• Mass Spectrometry Letters
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• v.5 no.2
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• pp.57-61
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• 2014

A gravimetric standard addition method combined with internal standard calibration has been successfully developed for the accurate analysis of total arsenic in a laver candidate reference material. A model equation for the gravimetric standard addition approach using an internal standard was derived to determine arsenic content in samples. Handlings of samples, As standard and internal standard were carried out gravimetrically to avoid larger uncertainty and variability involved in the volumetric preparation. Germanium was selected as the internal standard because of its close mass to the arsenic to minimize mass-dependent bias in mass spectrometer. The ion signal ratios of $^{75}As^+$ to $^{72}Ge^+$ (or $^{73}Ge^+$) were measured in high resolution mode ($R{\geq}10,000$) to separate potential isobaric interferences by high resolution ICP/MS. For method validation, the developed method was applied to the analysis of arsenic content in the NMIJ 7402-a codfish certified reference material (CRM) and the result was $37.07mg{\cdot}kg^{-1}{\pm}0.45mg{\cdot}kg^{-1}$ which is in good agreement with the certified value, $36.7mg{\cdot}kg^{-1}{\pm}1.8mg{\cdot}kg^{-1}$. Finally, the certified value of the total arsenic in the candidate laver CRM was determined to be $47.15mg{\cdot}kg^{-1}{\pm}1.32mg{\cdot}kg^{-1}$ (k = 2.8 for 95% confidence level) which is an excellent result for arsenic measurement with only 2.8 % of relative expanded uncertainty.

• Mass Spectrometry Letters
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• v.4 no.4
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• pp.75-78
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• 2013

A gas chromatography/mass spectrometric (GC/MS) method was developed as a candidate reference method for the accurate determination of essential fatty acids (linoleic acid, ${\alpha}$- and ${\gamma}$-linolenic acids) in food supplemental oil products. Samples were spiked with three internal standards (stearic acid-$d_{35}$, $^{13}C_{18}$-linoleic acid, and $^{13}C_{18}$-${\alpha}$-linolenic acid). Samples were then subject to saponification, derivatization for methylation, and extraction by organic solvent. For GC/MS measurement, an Agilent HP-88 column, designed for the separation of fatty acid methyl esters, was selected after comparing with other columns as it provided better separation for target analytes. Target analytes and internal standards were detected by selected ion monitoring of molecular ions of their methyl ester forms. The GC/MS method was applied for the measurement of three botanical oils in NIST SRM 3274 (borage oil, evening primrose oil, and flax oil), and measurement results agreed with the certified values. Measurement results for target analytes which have corresponding isotope-labeled analogues as internal standard were calculated based on isotope dilution mass spectrometry (IDMS) approach, and compared with results calculated by using the other two internal standards. Results from the IDMS approach and the typical internal standard approach were in good agreement within their measurement uncertainties. It proves that the developed GC/MS method can provide similar metrological quality with IDMS methods for the measurement of fatty acids in natural oil samples if a proper fatty acid is used as an internal standard.

• Nuclear Engineering and Technology
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• v.48 no.2
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• pp.299-303
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• 2016

Prompt gamma activation analysis using a thermal neutron-guided beam at Japan Atomic Energy Agency JRR-3M was applied for the precise determination of Si in silicon nitride ceramic reference materials [Japan Ceramic Reference Material (JCRM) R 003]. In this study, the standard addition method coupled with internal standard was used for the nondestructive determination of Si in the sample. Cadmium was used as internal standard to obtain the linear calibration curves and to compensate for the neutron beam variability. The analytical result of determining Si in JCRM R 003 silicon nitride fine powder ceramic reference materials using prompt gamma activation analysis was in good agreement with that obtained by classical gravimetric analysis. The relative expanded measurement uncertainty (k = 2) associated with the determined value was 2.4%.

• Applied Microscopy
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• v.29 no.1
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• pp.75-81
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• 1999

Optimum conditions for making the Au and Al internal standards for TEM have been determined experimentally. The Au internal standard was produced by sputter coating at 9mA for 100 seconds in low vacuum $(\leq1\times10^{-3})$. The Al internal standard was produced by evaporation coating at 7kV for 10 minutes in high vacuum $(\leq1\times10^{-5})$. Measurements of the lattice parameters of andalusite and albite feldspars with this Au internal standard resulted in errors of (a) $ \leq1.2%$ in precion and $\leq0.3%$ in accuracy for andalusite: (b) $\leq0.5%$ in precision and $\leq1.1%$ in accuracy for albite feldspars. The most significant error occurred from the measuring processes of distances and angles of electron diffraction patterns. By employing systematic procedures of measurement with high precision devices, this lattice parameter determination method utilizing the internal standard should be a good alternative to the conventional powder XRD method or the sophisticated CBED method for special samples.

• The Journal of Korean Academic Society of Nursing Education
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• v.23 no.4
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• pp.378-388
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• 2017

Purpose: The aim of this study was to identify the status of performance on standard precautions among nursing students and to examine the mediating effects of internal health locus of control on the relationship between awareness and performance on standard precautions of hospital-acquired infection control. Methods: The participants in this study were 134 nursing students. The measurements included a standard precautions awareness and performance scale, and a multidimensional health locus of control scale. Data were analyzed using independent t-test, one-way ANOVA, $Scheff{\acute{e}}$ test, Pearson correlation coefficient, and simple and multiple regression techniques. Mediation analysis was performed by the Baron and Kenny's method and Sobel test. Results: The mean score of standard awareness, standard performance, and internal health locus of control about standard precaution were $174.30{\pm}9.08$; $169.48{\pm}12.04$; and $20.43{\pm}2.82$; respectively. There was a positive correlation between standard awareness and performance (r=.414, p<.001). Also, standard awareness was significantly correlated with internal health locus of control (r=.413, p=.014). Internal health locus of control showed partial mediating effects in the relationship between awareness and performance. Conclusion: The results indicate a need to improve the internal health locus of control of nursing students. Therefore, an internal health locus of control improvement program should improve performance on standard precautions for patients and themselves.

• BMB Reports
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• v.29 no.5
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• pp.481-483
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• 1996

In competitive PCR, which is used to quantify target DNA an internal standard is needed. Here we present a simple method to construct homologous competitive standards. The method, which is based upon deletion of a portion of the target DNA, does not require any additional primers. This is the simplest method developed thus far to construct a competitive standard. The whole procedure. from construction of a competitive standard to quantitation by PCR, can be completed within a single day.

• Mass Spectrometry Letters
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• v.9 no.3
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• pp.77-80
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• 2018

The focus of this paper is to present techniques to overcome certain difficulties in quantitative analysis with a time-of-flight mass spectrometer (TOF-MS). The method is based on conventional solid-phase extraction, followed by reversed-phase ultra high performance liquid chromatography of the extract, and mass spectrometric analysis. The target compounds included atenolol, atrazine, caffeine, carbamazepine, diclofenac, estrone, ibuprofen, naproxen, simazine, sucralose, sulfamethoxazole, and triclosan. The matrix effects caused by high concentrations of organic compounds in wastewater are especially significant in electrospray ionization mass spectroscopy. Internal-standard calibration with isotopically labeled standards corrects the results for many matrix effects, but some peculiarities were observed. The problems encountered in quantitation of carbamazepine and triclosan, due to nonlinear calibration were solved by changing the internal standard and using a narrower mass window. With simazine, the use of a quadratic calibration curve was the best solution.

• Analytical Science and Technology
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• v.23 no.1
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• pp.24-35
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• 2010

To learn more about the calibration properties of reduced sulfur compounds (RSCs) by the combination of gas chromatography(GC)-pulsed flame photometric detector (PFPD) and thermal desorption method, a series of calibration experiments were conducted on the basis of both internal and external calibration approaches. For these experiments, gaseous standards of 4 RSCs ($H_2S$, $CH_3SH$, DMS, and DMDS) were prepared at two different concentration levels of both low (10, 20, 50,and 100 ppb) and high ranges (100, 200, 500, and 1000 ppb) along with $CS_2$ as an internal standard. First, the external calibration results were compared between fixed standard volume (FSV) and fixed standard concentration (FSC) method. Secondly, FSV-based calibration results were compared between external and internal calibration results. As FSV method suffers from sensitivity variations less significantly than FSC, the former is recommended to maintain the consistency in GC-TD sensitivity for RSC analysis. In addition, when the calibration data were examined in terms of RSE between external and internal calibration data, the results were not consistent enough to show improvements in internal method. Hence, diverse efforts are desirable to optimize the reproducibility in terms of GC-TD sensitivity for RSC analysis.

• Journal of Physiology & Pathology in Korean Medicine
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• v.26 no.3
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• pp.367-375
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• 2012

The goal of current study is to make a standard pattern identification for post stroke depression using a delphi method. Finally, ten experts of oriental medicine, especially of stroke or depression, participated in Dephi examination. At the first meeting, experts conducted free discussion and determined to use the previous published questionnaires of Deficiency-Excess identification and Cold-Heat identification. From the second round, experts participated in evaluating and correcting the questionnaire by email. New seven questions were added to the questionnaire of Deficiency-Excess identification through the second round. Finally, the standard pattern identification of Cold-Heat or Deficiency-Excess is composed 20 questions and 11 questions, respectively. These pattern identifications for post stroke depression will contribute to research and treatment of oriental medicine.

• Korean Journal of Food Science and Technology
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• v.43 no.5
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• pp.532-536
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• 2011

The internal standard method using ion chromatography combined with tandem mass spectrometry (IC-MS/MS) for quantifying perchlorate in different types of food was established. Because the presence of ions and other biomolecules in matrices usually interrupts accurate determination of perchlorate, it is necessary to develop efficient, reproducible method to determine perchlorate concentrations in food. In this study, the internal standard method was compared with the external standard method to determine perchlorate concentrations in standard samples. The obtained method detection limit (MDL) for perchlorate was 0.005 ${\mu}g/L$ for bottled water, 0.12 ${\mu}g/L$ for milk, 0.27 ${\mu}g/kg$ for rice, 0.16 ${\mu}g/kg$ for vegetables, and 0.07 ${\mu}g/kg$ for seaweed, respectively. The limit of quantitation (LOQ) was calculated by multiplying the MDL by 7. The recoveries of perchlorate from food samples spiked with perchlorate ranged from 98 to 105% and their percent relative standard deviation (%RSD) levels were <20%. This method was successfully applied for the quantitative determination of perchlorate in various kinds of food.