Because trace elements play an important role in environmental and biological fields, environmental and biological samples should be analyzed with good accuracy and precision. The best approach to ensure the accuracy and precision of a measurement is to use appropriate reference materials.The National Institute for Environmental Studies of Japan (NIES) has supplied various environmental certified reference materials (CRMs) for the quality assurance of environmental analysis.1 Our laboratory participated in an intercomparison analysis program of NIES candidate river sediment CRM No.16 by using instrumental neutron activation analysis (INAA).In INAA the Compton plateau from high-energy γ -rays often interfers with identification of nuclides with lower energy γ -rays. For example, 24 Na and 82 Br are the main interferents in INAA of environmental and biological materials. After the decay of short-lived interferents, such long-lived nuclides as 46 Sc and 65 Zn are responsible for a high Compton background, which leads to poor detection limits in the lower energy region. INAA combined with Compton suppression γ-ray spectrometry can reduce this problem. In order to determine as many trace elements as possible with high sensitivity, we used conventional γ -ray spectrometry with a coaxial Ge detector, and two Compton suppression γ-ray spectrometries (anti-coincidence 2 and coincidence 3 ) with a coaxial Ge detector and a well-type NaI(Tl) detector. By using γ-ray spectrometries, more than fifty elements can be determined instrumentally with satisfactory results.
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Experimental
Preparation of sampls and standardsFour samples (about 230 mg) of NIES candidate river sediment CRM, collected from the lower Tama River, were weighed. Each sample was doubly packed in clean polyethylene bags for irradiation.Approximately 1 g of a separate sample was dried for 4 h at 110˚C in an electric oven. The moisture content was 1.3%, and a weight-loss correction was applied in the final results. Acidic standard solutions for atomic absorption spectrometry were used as comparative standards. Each standard solution of 10 -200 µl was pipetted onto clean filter papers, which were doubly packed in clean polyethylene bags.
Irradiation and γ-ray countingThese samples and comparative standards were irradiated for a short time and a long time at the Rikkyo University Research Reactor (TRIGA Mark-II, 100 kW). Pneumatic transfer at a thermal neutron flux of 1.5×10 12 n cm -2 s -1 was used for short-time irradiation (10 s) and the central thimble at a thermal neutron flux of 3.7×10 12 n cm -2 s -1 was used for long-time irradiation (6 h).For long-time irradiation, neutron flux monitors (10 mg of Al wire containing 0.15% Sb) were irradiated together with samples and comparative standards. The neutron flux of samples and comparative standards was corrected using the 122 Sb and 124 Sb activities of irradiated Al wires.Irradiated samples were measured by conventional γ-ray spectrometry using a coaxial Ge detector, and by anti-coincidence and coi...