Determination of phosphorus in polymers by INAA

An INAA technique employing beta spectrometry was developed for the determination of phosphorus in polymers. The (n,γ) reaction on phosphorus produces³²P, half-life 14.3 days, a pure beta emitter with end-point energy 1.71 MeV. Polymer samples in the form of powders, films and pellets are irradiated and then counted with a plastic scintillator. The beta spectrum is corrected for interferences (especially Sb, Zn and Br which are quantified by gamma spectrometry) and for energy loss in the thick sample. Samples must also be analyzed for S and Cl which cause nuclear interferences. With an irradiation time of 4 hours at a neutron flux of 5·10¹¹ n·cm^{−2 s −1}, decay time 10 days and counting time 10 minutes, the sensitivity is 520 counts/μg phosphorus and the detection limit is typically 2μg/g.     

Determination of major,minor and trace elments in textile dyes by INAA

Thirteen textile dyes have been analyzed by the method of insturmental neutron activation analysis for their components of major and trace elements, and the concentration of thirteen elements in these samples are presented.     

Determination of trace elements in honey by INAA in Turkey

Instrumental neutron activation analysis was applied to the determination of As, Cr, Sb, K, Br, Zn, Fe, Co in Turkish honey. Irradiation time was 6 h underwater at a thermal flux of 10¹³ n cm^–2 s^–1; cooling times of 100 h and 3–4 weeks and counting times of 5000 s and 80.000 sec were used. The detection limit for As is 0.01 ppm for honey matrix under these conditions. A technique was developed for sealing the quartz tube containing the honey with flame.     

Determination of major,minor and trace elements in Iraqi vegetable samples by INAA

Our aim was to discover a method of separating zirconium(IV) and uranium(VI) from solutions. It is known that Zr(IV) and U(VI) are effectively extracted by tertiary amines from weak acidic sulfate solutions but the possibility of extraction decreases with increasing acidity. The transition from tertiary amine to primary amine Primene JMT enables the extraction of Zr also from more acidic solution. If both Zr and U are present in an aqueous solution, Zr is extracted preferentially and only the free part of the amine can convert uranium to an extract. The separation described below was carried out by preferentially stripping zirconium from the organic phase. The application of nitrate solution (2M HNO₃) to eliminate Zr from the solvent was tested. This method does not demand any special regeneration of the extraction agent and the amine nitrate, formed in the organic phase, can be used for further extraction of Zr without modification. Using this method of separation, a solution for producing pure ZrOCl₂·8H₂O was obtained.     

Determination of rare earth elements in rice by INAA and ICP-MS

In order to improve the accuracy of reactor neutron activation analysis, flux gradients and spectrum changes in the irradiation capsule have been studied at the Kyoto University Reactor (KUR). The flux and spectrum monitoring samples of Fe, Co, Au, Sb, U and Ni were placed at several positions in a polyethylene irradiation capsule of 24 mm inner diameter and 98 mm length, and were irradiated in a pneumatic irradiation facility (Pn-2). The flux gradients were found to be rather negligible in the vertical (axial) direction while they were considerable in the radial one. The flux gradient was around 5%/cm for thermal neutrons and 10%/cm for epithermal and fast neutrons. The spectrum changes were dependent on the materials (polyethylene and silica) filled in the capsule. Based on these observations, the effect of the flux gradients and spectrum changes on the accuracy of reactor neutron activation analysis was discussed.     

Determination of dysprosium by INAA in some Bulgarian standard rocks

Dy content has been determined by INAA in the Bulgarian standard rocks BV, GV, DM, MrA, OgG, OZnO and in the IAEA standard reference materials SL-1, SOIL-5, and SOIL-7. Results are compared with Dy values obtained by interpolation of the chondrite-normalized contents of other REE in these samples.     

Determination of REE by INAA in conodont apatite of Triassicage

Instrumental neutron activation analysis is applied to determine REE in very small, toothlike elements of an extinct animal, the conodont. The results are useful to obtain records of local oceanic events and processes connected to plate tectonics in the Tethys ocean from about 250 to 200 million years ago.     

Determination of hafnium in zircaloy clad by means of INAA

Three reactions are described for the analysis of small concentration of Hf in zircaloy clads used for BWR and PWR reactor. One of the measurements is based on the measurement of short-lived^179mHf /18.7 sec/. The method is fast, selective, highly sensitive, non-destructive and has a detection limit of 1.3 ng for Hf.     

Determination of trace elements in Wuxi fallen ice by INAA

The concentrations of 14 elements, including Ir, Au, Co, Cr, Fe, Sr, Rb, K, Ta, Zn, Sb, Ba, Sc and Se, in the Wuxi fallen ice were determined by neutron activation analysis. The experimental results show that the relative concentration ratios of Ir/Co, Ir/Cr and Ir/Sc etc. in the ice water (0.0069, 0.00024 and 0.11, respectively) are quite close to those of Type C1 chondrite (0.0102, 0.00021 and 0.092, respectively), which implies that the fallen ice might be a piece of extraterrestrial substance.     

石墨炉原子吸收法直接测定血清中硒,砷

选用Ｐｄ－Ｎｉ－Ｔｒｉｔｏｎ Ｘ－１００为基体改进剂，用石墨炉原子吸收法直接血清中砷、硒。该法具有操作简单、快速、灵敏度高的特点，为临床测定血清中砷、硒提供了一种新方法。     

Determination of trace and toxic elements in Korean rice CRM by INAA, ICP and AAS

Trace and toxic elements in Certified Reference Material (CRM) made of Korean rice at the Korea Research Institute of Standards and Science have been analyzed by Instrumental Neutron Activation Analysis (INAA). Data intercomparison from the measurement with those of Atomic Absorption Spectrometry (AAS) and Induced Coupled Plasma Spectrometry (ICPS) has been studied. The powdered samples were sterilized at 1.5·10⁶ rad in the bottles using a⁶⁰Co source after sieving and spiking to specific elements such as As, Cd, Cr, Cu and Hg and then the homogeneity of samples was assessed. Rice flour (SRM 1568a) and standard solutions made by the National Institute of Standards Technology (NIST) were used to construct the calibration curves for the INAA and the chemical methods, respectively. The uncertainties and concentration of constituent elements were determined and the possibility of their use for analytical quality control was considered.     

Determination of trace elements in Na-bentonitic clay by INAA in Turkey

Instrumental neutron activation analysis was applied to the determination of trace elements in a Na-bentonitic clay. The irradiation was done in the Triga Mark II type reactor of ITU Nuclear Energy Institute. The sample was irradiated in two steps for short- and long- lived isotopes. After irradiation, spectra were taken using a germanium detector, multichannel analyzer Canberra System 100 and a fitting program called Sampo 90. The spectra of short-lived isotopes were analyzed to determine Al, Mg, Na, K, Ca, Ti elements and Mn, V trace elements. The spectra of long-lived isotopes were analyzed to determine Sc, Br, Sb, Cs, La, Ce, Sm, Yb, Hf, Pa, Np trace elements.     

HG-ICP-AES测定马蹄金中As、Se含量

采用流动氢化物发生电感耦合等离子体-原子发射光谱法(HG-ICP-AES)分别对马蹄金在酸性条件下经超声煎煮后得到的酸提取液和滤渣中As、Se含量进行了测定。结果表明:(1)马蹄金中As含量较低,低于1.0μg/g,而Se含量则较高,可达6.298μg/g;(2)酸提取液中Se含量随煎煮时间延长有所增加,而As含量则有所降低。为进一步研究马蹄金的药理药效和合理开发利用药物资源提供了科学依据。     

Determination of trace elements in high purity copper by INAA, GFAAS and ICP/AES

Trace impurity elements in high purity copper metal (4 mine class) put on the market were analyzed by Instrumental Neutron Activation Analysis (INAA) and the results compared with those from Graphite Furnace Atomic Absorption Spectrophotometry (GFAAS) and Inductively Coupled Plasma Atomic Emission Spectrophotometry (ICP-AES). The sample irradiation was done at the irradiation facilities (thermal neutron flux, 5·10¹² n·cm⁻²·s⁻¹) of the TRIGA Mark-III research reactor in the Korea Atomic Energy Research Institute. Four unalloyed copper standards (NIST SRM # 393, 394, 395 and 398) were used to identify the accuracy and precision of the analytical procedure. The homogeneity of samples was assessed by means of the elements such as Ag, As, Co, Sb, Se and Zn. The analytical results of INAA, GFAAS and ICP-AES were in good agreement within expected uncertainties each other and showed the possibility of using them for the analytical quality control.     

Determination of some trace elements in the thyroid gland by INAA

Neutron activation analysis without radiochemical separation was used for simultaneous analysis of eight trace elements in thyroid glands, obtained as necroptic material from persons not suffering from diseases of this gland. Inorganic standard solutions were used for calculations of concentrations of measured elements. Concentrations are expressed in ppm, or ppb. IAEA reference materials were used for quality assurance of analyses. From analyses of 42 thyroids concentration levels of Se, Cs, Sc, Fe, Cr, Zn, Co, and Rb and their variances in the thyroids were calculated. These results might serve as comparison material for medical research of pathological and functional changes in thyroid glands.     

INAA study of Hg, Se, As, and Br irradiation losses from l-cysteine treated and untreated reference materials

U. S. Food and Drug Administration in-house reference material (RM) Cocoa Powder and National Institute of Standards and Technology Standard RMs (SRMs) 1515 apple leaves, 1547 peach leaves, 1571 orchard leaves, 1566a oyster tissue, and 1568a rice flour were co-irradiated together with polyethylene blanks and analyzed for Hg and Se by anticoincidence instrumental neutron activation analysis. The three botanical SRM portions showed a combined Hg recovery of 70 % while the other portions showed a combined Hg recovery of 169 %, indicating that volatile Hg was lost from botanical SRMs and absorbed by the other irradiated portions. Total Hg recovery for all portions was 82 %. Se results showed no evidence of cross-contamination and all results agreed with certified and known values. National Research Council of Canada Certified RMs DOLT-3 dogfish liver, TORT-2 lobster hepatopancreas, and DORM-3 fish protein were separately analyzed either with no treatment or after treatment with l-cysteine solutions followed by drying over magnesium perchlorate. Each set of portions was co-irradiated with polyethylene and treated filter blanks. Analysis of all components of each treated portion irradiation package showed that essentially all Hg was retained within the package. Treated DOLT-3 portions (inorganic Hg content 53 %) showed a tenfold improvement with 99 % Hg retention. Hg retention for DORM-3 (7 % inorganic Hg) was 85 % (a twofold improvement) while retention for TORT-2 (44 % inorganic Hg), was 94 %, similar to that for untreated portions (96 %). Small irradiation losses (≤0.5 %) of volatile species of Se, As, and Br were observed.     

Determination of the total amount of organically bound chlorine,bromine and iodine in environmental samples by instrumental neutron activation analysis

The determination of chlorine, bromine and iodine present as non-polar, hydrophobic hydrocarbons in environmental samples is reported. The organohalogen compounds are separated from water into an organic phase by on-site liquid—liquid extraction, and from biological material by procedures based on lipid phase extraction and codistillation. After removal of inorganic halides by washing with water and concentration of the sample by evaporation of the solvent, the resulting extracts are analyzed for their chlorine, bromine and iodine contents by instrumental neutron activation analysis. Strict attention is paid to the possibility of contamination in every step of the procedure. Background values in routine analysis are approximately 100–200 ng of chlorine, <5 ng of bromine and <3 ng of iodine.     

Determination of 21 elements by INAA for certification of SRM 1570a,Spinach

Analyses for certification have been made by instrumental neutron activation analysis (INAA) for the determination of 21 elements in the National Institute of Standards and Technology (NIST) Spinach renewal reference material, SRM 1570a. Elements determined included ones with short halflife products (Al, V, Ca, Mg), intermediate halflife products (Mn, Na, K, La), and long halflife products (Ba, Co, Cr, Cs, Eu, Fe, Rb, Sb, Sc, Se, Sr, Th, and Zn). For the first time a new robotic sample changer was used in the counting of long halflife indicator isotopes for certification of an SRM. Uncertainties obtained averaged±1.80% for the four major and minor constituents (Ca, K, Mg, Na); ±3.14% for elements with concentrations from 1 to 400 mg/kg (Al, Ba, Cr, Fe, Mn, Rb, Sr, and Zn); and±8.31% for the ultra trace elements (<1 mg/kg) (Co, Cs, Eu, La, Sb, Sc, Se, Th, and V).     

Use of INAA to study the interaction between Ag and Se,Zn, Rb,Fe or Co in mice

The interaction of inorganic silver (as AgNO₃) with SeO₂ and Se-compounds was studied. Instrumental neutron activation analysis (INAA) was applied as the analytical method. Organ concentrations of Ag were always significantly higher 72 hours after simultaneous intraperitoneal injections with AgNO₃ and Se-compounds. Moreover, simultaneous injections elevated the Se-content in organs examined. We suggest that Se-compounds protect against liver lesions by markedly decreasing the concentration of Ag in this organ 2 hours after simultaneous injections. It was also found that Ag supply affects the contents of Zn, Rb, Fe and Co.     

Determination of concentrations of U and Th in their mixed oxides by INAA methods

Uranium and thorium mixed oxides are being prepared using natural U and Th for studies on fuels for Advanced Heavy Water Reactors, wherein composition of U and Th is specific and requires strict control in terms their contents and homogeneity. Chemical quality control necessitates accurate and precise compositional characterization of the fuel material by a suitable analytical method. Among various analytical methods for U and Th, instrumental neutron activation analysis (INAA) is one of the best methods for their simultaneous determination without chemical dissolution and separation. INAA methods using reactor neutrons namely thermal NAA and epithermal NAA were standardized for the determination of U and Th in their mixed oxides. Standards, synthetic samples and U–Th mixed oxide samples, prepared in cellulose matrix, were irradiated at pneumatic carrier facility of Dhruva reactor as well as at self serve facility of CIRUS reactor under cadmium cover (0.5 mm). Radioactive assay was carried out using a 40% relative efficiency HPGe detector. Both activation and daughter products of ²³⁸U (²³⁹U and ²³⁹Np) and ²³²Th (²³³Th and ²³³Pa) were used for their concentration determination. The method was validated by analyzing synthetic samples of 6–48%U–Th mixed oxides. The standardized method was used for the concentration determination of U and Th in 4–30%U–Th mixed oxide samples. Results of U and Th concentrations including associated uncertainties obtained from the INAA methods are presented in this paper.