine distribution of other

elements during welding.

Heat treatment of articles after welding was also shown to

equalize concentration gradients of the above elements.

19

OAK LEAVES FEASIBILITY AS

GASEOUS POLLUTION MONITOR

G. Capannesi, A. F. Sedda

ENEA C.R.E. Casaccia, S.P. Anguillarese 301,

Roma, Italy

A. Cecchi

Istituto Nazionale di Fisica Nucleare,

Largo E. Fermi 2, 50125 Firenze, Italy

A meaningful evaluation of air pollution in urban and in-

dustrial areas generally involve a great amount of measure-

ments over long time periods in order to minimize local

microclimates and sampling fluctuations.

The approach of choosing a biological monitor as repre-

sentative of the area of interest is highly attractive in

this respect.

In the past has been demonstrated that not only epiphytic

plants (Lichens, Briophytes) have the capability of equi-

librating their mineral contents with the environment, but

also superior plants, like evergreen oaks, "describe" quite

well their natural environment.

In the present work a wide set of analytical data from INAA

and PAA measurements on urban oak leaves (Rome) is examined

in detail.

Elements Correlation and Clustering was performed on the raw

data, so showing evidence of the capability of oak leaves as

20

gaseous pollution monitor.

Multiparameter Canonical Correlation Analysis and Principal

Components Analysis were performed, by taking into account

the analytical data and the characteristics of each of the

41 studied sites.

The capability of a quantitative description of the urban

pollution, also in relation with specific microsituations,

is investigated by Pattern Recognition Techniques.

21

STUDY OF TRACE ELEMENT IN HAIR SAMPLES FROM

TWO CHILDREN AT DIFFERENT DATE BY USING INAA.

G. Capannesi, L. Renzi, F. Sedda

ENEA C.R.E. Casaccia, S.P. Anguillarese 301,

Roma, Italy

Jin Li-Yun1

Institute of Atomic Energy. P.O. Box 275(29),

Beijing,China

Abstract: A study of trace element in hair samples from two

different sex children at different date by using INAA has

been carried out. The girl was born on Dec. 12,1973 and the

boy was born on Apr.27,1977. Both of them were born and live

in Roma. They are sister and brother. Each hair sample was

collected from the whole head by using a pair of stainless

steel scissors during hair-cut in barber shop. A total of 42

samples were collected, among them 10 for the girl and 32

for the boy.

Before irradiation, the hair samples were washed separately

by sonication in acetone and dried in a vacuum oven. Weigh

about 1 gram hair sample in a plastic tube for irradiation.

Standard pure solutions of the elements of interest and SRM

NBS 1573(tomato leaves), SRM NBS 1571(orchard leaves) were

used as comparison standard.

Hair samples were irradiated at TRIGA MARK 11 reactor of

ENEA,Casaccia. Long and middle-lived nuclides were produced

through 3 0 hours irradiation in the rotatory rack with

neutron flux of 2,6*1013n/(cm2*sec) . While the short-lived

nuclides were obtained after 100 seconds irradiation in an

in-core system provided with pnuematic transfer having

neutron flux of 1,l*1012n/(cm2*sec).

1. As a visit-scientist worked in ENEA C.R.E Casaccia during 1989.

22

neutron flux of 1,l*1012n/(cm2*sec).

The gamma-spectra of irradiated hair sample were measured by

means of a Ge(Li) detector with a resolution of 1,9 keV

(FWHM), efficiency 30 % and peak/compton ratio 57:1 at 1332

kev of 60Co photo-peak. The detector was connected to a

"LIVIUS" 16k multi-channel analyzer with gamma-spectrum

processing program, using several combinations of irradia-

ti»i:; time, cooling time and counting time, forty elements

were quantitatively analyzed. These elements are Al, Ag, As,

Au, Ba, Ca, Cd, Ce, Cl, Co, Cr, Cs, Cu, Dy, Hf, Hg, I, In,

K, La, Mg, Mn, Mo, Na, Rb, S, Sb, Sc, Se, Sm, Ta, Th, Ti,

Tm, Uf V, W, Zn.

The following conclusions could be drqwn from the data

obtained:

1, No regular changes were found for the trace element

content in the hair as a function of sampling date.

Some changes approximate to events such as breast fed

term and puberty term may be shield by other multi-

factors .

2, Significant changes for some trace element contents in

a few hair samples have been observed due to known ex-

ogenous and endogenous deposition, for example 841107

sample.

3, The relative variability of trace element content in

the hair is rather large for some elements such as K,

Rb, while for some other elements is much small, such

as Zn, Fe.

4, No significant differences for trace element content in

the hair were found as a function of sex. Nevertheless,

our data seem to indicate a trend towards higher con-

centrations in the girl.

5, The arithmetic mean of the hair trace element con

centration measured in the two children are rather

agreement with the comparable data reported for Italian

population.

23

D E T E R M I N A T I O N OF REE A B U N D A N C E S IN M I N U T E BIOGENIC APATITE B Y N A A A N D ITS GEOCHEMICAL SIGNIFICANCE

Chai Cliifang1, Ma Shulan1, Zhao Zhenliua2, Zhao Huilan2, Mao Xueying1, Ma Jiauguo1, Zhou Yaoqi1

1 Institute of High Energy Physics, Academia Sinica, P.O.Box 2732, Beijing 1000S0, China

2 Institute of Geochemistry, Academia Sinica, P.O.Box 91, Guiyang 550002, China

The biogenic apatites, like inarticulata and conodont, can be used indicators in the study of sedimentary paleoenvironment, since they are highly enriched in RES and bring the elemental geochemical signature of primitive marine sedimentary envi-ronment [1]. However, analytical methods with high sensitivity are indispensable to determine the REE abundances in such small fossil samples, usually several to tens micrograms in weight. Recently, Chen, et al. [2] analyzed the REE abun-dances in inarticulata by ICP. But it has some intrinsic disadvantages, e.g. large amount of sample and tedious chemical pretreatment, etc. For this reason, we used NAA to determine REE content in minute biogenic apatites, thereby deciphering their geochemical constraint on paleoenvironment.

The inarticulata and conodont fossil samples studied in this work are taken from the Cambrian-Ordovician boundary stratotype section at Dayangcha, Jilin province. Rinse the rock samples with 13% glacial acetic acid to remove the carbonate ma-trix. Separate the acid-insoluble residues with the CHBi-3 heavy liquid. Pick out inarticulata and conodont fossil samples from the heavy fraction under binocular microscope. Carefully clean the biogenic apatite with bidistilled water in an ul-trasonic cleaner to remove the detrital debris adhering to the apatites. Weigh the carefully cleaned inarticulata and conodont by a photoeletric balance (minimum readabilityiljUg). Due to small amount of sample, the neutron integral flux was 2xlO l &n/cm2 and the counting time was 104s or longer. In addition, a set of special dilute mix-standard was prepared to reduce geometric factor caused by difference between sample and standard in weight and size.

The REE abundances and their counting statistical errors of 12 inarticulata sam-ples and 1 conodont sample are listed in table 1, where also included are the REE abundances of NASC as a normalized reference. The geochemical significance of our results will be discussed in the full paper.

24

Wright, J., et al., Geol.Soc.Amer., Spec.Pap., 196(1984)325. Chen, .T.N., et al., Aspects of Cambrian-Ordovician Boundary in Dayan China, China Prospect Publishing House, Beijing, (1986) pp.62-91.

53 »rM O CI ••H =3

-*-» o> O

a

C M -^- 00 to *—« co co *—« co co co co e— ^« c— ^ OT> CO OO OO CM e— CM ~-* . . . . . . . . . . c*a

tO t« " 4 •^f ^t* CO CO t o p— IA •*• ~—< ^t*

CM tO ^ - CO >H - C«— CM CO tO tO CM CO ^** •

0*1 00 c— uri C M to 1 0 — * to C M co C M e— c o —< —i en C M -^* -̂» co -*• C M oa us 0 0

v—1 co to to -̂ r* c— cr> to t-» crt co ^ri 0 0 ~—* t-» co t— c»* 1 0 co co t-» co C M co cr» cr» co co trs C M ^ H t— C M - ^ 1—t ,—1 CO C— CM CO '—< CM 1—< 1—< CM tr>

IA CO CO OO » en >^ co oa t o •• en ~-i c—* cr» - •

t o ^» t— co co ^—* 00 - ^ —̂ tea |

J"1 iiiiiii

»—H C-"» •-* C O J 3 - C

^=S — 1

on - t s -*H I U C3 C O -fcJ OJ « j - — • U*

e s s

25

STUDIES ON SPECIATION OF TRACE ELEMENTS IN BIOLOGICAL

MACROMOLECULES

A. Chart* and C.K. Jayawickreme

Trace Analysis Research Centre, Department of Chemistry Dalhousie University, Halifax, Nova Scotia, B3H 4J1 Canada

Trace elements play an important role in the biological activities of living matter. A considerable amount of data on trace element levels of various biological tissues already exists in literature. In the past, many studies have been carried out to determine total elemental content. However, trace elements are mainly incorporated with proteins in biological matter. It is therefore important to isolate these protein-bound trace elements to identify the chemical species, and to characterize them for understanding their possible biological activities. Our interest lies in the development of analytical and bioanalytical methods for the characterization of metalloproteins and protein-bound trace elements in sub-cellular fractions of bovine kidneys.

Characterization of a metalloprotein may be carried out by one of the three following techniques. These are: (1) isolation of the protein followed by measurement of its biological activity; (2) incorporation of a radioactive tracer into experimental animals, and subsequent measurement of the tracer activity; and (3) purification of the metalloprotein followed by direct measurement of the trace element by a suitable analytical technique. The application of the first technique is obviously difficult because of limited knowledge of the biological (enzymatic) activity of a new metalloprotein prior to its isolation and identification. Although the second technique is widely used, the question remains whether a short-term exposure to a radiotracer could label all the proteins of that element to the same natural proportion. We have opted for the third technique. We have recently shown that the last procedure can provide new and exciting results on metallo-proteins if appropriate techniques are selected and applied.

Biological macromolecular species can sometimes be separated according to their isoelectric points, mobility, size, charge etc., and then the trace elements present in the species can be identified by a suitable analytical technique. The bioanalytical techniques being employed in this laboratory to separate, purify and characterize metalloproteins in bovine kidneys include dialysis, pH variation, ammonium sulphate precipitation, gel filtration, ion-exchange and hydroxylapatite chromatography, chromatofocusing, isoelectrofocusing and isotachophoresis.

26

The metal determination technique should meet several requirements including multielement specificity, ability to analyze a few milligram quantities of solid and liquid samples instrumentally, and excellent precision, accuracy and sensitivity. Instrumental neutron activation analysis (INAA) is ideally suited for such purposes.

The biological essentiality of Se for animals was first evidenced in 1957. However, it was not until 1973 that an enzyme called glutathione peroxidase was proven to be a selenoenzyme. At present, Se is known to be a normal component of several enzymes, proteins and some aminoacryl transfer nucleic acids. Certain Se compounds have been reported to possess anti-carcinogenic properties. Almost all of the work on selenoproteins reported in literature involves the usage of 75-Se radiotracer in rats and mice. We are concentrating our efforts in the separation and purification of selenoproteins in bovine kidneys followed by direct measurement of Se by cyclic instrumental neutron activation analysis (CINAA) using the Dalhousie University SLOWPOKE-2 Reactor.

Selenoproteins are generally known to concentrate in the cytosol fraction of animal tissues. An unusual enrichment of about 75% of Se in the nuclei fraction of bovine kidneys attracted our attention for an in-depth study. About 98% of this Se is bound to proteins. An elaborate extraction method has been developed at four different pH (7.0, 7.5, 8.5 and 9.5) to fractionate several selenoproteins from the nuclei fraction. Extensive studies of the fraction at pH 9.5 show the presence of three new selenoproteins called Selenoprotein C1 (Se content of 1200 ppm, molecular weight of 30 000 daltons), Selenoprotein C2 (270 ppm, 70 000 daltons) and Selenoprotein C3 (360 ppm, 80 000 daltons).

In addition to selenoproteins, several other metalloproteins and protein-bound trace elements have been detected in both nuclei and cytosol fractions of bovine kidneys. The existence of an arsenoprotein (MW 27 000 daltons) has been confirmed. In addition, gel filtration experiments show the presence of several proteins containing Ca, Cd, Cr, Cu, Fe, Mn, Mo, V and Zn. Most of these metalloproteins and protein-bound elements have not yet been reported in the literature. A systematic study on their separation, purification and identification is being done. Details of the approach and methodologies will be presented.

27

NEUTRON ACTIVATION ANALYSIS OF RHENIUM IN ROCKS

Chen YInliang and Vang Xiaoling Southwest Institute of Nuclear- Physics and Chemistry P.O. Box 515-25, Chengdu, Sichuan, China

A simple neutron activation method for the determination of rhenium preconcentrated from rocks Is described. The preeoneentration Is based on a prel Iiuinary extraction separation with acetone and latter separation with TBP column to eliminate the metal Impurities. The chemical recovery of each sample was determined by an Isotope tracer technique using Re-186. The method has been applied to the determination of rhenium in rocks and the experimental results are very well.

A sample and a known amount of Re-186 tracer In an teflon beaker (packed with copper beaker) and the mixture Is kepi: for 1 hour In a molten state In olee,trie stove. When the melt is cool, a amount of water are added and the teflon beaker is left for 20 min on a boiling water bath. Then the contents of the beaker are transferred quantitatively into a centrifuge tube and perform a two-fold extraction with 40 ml aceton saturated with 5 N KOH. Evaporate the combined aceton extracts to dryness In a beaker on a water- bath. The residue was' dissolved in 5 ml water and the resulting solution was passed through a column (h = 50 mm, d = 0 mm) packed with TBP. Thus all metal Impurities were eliminated. Perrhenlc acid together with washing liquors was collected in a teflon beaker. After treated with ammonia, thts solution was evaporated to a volume or 1 - 2 drops under an infrared lamp. Then it was transferred on a polyethylene foil and sealed with polyethylene. After the determination of the chemical recoveries, the penals and standards were irradiated in an reactor for 20 hours under the neutron flux of 1E13 n.cm(-2),seo(-l), cooled for 40 hours and counted with GefLi) detector.

28

PREPARATION AND CERTIFICATION OF THE HlffJAN HAIR REFERENCE MATERIAL

Cheng Yuandi, Wang Xuepeng, Qian Yine, Zhang Yuanxun, Tan Mingguang

Shanghai Institute of Nuclear Research, Academia Sinica

P.O.Box 800-204, Shanghai 201800, China

In order to meet the ever increasing requirements for the analytical

quality control in application of hair analysis, a human hair refe-

rence material has recently been prepared and certified by Shanghai

Institute of Nuclear Research, Academia Sinica.

Approxiamately 30kg of human scalp hair from normal male individuals

was collected. After pre-cleaning steps, the hair samples were

washed with a combined procedure of dilute non-ionic detergent, de-

ionized water and acetone successively with stirring. The dried hair

segments were pulverifsedto fine power (

values for t h i s material ( see Tab.l ) . Concentrations of these

elements are comparable with the typ ica l data for normals in l i t e r a -

t u r e s .

This ce r t i f i ed human hai r reference material vjill toe of prac t ica l

use for analyt ical qual i ty control and assurance in laborator ies

engaged in toiomedical and environmental s tudies .

Table 1 Certified Values for the Chinese Hair Reference Material (in /u,g/g dry weight)

Element

Ag

Al

As

Ba

B r

C a

Cd

CI

Co

C r

Cu

Fe

Hg

I

K

C o n t e n t

( 0 . 3 5 ) *

13.3 ± 2 . 3 * *

0 .59 £ 0 .07

(5 .41)

(0 .602)

1090 £ 72

0.095 £ 0.012

(152) -

0.135 £ 0 .008

4.77 £ 0 .38

23.0 £ 1.4

71 .2 ± 6 .6

2.16 £ 0 .21

(0 .875)

(11 .8)

Element

La

Mg

Mn

Mo

Na

Ni

P

Pb

' S

S b

Sc

S e

S r

V

Zn

C o n t e n t

(0 .014)

105 t 6

2 .94 ± 0 . 20

(0 .58 )

266 l 12

3 .17 ± 0 .40

(184)

7 .2 £ 0.7

(4.69%)

(0 .21 ) .

(0 .00287)

0 .58 ± 0 . 0 5

4 .18 £ 0.14

(0 .069)

189 £ 8

* Values in parentheses are reference values

** Certified values, uncertainties given are £ 2 standard deviation

30

UNCERTAINTIES IN THE CHARGED-PARTICLE ACTIVATION ANALYSIS AT CYCLOTRON

Era.Cincu and Al.Popa-Nemoiu

I n s t i t u t e of Atomic Physic ' s , Cyclo t ron Labora to ry P.O.Box MG-6, B u c h a r e s t , ROMANIA

In t h e l a s t y e a r s a number of works have r e v e a l e d a growing i n t e r e s t in t h e C h a r g e d - P a r t i c l e A c t i v a t i o n Analy-s i s , as a p p l i e d t o d i f f e r e n t f i e l d s , e s p e c i a l l y fo r i t s ad-vantage in i n v e s t i g a t i n g the t h i n s u r f a c e l a y e r s of mate -r i a l s , fo r i t s s p e c i f i c i t y and s e n s i t i v i t y in d e t e r m i n i n g t r a c e e lements - up t o s e v e r a l ppb -- as w e l l as for t h e p o s -s i b i l i t y of t h e s imul t aneous assay of many e lements by a n o n - d e s t r u c t i v e way / l / .

In d e f i n i n g t h e c o m p e t i t i v e n e s s of t h e method, t h e t o -t a l u n c e r t a i n t y on the weight f r a c t i o n va lues of the e l e -ments i s a major pa ramete r . This work dea l s wi th a d e t a i l -ed survey of t h e u n c e r t a i n t y s o u r c e s in CPAA, aiming at e v i d e n c i n g t h e l a r g e s t ones and at comparing them wi th t h e r e q u e s t e d s t a n d a r d i z e d va lues / 2 / and l i m i t s i n app ly ing t h i s t e c h n i q u e in i n d u s t r y .

CPAA was g e n e r a l l y developed at Cyclot ron f a c i l i t i e s at a medium energy range / 3 / . I t c o n s i s t s of four main com-p u l s o r y s t a g e s : sample p r e p a r a t i o n , t a r g e t i r r a d i a t i o n , measurements of t h e n u c l i d e induced a c t i v i t i e s - u s u a l l y by y - r ay s p e c t r o m e t r y - and c a l c u l u s of t h e weight f r a c -t i o n s of t h e e lements which g e n e r a t e d them: t h e r a d i o c h e -mical p rocedu re s as a u x i l i a r y s t a g e s , a re no t taken i n t o account .

The " t a r g e t r y " problems, t h a t i s t h e i n f l u e n c e of sam-p l e s c h a r a c t e r i s t i c s on the accuracy of t h e f i n a l r e s u l t s of n u c l e a r da ta measurements J2/, as t h e u n c e r t a i n t i e s i n -volved in t h e e s t i m a t i o n of t h e i n c i d e n t energy of t h e a c c e -l e r a t e d p a r t i c l e s in t h e a b s o l u t e beam c u r r e n t m o n i t o r i n g and t h o s e due t o t he i n s t a b i l i t y and geometry f a c t o r s in t h e i r r a d i a t i o n and measurement c o n d i t i o n s a re d i s c u s s e d .

An o v e r a l l va lue of t h e r e p r o d u c i b i l i t y u n c e r t a i n t y fo r t he l a t t e r combined s o u r c e s was s p e c i a l l y , e v a l u a t e d in exper iments conducted at t h e Cyclot ron of t h e I . A . P . - in Buchares t - and i s p r e s e n t e d in t h i s work : t h e maximum value of t h i s s t a g e was found £3% at a 95% conf idence l e v e l .

The u n c e r t a i n t i e s a s s o c i a t e d w i th t h e t h i r d s t a g e of t he a n a l y s i s , i n v o l v i n g t h e c o r r e c t e v a l u a t i o n of t h e ne t a rea of a f u l l energy peak ( . l oca t ion , shape , e f f i c i e n c y c a l i b r a t i o n , m u l t i p l e t deconvo lu t i on , v a r i o u s c o r r e c t i o n s ) and t h e a b s o l u t e c a l i b r a t i o n of t he y - r a y s p e c t r o m e t e r -

31

nuclear decay data included - are reviewed; the values range from 0.1% t o values

LIGHT ELEMENTS DETERMINATION USING ACTIVATION METHOD AT

THE IMPi! CYCLOTRON

B.Constantinescu, G.Pascovici, D.Plos/tinaru

Institute of Nuclear Physics and Engineering

Bucliar est, P.O. Box fcIG-6, Romania

During the past few years, elemental analysis methods

(Pl'XE - for Z > 17 elements, PIGE for IT, 0, P, Na, Mg,

Al, Si) using 4.7 MeV alpha particles at our variable-

energy U-120 Cyclotron have been developed /l/. For the

other light elements the charged-particle activation

• method can be suitable. V/e present some results about P

and S determination using 22 JileV alpha particles, 14 I.ieV

protons respectively, and some considerations about the

possibility to use in elemental analysis (especially for

0) fast neutrons produced by Cyclotron deuterons on a

berrylium thick target.

So, for P we have used the reaction:

^P(

irradiation (10-15 min) through a 100 jx Al foil. The

samples (various polymers) were measured 15 min after th?

end of irradiation using a 70 cm Ge(Li) detector in a

lead shielded area. Triphenylphosphyne (CTOH-JCP) mixed

with polyethylene standards were used. For polymers the

sensitivity is about 5 ppm.

For S v/e have used the reaction:

lGs(P>n)3/^'Cl (T1/2 = 32.5 min) Ji) ̂ = 2120 keV

in the same irra'diation and measurement conditions.

Ammonium sulphide (NH^gSO^ mixed with polyethylene

standards 'were used. The sensitivity for polymers is

about 30 ppm.

Intense fast-neutron beams (7.8 x 10 n/cm4«s, E = 5 MeV

can be produced using 13 MeV Cyclotron accelerated

deuterons on a berrylium thick target.

For 0 determination, the reaction:

1|o(n,p)1^T (T1//2 = 7.3 s) E-, = 6130 k-V is suitable

10 s irradiation and 20 s measurements with a 12.5 cm x

12.5 cm Nal(Tl) crystal can be used. In this mode, we can

aloo determine Mg, Al, Si, Fe. The work is in progress.

/I/ Constantinescu, B. et al, Appl.Radiat.Isot. 37, 1

(1986) pp. 53-60.

34

AMAZON BASIN: TRACE ELEMENTS IN VARZEA SEDIMENTS

Elisabete A. De Nadai Fernandes; Epaminondas S.B. Ferraz; Luiz A. Martinelli & HelderdeOliveira Centro de Energia Nuclear ne Agriculture, USP P.O.Box 96 13400, Pirocicaba, Sao Paulo, Brasil

The Amazon Basin is the largest active river system both in drainage area (7-106 km2) and in freshwater volume discharged to the oceans (5.5 -102

kmVa) [1]. In terms of sediment yield as a consequence of weathering process, large amount of material originated from the upper drainage areas enters the streams of the region like suspension sediments, which can be temporarily stored or trapped in the lower drainage areas (Amazonian depression) every year through periodic floodings, instead of reaching directly the ocean. These floodlands in the Amazonian landscape ore called by varzea and occupies an enourmous area of about 60,000 km2, being a very productive land which is fertilized annuely by the flood-water.

<

As part of an effort to improve the knowledge concerning weathering rates in Amazonian rivers, the chemical composition of sediments and suspended matter is being assessed applying complementary analytical techniques. In the present paper the main attention is paid to the determination of some trace elements in varzea sediments by neutron activation analysis. In 1985, after reaching the peak of the annual flood (discharge of 203,000 nf .s - l in Obidos, site 16), twenty-four samples of the uppermost 20 cm of the sediments were collected, being 19 8long 2,300 km from the Amazon itself and 5 from all the major tributaries (Fig.1).

. R. Amazonas .—^

B | \ 2 3 4 5 6 ? V 8 9 10 Il\l2 13 J4\l5 16 17 18 19

2000 Km _J I i i — i -

Fig. 1. Schematic drawing of drainage area of the Amazon.

Special care has been taken to assure homogeneity in preparing the samples. Ca 200 mg of each sample were placed in polyethylene tubes and irradiated

35

together with IAEA standards in a nuclear reactor at a flux of about 5 MO12

n.cm"2.s"1 for 8 hours. Following by high resolution gamma-ray spectrometry with a germanium semiconductor, over 23 elements were determined. Analytical data showed in Fig.2 were normalized by dividing the compositions of tributaries samples by the average for the main river samples. The hypothesis that there is a difference in trace element composition of v&rzeas from various sites in the whole drainage area was tested. No significant differences in chemical composition were apparent except for Negro river in which i t changed abruptly, falling out of general trend and showing distinct variations from the average, as i t was expected. According to geomorphologycal studies 12), the basins of tributaries lea, Jurua, Purus and Madeira have the same sedimentary origin from Tertiary-Quaternary, while the Negro basin is related to the Crystalline basement. It has been noted that the same behaviour was achieved for macronutrients analysed in the same samples 13].

300

200

100-1=*,

Fe Sc Hf La Co Th

Fig. 2. Relative contents of some elements.

I I ] Kronberg, I.B.& W.S. Fyfe, SCOPE/UNEP, 55(19Q3) 215-222. 121 Sioli, H. Tropica) River: The Amazon. In: B.A. Whitton, ed. RIVER ECOLOGY,

Berkeley, U.C. Press, 461 -487. [31 MartinelU, LA. Thesis, ESALQ/USP, Plrecicaba, SP (1986) 214 p.

36

QTimv ni? nnDnw TM i F T J I M P pnDPAr.p

flower tissues, ca(yx has the,highest boron content.

B tracer experiment shows that root application of boron

has the highest rate of boron absorption by plant and

boron applied to leaves mainly remains in the treated

areas.

CI) Duval, Y., Thellier, M. J., Radioanal. Chem. 55 (2),

1980.

\Z) Szabo, A. S., Isotopenpraxis, 17 (7) (1981) pp. 275

- 278.

\3) Deng Hongnin et al., Research and Application of Trace-

Element fertilizers, Hubei Science and Technique Fress

U985.J PP. 31/+ - 32A.

38

MEASUREMENT OF FILM THICKNESS BY 14 MeV NEUTRON ACTIVATION

ANALYSIS

P.M. Dighe, G.R. Pansare and V.N. Bhoraskar

Department of Physics, University of Poona,

Pune-411 007, India.

Thickness of individual copper, aluminium and silicon thin

films deposited as single and multilayer coatings have been

measured using 14 MeV neutron activation analysis . technique.

Weights of aluminium films estimated with an accuracy of 1 %

indicate slight deficit in the film density below thickness

around 300°A. Several methods are routinely used for thickness

measurement of single layer films which are however not useful

for multilayer coatings. The RBS is a powerful technique for such

studies however tedious calibration procedures are to be carried

out and many a times the spectrum is masked with continuous

energy of the backscattered He-4 ions when the first layer is

thick and of high z material,,followed by low z layers. The 14 MeV

neutron activation analysis technique has no such limitations.

Thin films of pure aluminium, copper and silicon were deposited

in clean vacuum ~ 10~6 torr on perspex and glass substrates by

vapour evaporation technique, keeping area of each film close to

one sq cm. Thickness of each film was measured in situ by a

quartz crystal monitor and later on by stylus method. Each film

on irradiation with 14 MeV neutron flux ~ 10° n/cm /sec was

brought to HPGe (30 %) detector and the induced gamma ray

activity was recorded in a M.C.A. The nuclear reactions used for

aluminium, silicon and copper are given below respectively by

expressions [1], [2] and [3].

39

27Al(n,«C)24Na, T 1 / 2 = 15 28Si(n;p)

28Al, T 1 / 2 = 2.3 Hrs.

USE OF 14 MeV NEUTRONS IN ANALYSIS OF EXPLOSIVE CLASS MATERIALS

P.M. Dighe, G.R. Pansare, S.G. Kulkarni and V.N. Bhoraskar

Department of Physics,

University of Poona,

Pune-411 007, India.

Analysis of explosive and propellants is often carried out

to assess their suitability for practical applications. Among

other contributing factors, the type of elements and their

relative concentrations are important to decide optimum power

levels obtainable from given sets of explosives and their

ingredients. Nitorgen and oxygen are present in various classes

of explosives and propellants whereas aluminium is added to

increase power of underwater explosives. Ammonium percholarate is

another important compound and its concentrations can be obtained

on the basis of chlorine content. It is known that propellants,

specially double base and CMDB type on long storage have tendancy

to undergo slow decomposition with evolution of nitrogen in the

form of its oxides. As a result the value of the nitrogen to

oxygen ratio deviates from the original set value which often

adversely affect the properties of the propellants. There are

several known methods [1-3] based on chemical analysis which can

be used for estimation of concentrations of oxygen, nitrogen,

aluminium and chlorine. However most of these methods are

destructive, need considerable handling of materials, time

consuming and carry added risk of explosion when used for

it Institute of Armament Technology, Pune-411 025, India.

41

explosive class materials. Overcoming all these difficulties, 14

MeV neutrons activation analysis technique has been successfully

used in this laboraotry for analysis of several type of explosive

class materials, such as torpex and dentex familir es, containing

RDX, TNT, HMX, Al and wax. Some of the polymers like

nitrocellulose, polymeric binders, and plastic bonded explosives

were also analysed. Sample of quantity in the range 10 to 100 mg

was irradiated with 14 MeV neutron flux - 10 ii/cm"/sec and the

induced gamma ray activity was measured using a 3"x3" Nal(Tl)

detector or HPGe (30 %) detector coupled to a 4096 channel

analyser. To estimate concentrations oF. oxygen, nitrogen,

aluminium and chlorine following nuclear reactions were used

160(n,p)14N, T 1 / 2 - 7-35 sec. 6 = 42 mb (1) 14N(n,2n)13N, T 1 / 2 = 9-96 Min. 6" = 5.7 mb (2) 27Al(n,p)27Mg, T 1 / 2 = 10 Min.

INAA OF VEINED PYROCLASTIC ROCKS FROM ABAKALIKI, LOWER BENUE TROUGH, NIGERIA.

L.A. Dim, J, Adetunji, CD. Okujeni , *

S.A. Agaja and G. Gudmar

Department of Physics, Department of Geology,

Ahmadu Belle University, Zaria, NIGERIA.

Department of Reactor Physics, Chalmers

University of Technology, Gothenburg,

SWEDEN.

Abs