• Analytical Science and Technology
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• v.13 no.3
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• pp.297-303
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• 2000

Isotope-dilution inductively coupled plasma mass spectrometry was used to determine trace amounts of Cd, Cu, Pb, Ni and Zn in sediment. Sediment samples were dissolved by microwave digestion with addition of mixed acid ($HNO_3$, HF and $HClO_4$). Lead was determined after separation of alkaline and alkaline earth metals by an ammonium pyrrolidenedithiocarbarmate (APDC) solvent extraction. The other elements were determined after separation of iron, tin and titanium by hydroxide precipitation. Recovery efficiency of the analyte elements was not satisfactory, but most of matrix elements causing the isobaric interference could be effectively eliminated by the separation. Good agreement was achieved with the certified values in the analysis of the two sediment reference materials.

• Journal of Sensor Science and Technology
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• v.22 no.6
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• pp.404-409
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• 2013

We devised calibration procedure for industrial thermometers by a comparison method at the boiling point of nitrogen (${\sim}-196^{\circ}C$). The uncertainty of the calibration was 4 mK (k = 2). As experimentally demonstrated in this work, the effect of the atmospheric pressure on the boiling point of nitrogen can be easily detected by the thermometer. Therefore, when the boiling point of nitrogen is used for calibration of thermometer by comparison, either a reference thermometer must be used to provide the reference temperature or the effect of atmospheric pressure should be carefully considered. The use of a copper block with a large thermal mass soaked into the liquid nitrogen was proven to be more reliable, and the stability of the temperature immersed into the copper block was 1.4 mK. The temperatures at the thermometer wells, evaluated by the crossed-measurement method to compensate for the inaccuracy of the thermometers and the linear drift of the temperature of the copper block, were equivalent within 0.23 mK of standard uncertainty.

• Analytical Science and Technology
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• v.22 no.4
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• pp.302-306
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• 2009

A trace amount of boron in steel significantly influences its mechanical and physical properties. A prompt gamma ray activation analysis (PGAA) method is used to measure boron in low alloy steel samples of KRISS 101-01-C21~C26. NIST SRMs of 362, 364, 1761 and 1767 serve as the control standards to validate the measurement method. The measured values of the NIST SRMs are consistent with their certified values within the expected uncertainties, except for that of NIST SRM 362. Experimental uncertainties are evaluated according to the guidelines given by the International Organization for Standardization (ISO). The expanded uncertainties are calculated with a coverage factor of 2, at approximately 95% confidence level. The calculated relative expanded uncertainties of boron mass fractions are between 3% and 7% at the mg/kg level. The results are compared with the results measured by the solvent extraction-inductively coupled optical emission spectrometry (ICP/OES) method.

• Analytical Science and Technology
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• v.23 no.5
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• pp.485-491
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• 2010

A certified reference material (CRM) of KRISS 109-03-SSD was developed for the analysis of hazardous elements in soil. The target elements were As, Cd, Cr, Cu, Hg, Ni, Pb, Zn being regulated by the Soil Environment Conservation Act. Starting material was collected from tailing dump of an unworked tungsten mine at Sangdong (Gangwon-do, Korea). The starting material under-went through a series of fabricating process steps of screening, drying, grinding, sieving, blending, bottling, sterilization and was certified according to the ISO Guide 35. Isotope dilution-inductively coupled mass spectrometry (ID-ICP/MS) and instrumental neutron activation analysis (INAA) were used for the measurement. Homogeneity was tested according to ISO 13528 annex B. The certified values were determined using the results from two different methods or from two independent measurements using a method. Finally, certified values of seven elements of arsenic, cadmium, chromium, copper, lead, nickel and zinc were determined. Mercury did not satisfied the criteria of homogeneity and the result would be provided for information only, together with iron and tungsten. It was also studied, the extractable fraction of elements by aqua regia according to the ISO 11466 protocol being frequently studied for the purpose of environmental monitoring. It was performed as a inter-laboratory study by 6 laboratories of a public institute and universities. Standard deviation among the laboratories was much bigger than the uncertainty of the certified value. The result of inter-laboratory study on the extractable fraction will be provided for information, only.

• Bulletin of the Korean Chemical Society
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• v.26 no.5
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• pp.740-746
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• 2005

In this article, we report the tandem mass spectrometry investigations for the electron capture efficiencies of the protons belonging to the different locations (generations) in a poly(propylene imine) dendrimer with three layers of a repeat unit (named as the third generation dendrimer). The employed tandem mass spectrometry methods include SORI-CAD (sustained off-resonance irradiation collisional activation dissociation) and ECD(electron capture dissociation) mass spectrometry. We obtained SORI-CAD spectra for the dendrimer ions in the different charge states, ranging from 2+ to 4+. The analysis of fragmentation sites provides the information as to where the protons are distributed among various generations of the dendrimer. Based upon this, a new strategy to study the electron capture efficiencies of the protons is utilized to examine a new type of triplycharged ions by SORI-CAD, i.e., the 3+ ions generated from the charge reduction of the native 4+ ions by ECD: (M+4H)$^{4+}\;+\;e^-\;{\rightarrow}$ (M+4H)$^{3+\bullet}$ ${\rightarrow}\;({H^{\bullet}}_{ejected}$) + (M+3H)$^{3+}\;\rightarrow$ CAD. Interestingly, comparison of these four SORICAD spectra indicates that the proton distribution in the charge-reduced 3+ ions is very close to that in the native 4+ ions. It further suggests that in this synthetic polymer ($\sim$1.7 kDa) with an artificial architecture, the electron capture efficiencies of the protons are actually insensitive to where they are located in the molecule. This is somewhat contradictory to common expectations that the protons in the inner generations may not be well exposed to the incoming electron irradiation as much as the outer ones are, thus may be less efficient for electron capture. This finding may carry some implications for the case of medium sized peptide ions with similar masses, which are known to show no obvious site-specific fragmentations in ECD MS.

• Journal of Environmental Impact Assessment
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• v.21 no.5
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• pp.725-734
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• 2012

The outbreak of foot and mouth disease in November 2010 raised many social, economic and environmental issues and water contaminations by leachate from carcass disposal sites particularly emerged as a serious concern. In oder to efficiently handle these problems, a critical method is required to transport leachate to livestock manure and sewage treatment plants and purify it. This study aims to present the best applicable method to transport leachate from carcass disposal sites into livestock manure and sewage treatment facilities. We investigated the biological and chemical characteristics such as BOD, COD, SS, TN, TP and Total coliforms. Current conjugated treatments in livestock manure and sewage treatment plants was studied by surveying the operations of those facilities. The NIER-MASS(National Institute of Environmental Research - Mass Balance Evaluation System of Sewage Treatment Facilities) program was applied to present the best conjugated treatment method through estimating the maximum daily load to meet the water quality standards in effluent.

• Bulletin of the Korean Chemical Society
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• v.35 no.11
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• pp.3275-3279
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• 2014

A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.

• Journal of Sensor Science and Technology
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• v.12 no.6
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• pp.258-264
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• 2003

The present paper studies how to calibrate hydrometer using image process. The method aligns particular scales of hydrometer selected for calibrating the hydrometer with the horizontal plane of the reference liquid automatically without man's operation. Major parts composing the system are CCD camera, frame grabber, stepping motor and image process program. The image process program is composed of a part that locates the meniscus and aligns it with a scale and a part that controls the step motor. To verify the performance of the developed method, this study compares the meniscus and scale observed directly with the naked eye with the result of calibration by the manual calibration method. The differences between the corrections were less than $0.004\;kg/m^3$ with uncertainty of $0.06\;kg/m^3$. These showed that the calibration results of the developed hydrometer calibration using image process nearly equal to manual method.

• Bulletin of the Korean Chemical Society
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• v.28 no.5
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• pp.737-744
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• 2007

An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.

• Asian Journal of Atmospheric Environment
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• v.2 no.2
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• pp.90-101
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• 2008

The chemical compositions of $PM_{2.5}$ and $PM_{10}$ and associated high-molecular-weight polycyclic aromatic hydrocarbons (PAHs) were investigated during winter and summer at a roadside and an urban background site in Saitama, Japan. The average concentrations of $PM_{2.5}$ exceeded the United States Environmental Protection Agency standards during both periods. Carbonaceous components were abundant in both the observed and calculated (by means of a mass closure model) chemical composition of $PM_{2.5}$. Traffic-related pollutants (elemental carbon and high-molecular-weight PAHs) were strongly associated with $PM_{2.5}$ rather than with larger particles. The mass concentrations of $PM_{2.5}$, as well as those of EC and PAHs associated with the particles, at the two sites were strongly correlated. Comparison of our data with source profile ratios indicates that diesel-powered vehicles were probably the main source of the measured PAHs. The PAHs concentrations were affected by meteorological conditions during our study. Our results highlight the need for the establishment of standards for $PM_{2.5}$ in Japan.