• Title/Summary/Keyword: Error Calibration

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Quantifying Uncertainty of Calcium Determination in Infant Formula by AAS and ICP-AES (AAS 및 ICP-AES에 의한 조제분유 중 칼슘 함량 분석의 측정불확도 산정)

  • Jun, Jang-Young;Kwak, Byung-Man;Ahn, Jang-Hyuk;Kong, Un-Young
    • Korean Journal of Food Science and Technology
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    • v.36 no.5
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    • pp.701-710
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    • 2004
  • Uncertainty was quantified to evaluate calcium determination result in infant formula with AAS (Atomic Absorption Spectrometry) and ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry). Uncertainty sources in measurand, such as sample weight, final volume of sample, sample dilution and the instrumental result were identified and used as parameters for combined standard uncertainty based on the GUM (Guide to the expression of uncertainty in measurement) and Draft EURACHEM/CITAC Guide. Uncertainty components of each sources in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, standard material molecular weight, standard solution concentration, standard solution dilution factor, sample dilution factor, calibration curve, recovery, instrumental precision, reproducibility, and stability, Each uncertainty components were evaluated by uncertainty types and included to calculate combined uncertainty. The kinds of uncertainty sources and components in the analytical method by AAS and ICP-AES were same except sample dilution factor for AAS. The analytical results and combined standard uncertainties of calcium content were estimated within the certification range $(367{\pm}20\;mg/100g)$ of CRM (Certified Reference Material) and were not significantly different between method by AAS followed by ashing and method by ICP-AES followed by acid digestion as $359.52{\pm}23.61\;mg/100g\;and\;354.75{\pm}16.16\;mg/100g$, respectively. Identifying uncertainty sources related with precision, repeatability, stability, and maintaining proper instrumental conditions as well as personal proficiency was needed to reduce analytical error.

A comparison study of 76Se, 77Se and 78Se isotope spikes in isotope dilution method for Se (셀레늄의 동위원소 희석분석법에서 첨가 스파이크 동위원소 76Se, 77Se 및 78Se들의 비교분석)

  • Kim, Leewon;Lee, Seoyoung;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.170-178
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    • 2016
  • Accuracy and precision of ID methods for different spike isotopes of 76Se, 77Se, and 78Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and 78Se showed was a bit better than 76Se and 77Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for 78Se, 76Se and 77Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of 78Se isotope spike (over 100 % RSD). 76Se and 77Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, 78Se should be avoided when large amount of Br exists in matrix. Either 76Se or 77Se would provide accurate results.

Mathematical Transformation Influencing Accuracy of Near Infrared Spectroscopy (NIRS) Calibrations for the Prediction of Chemical Composition and Fermentation Parameters in Corn Silage (수 처리 방법이 근적외선분광법을 이용한 옥수수 사일리지의 화학적 조성분 및 발효품질의 예측 정확성에 미치는 영향)

  • Park, Hyung-Soo;Kim, Ji-Hye;Choi, Ki-Choon;Kim, Hyeon-Seop
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.36 no.1
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    • pp.50-57
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    • 2016
  • This study was conducted to determine the effect of mathematical transformation on near infrared spectroscopy (NIRS) calibrations for the prediction of chemical composition and fermentation parameters in corn silage. Corn silage samples (n=407) were collected from cattle farms and feed companies in Korea between 2014 and 2015. Samples of silage were scanned at 1 nm intervals over the wavelength range of 680~2,500 nm. The optical data were recorded as log 1/Reflectance (log 1/R) and scanned in intact fresh condition. The spectral data were regressed against a range of chemical parameters using partial least squares (PLS) multivariate analysis in conjunction with several spectral math treatments to reduce the effect of extraneous noise. The optimum calibrations were selected based on the highest coefficients of determination in cross validation ($R^2{_{cv}}$) and the lowest standard error of cross validation (SECV). Results of this study revealed that the NIRS method could be used to predict chemical constituents accurately (correlation coefficient of cross validation, $R^2{_{cv}}$, ranging from 0.77 to 0.91). The best mathematical treatment for moisture and crude protein (CP) was first-order derivatives (1, 16, 16, and 1, 4, 4), whereas the best mathematical treatment for neutral detergent fiber (NDF) and acid detergent fiber (ADF) was 2, 16, 16. The calibration models for fermentation parameters had lower predictive accuracy than chemical constituents. However, pH and lactic acids were predicted with considerable accuracy ($R^2{_{cv}}$ 0.74 to 0.77). The best mathematical treatment for them was 1, 8, 8 and 2, 16, 16, respectively. Results of this experiment demonstrate that it is possible to use NIRS method to predict the chemical composition and fermentation quality of fresh corn silages as a routine analysis method for feeding value evaluation to give advice to farmers.

Development of Continuous Monitoring Method of Root-zone Electrical Conductivity using FDR Sensor in Greenhouse Hydroponics Cultivation (시설 수경재배에서 FDR 센서를 활용한 근권 내 농도의 연속적 모니터링 방법)

  • Lee, Jae Seong;Shin, Jong Hwa
    • Journal of Bio-Environment Control
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    • v.31 no.4
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    • pp.409-415
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    • 2022
  • Plant growth and development are also affected by root-zone environment. Therefore, it is important to consider the variables of the root-zone environment when establishing an irrigation strategy. The purpose of this study is to analyze the relationship between the volumetric moisture content (VWC), Bulk EC (ECb), and Pore EC (ECp) used by plant roots using FDR sensors in two types of rockwool media with different water transmission characteristics, using the method above this was used to establish a method for collecting and correcting available root-zone environmental data. For the experiment, two types of rockwool medium (RW1, RW2) with different physical characteristics were used. The moisture content (MC) and ECb were measured using an FDR sensor, ECp was measured after extracting the residual nutrient solution from the medium using a disposable syringe in the center of the medium at a volumetric moisture content (VWC) of 10-100%. Then, ECb and ECp are measured by supplying nutrient solution having different concentration (distilled water, 0.5-5.0) to two types of media (RW1, RW2) in each volume water content range (0 to 100%). The relationship between ECb and ECp in RW1 and RW2 media is best suited for cubic polynomial. The relationship between ECb and ECp according to volume moisture content (VWC) range showed a large error rate in the low volume moisture content (VWC) range of 10-60%. The correlation between the sensor measured value (ECb) and the ECp used by plant roots according to the volumetric water content (VWC) range was the most suitable for the Paraboloid equation in both media (RW1, RW2). The coefficient of determination the calibration equation for RW1 and RW2 media were 0.936, 0.947, respectively.