• Journal of The Korean Society of Grassland and Forage Science
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• v.27 no.3
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• pp.167-172
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• 2007

Manure recycle is an emerging issue in agriculture in Korea these days. Farmers are keeping eye on legume mixture with grasses for nitrogen fixation and transfer to companion crops by legumes. We had a trial to investigate the effect of different legume mixtures on nitrogen fixation and transfer in spring soil. The treatment was arranged in a randomized complete block design with three replications. Three different mixtures were used(rye+hairy vetch, Italian ryegrass+crimson clover, oat+pea) and sowed in pots with paddy soil from western part of Korea(Seo Chon County). Pots with rye+vetch were transplanted from field of RDA(rural development administration) in Suwon on 2 February 2007 and other mixture treatments were sowed on early March with different sowing rate(7:3=Italian:crimson, 6:4=oat:pea). $(^{15}NH_4)_2SO_4$ solution at. $99.8\;atom%^{15}N$ was applied to the each pot at the rate of $2kg\;N\;ha^{-1}$. Application was done on 6 April at rye+vetch pots and remainder were applied on April 16. Forage were harvested from each pot at ground level in heading stage and separated into legume and grass. Total N content and $^{15}N$ value were determined using a continuous flow stable isotope ratio mass spectrometry. DM yield of rye+vetch, Italian+crimson and oat+pea were 6,607, 3,213 and 4,312 kg/ha, respectively. Proportion of N from fixation was 0.73(rye+vetch), 0.42(Italian+crimson) and 0.93(oat+pea). The percentages of N transfer from legume to grass were from 61% to 24% in different method by treatment and -35% to 21% in isotope dilution method.

• Nuclear Engineering and Technology
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• v.21 no.4
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• pp.277-286
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• 1989

Destructive methods are used for the turnup determination of an irradiated PWR fuel. One of the methods includes U, Pu, Nd-148 and Nd-(145+146) determination by an isotope dilution mass spectrometry using triple spikes (U-233, Pu-242 and Nd-150). The method involves two sequential ion exchange resin separation procedures. Pu is eluted from the first anion exchange resin column (Dowex AG 1$\times$8) with 12 M HCl-0.1 M HI mixed solution, followed by U elution with 0.1 M HCl. Nd is isolated from other fission products on the second anion exchange resin column (Dowex AG 1$\times$4) with a nitric acid-methanol eluent. Each fraction is analysed by thermal ionization mass spectrometry. The difference between Nd-148 and Nd-(145+146) method is found with an average 2.07%. The results are compared with those by the heavy element method using U and Pu isotopes and by the destructive y-spectrometric measurement of Cs-137. The dependences of isotope composition of U and Pu on burn-up, and correlation between those isotopes are illustrated graphically.

• Analytical Science and Technology
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• v.15 no.5
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• pp.417-426
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• 2002

Inductively Coupled Plasma Dynamic Reaction Cell Quadrupole Mass Spectrometry (ICP-DRC-QMS) was characterized for the detection of the six naturally occurring calcium isotopes. The effect of the operating conditions of the DRC system was studied to get the best signal-to-noise ratio. This experiment shows that the potentially interfering ions such as $Ar^+$, ${CO_2}^+$, ${NO_2}^+$, $CNO^+$ at the calcium masses m/z 40, 42, 43, 44 and 48 were removed by flowing $NH_3$ gas at the rate of 0.7 mL/min $NH_3$ as reactive cell gas in the DRC with a RPq value (rejection parameter) of 0.6. The limits of detection for $^{40}Ca$, $^{42}Ca$, $^{43}Ca$, $^{44}Ca$, and $^{48}Ca$ were 1, 29, 169, 34, and 15 pg/mL, respectively. This method was applied to the determination of calcium in synthetic food digest samples (CCQM-P13) provided by LGC for international comparison. The isotope dilution method was used for the determination of calcium in the samples. The uncertainty evaluation was performed according to the ISO/GUM and EURACHEM guidelines. The determined mean concentration and its expanded uncertainty of calcium was ($66.4{\pm}1.2$) mg/kg. In order to assess our method, two reference samples, Riverine Water reference sample (NRCC SLRS-3) and Trace Elements in Water reference sample (NIST SRM 1643d), were analyzed.

• The Korean Journal of Zoology
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• v.3 no.1
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• pp.24-30
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• 1960

본실험의 목적은 탄산기에 방사성동위원소 C14를 표식한 sodium acetate ($CH_3$C14 OONA)를 사용하여 염소의 위내에 존재하는 acetate 의 위벽으로부터의 흡수율과 위의 acetate의 평균함량을 측정하는데 있다. C14 로 표식된 sodium acetate(specific activity 1.35$\times$108 cpm./g.)를 급사 3 시간후의 염소의 위내에 주입하고 주입 2분후부터 약 2분간격으로 위 내용물을 추울하여 column chromatograpy를 이용하여 acetate를 분리정량한 후 그의 specific activity를 측정하였다. 주입후 3 분경까지는 위내에 존재하는 acetate에 의한 표식 acetate의 희석으로 말미암아 specific activity 는 급격히 감소되어 갔고 3 분후부터는 감소도가 비교적 완만하였으나 역시 계속적으로 감소되어갔다. 희석완료후의 이 specific activity 감소는 위벽을 통한 acetate를 흡수와 위 내용물로부터의 acetate 생성으로 인한 것으로서, 이 감소율로부터 acetate의 위벽흡수속도를 추정할 수 있다. 상기 specific activity의 감소 graph 로부터 추정된 위내 acetate의 량은 본실험의 제조건하에서 약 30 g이었으며 위내 acetate 의 specific activity가 1/2 로 감소되는데 요하는 평균 시간은 약 4 분이었다. 이는 위내에 존재하는 acetate량의 약 절반은 4 분동안에 위벽을 통과함을 의미한다.

• Mass Spectrometry Letters
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• v.11 no.4
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• pp.108-112
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• 2020

A certified reference material (CRM) for the analysis of nutrient elements in an edible mushroom (Ganoderma lyceum) powder has been developed (KRISS CRM 108-10-011). The mass fractions of calcium (Ca), iron (Fe), and zinc (Zn) were measured by isotope dilution inductively coupled plasma mass spectrometry (ID ICP/MS). To dissolve the fungi cell wall of mushroom consisted of chitin fibers, sample preparation method by single reaction chamber type microwave-assisted acid digestion with acid mixtures was optimized. The mean measurement results obtained from 12 sample bottles were used to assign as the certified values for the CRM and the between-bottle homogeneities were evaluated from the relative standard deviations. The certified values were metrologically traceable to the definition of the kilogram in the International System of Units (SI). This CRM is expected to be used for validation of analytical methods or quality control of measurement results in analytical laboratories when they determine the mass fractions of elements in mushroom or other similar samples.

• Toxicological Research
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• v.31 no.3
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• pp.255-264
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• 2015

Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, $A{\alpha}C$, $MeA{\alpha}C$, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including $IQ-d_3$, $MeIQx-d_3$, $PhIP-d_3$, $Trp-P-2-^{13}C_2-^{15}N$ and $MeA{\alpha}C-d_3$ was spiked for quantification of HCAs and $^{13}C_3$-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.

• Analytical Science and Technology
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• v.21 no.5
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• pp.364-374
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• 2008

Antarctic Environmental Monitoring Handbook' was published by COMNAP/SCAR in 2000. The standardized method described in this handbook is recommended for monitoring of antarctic environment. High pressure bomb technique in this guide was used to decompose soil samples. In compliance with this guide book, high pressure bomb technique was applied to decompose the antarctic soil sampled at the King Sejong Station. An Isotope Dilution-Inductively Coupled Plasma-Mass Spectrometry (ID-ICP-MS) was applied to determine mass concentrations of Pb, Cu and Zn in the soil. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of NIST 2702 (marine sediment). The analytical results agreed with certified value within the range from 99.5~100.8%. Matrix separation was necessitated for the determination of Cu and Zn by Chelex 100 ion exchange resin. As a result, the average mass concentrations of Pb, Cu and Zn which are suspected to be caused by anthropogenic pollution were 332.9 mg/kg, 95.6 mg/kg and 115.3 mg/kg, respectively. Those for the metals sampled in the soils of the remote regions from the station were 28.1 mg/kg, 101.8 mg/kg and 115.6 mg/kg, respectively.

• Nuclear Engineering and Technology
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• v.25 no.2
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• pp.259-264
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• 1993

Ion chromatographic method has been applied for burnup measurement of irradiated nuclear fuel by dynamic system using 1-octanesulfonate as a cation exchanger and $\alpha$-hydroxyisobutyric acid as an eluant. A number of elution techniques were evaluated for the optimum separation of plutonium, uranium and neodymium. These elements were individually separated and collected by gradient elution between 0.05 M and 0.40 M of $\alpha$-hydroxyisobutyric acid in a single column, and finally determined by isotope dilution mass spectrometry. The burnup data from this method were compared with those from conventional anion exchange method. The results showed a good agreement within 3.5 % of difference between two methods.

• Journal of The Korean Society of Grassland and Forage Science
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• v.25 no.1
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• pp.1-6
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• 2005

With recent interest organic farming the use of legumes including vetch and clover to provide N to adjacent crops is increasing in Korea. In the present studies, we conducted a trial to investigate the effects of the application of N rate on nitrogen fixation and transfer from vetch to barley in mixed stands. The experiment was arranged in a randomized complete block design with three replications. Four different N rates(0, 75, 113 and 150/ha) was used and vetch+barley was broadcasted manually on 1.5 $\times$2 m plot in Oct. 2001. Half of urea and K$_{2}O, 200 Phosphate and 75 kg potash per ha were applied as basal dressing md half of N md 75 potash were used for topdressing to soil surface on MarctL 2002. The equivalent of 1kg ha$^{-1}$ at($^{15}$NH$_{4}$)$_{2}$SO$_{4}$ solution at 99.8 atom $\%$$^{15}$N excess was applied to the microplot in mid April. Forage was harvested from each plot at ground level and separated into barley and vetch. Total N content and It values of samples were determined using a continuous flow stable isotope ratio mass spectrometry(IsoPrime-EA. Micromass, UK.). The percentage of legume H fixed from atmospheric N2 were 95.0, 93.8, 94.4 and $84.8\%$ with increment of N levels. The percentage of N transfer from vetch to barley by N-difference method with increment of N fertilizer were from 58 to$49\%$ while 39 to $23\%$ in $^{15}$N-dilution method. The amount of transfer from vetch to barley were 87 to 68 kg/ ha with N level by N-difference moth여 and 58 to -56/ha with N application levels by $^{15}$N dilution method. The amount of nitrogen fixation per ha were from 150 kg / ha to 219 kg / ha by different method, but on the other side 49 to 105kg/ha by N$^{15}$-dilution.

• Journal of the Korean Vacuum Society
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• v.11 no.4
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• pp.218-224
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• 2002

A domestic round robin test(RRT) for the quantitative analysis of minor impurities was performed by a standard procedure and standard reference material. The certified reference material(CRM)s for B-doped Si thin film and analysis specimens and the analysis specimens were prepared by an ion beam sputter deposition method. These samples were certified by inductively coupled plasma mass spectrometry(ICP-MS) with isotope dilution method which il one of the most quantitative methods in chemical analysis. By using an international standard procedure(ISO/DIS-l4237) for the quantitative analysis of B in Si by SIMS, a domestic RRT was performed for these specimens. Although only a few laboratories participated in this RRT, the average B concentration well agreed with the certified value within 2% error.