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3 (1999) 693-701
The concentration of 35 elements (AI, As, B, Ba, Be, Ca, Cd, Co, C1, Cr, Cu, Fe, K, Mg, Mn, Mo, N, Na, Ni, P, Pb, Rb, S, Sb, Sc, Si, Sr, Tb, Th,
Ti, U, V, Yb, Zn and Zr) in six different imported, NPK, NP and K fertilizers were determined by ICP-OES in two different laboratories and by
INAA. The fertilizers were labeled as 24/12 (Belgium), 46/18 (Morocco), 50% ammonium sulfate 50% K20 (Belgium), New 24/12 (Belgium),
16.8.24 (France) and 17.17.17 (France). It is clear that these fertilizers vary widely in their heavy metals and uranium content, and the
accumulation of certain elements in vitally important media such as water, soil and food is undesirable from the medical point of view. The results
obtained were acceptable and intercomparison between various methods was carried out.
(1) Dissolution in nitric acid or a mixture of nitric The resulting liquid samples are nebulized by a V-
and hydrochloric acid. 700 mg fertilizer sample powder groove nebuliser arrangement with an argon flow rate of
was measured into a glass flask on an analytical balance; 0.8 dm3/min, giving approximately a 3.0 cm3/min sample
then 3 cm 3 of high purity HNO 3 (70 m/v%) was added to uptake rate. The specification of the operating conditions are
the sample, the flask was placed into a block heater and given in Table 2. For calibration and quality control a set of
heated below the boiling point of the acid (set to 120 ~ multielement standard solutions was used.
for 30 min). This time was sufficient to dissolve most of
the samples. Sample No. 4 was not fully dissolved, some Instrumental neutron activation analysis (INAA)
black material was observed floating, by adding a few
drops of HC1 acid and heating for another 30 minutes The irradiations were performed in the Training
most of the residue was dissolved, but some black reactor of the Institute of Nuclear Techniques, Technical
material remained. By subjecting sample No. 4 to HPLC University of Budapest. The maximal thermal neutron
analysis, an oil layer coating the sample was observed. flux was 2"1012n'cm-2"s-1 and the maximal thermal
This oil was used for controlled-release of this type of power was 100 kW. The samples were irradiated in two
fertilizer. All the sample solutions were cooled down and steps and the ~/-spectra were detected by a HPGe well-
filtered into a volumetric flask and made up to a final type detector (FWHM: 2.1 keV, and 17.5% relative
volume of 25 cm 3 with distilled water for ICP analysis. efficiency at 1332.5 keV) for the analysis of short-lived
The solutions represent the acid soluble part of the nuclides, and a HPGe Pop Top type detector (FWHM:
fertilizers. 1.7 keV, and 26% relative efficiency at 1332.5 keV) for
(2) Dissolution in hydrofluoric acid. 0.150 g of the long-lived nuclides. The resulting T-spectra were
powdered sample was transferred into a PTFE bomb. analyzed by using Sampo 90.
Then, 2 cm 3 hydrochloric acid (36 m/v%), 1 cm 3 nitric Standards from NIST (SRM 1633a and 1571) and
acid (70 m/v%) and 1 cm 3 hydrofluoric acid (40 m/v%) IAEA soil-7 were used for calibration and quality
were added. The bomb was closed and the dissolution control. Detailed descriptions of the 1NAA procedures
was carried out under pressure at 130 ~ for 4 hours. have been published earlier. 4
Then the bomb was cooled down to room temperature Direct gamma-spectrometry: Samples and standards
and opened. Ten cm 3 of 6% by weight boric acid were placed in plastic tubes of 5 cm 3 volume capacity.
solution was added and the bomb was closed again and The cell was closed and left for at least four weeks
kept at 80 ~ for 30 minutes to complex the excess of before being counted to allow for radium and its short-
hydrofluoric acid. Then the solution was transferred into lived progeny to be in radioactive equilibrium when
a 50 ml volumetric flask made of polyethylene. The measured.
bomb was rinsed and filled up with 6% by weight boric The samples were counted, using a HPGe well type
acid solution. The ICP multielement standard solutions detector, with a well-volume of 5 cm 3, while the spectra
were also diluted with 6% by weight boric acid solution were analyzed using the Sampo-90 program.
for the measurement of these samples.
(3) Dissolution in water. 0.500 g of powdered sample Table 2. Operating conditions
was transferred into a glass beaker and 10 cm 3 deionised
Instrument Plasma lab. ICP spectrometer
water was added. The solution was heated at 95 ~ for
30 minutes using an electrical heating block. The Plasma (At-At) 27.12 MHz
Power 1.3 kW
solution was filtered into a 25 cm 3 volumetric flask. The Outer argon 10 I/min
residue was washed by deionised water. The filtered Intermediate argon 1.2 I/rain
solution was acidified by 3 cm 3 of high purity HNO 3 Inner argon 0.8 I/min
Observation height 13 mm
(70 m/v%) and the volume was set. For nebulisation the Sample flow rate 3 ml/min
same conditions were used. Integration time 5 s
Sample introduction by Gilson Minipuls pump
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