Residual solvents in foods are defined as organic volatile chemicals used or produced in manufacturing of extracts or additives, or functional foods. The solvents are not completely eliminated by practical manufacturing techniques and they also may become contaminated by solvents from packing, transportation or storage in warehouses. Because residual solvents have no nutritional value but may be hazardous to human health, there is a need to remove them from the final products or reduce their amounts to below acceptable levels. The purpose of this study was to develop and evaluate an analytical method for the screening of residual solvents in health functional foods. Furthermore, the aim of this study was to constitute a reasonable management system based on the current state of the market and case studies of foreign countries. Eleven volatile solvents such as MeOH, EtOH, trichloroethylene and hexane were separated depending on their column properties, temp. and time using Gas Chromatography (GC). After determining the GC conditions, a sample preparation method using HSS (Head Space Sampling) was developed. From the results, a method for analyzing residual solvents in health functional foods was developed considering matrix effect and interference from the sample obtained from the solution of solvents-free health functional foods spiked with 11 standards solutions. Validation test using the developed GC/HSS/MS (Mass Spectrometry) method was followed by tests for precision, accuracy, recovery, linearity and adequate sensitivity. Finally, examination of 104 samples grouped in suits was performed by the developed HSS/GC/MS for screening the solvents. The 11 solvents were isolated from health functional foods based on vapor pressure difference, and followed by separation within 15 minutes in a single run. The limt of detection (LOD), limit of quantification (LOQ), recovery and coefficient of variation (C.V.) of these compounds determined by the HSS/GC/MS were found to be 0.1 pg/mL, 0.1-125 pg/g, 51.0-104.6%, and less than 15%, respectively. Using the developed HSS/GC/MS method, residual solvent from 16 out of 104 health functional products were detected as a EtOH. This method therefore seems t o be a valuable extension ofanalytical method for the identification of residual solvents in health functional food.
Kim, Ji-Yong;Kim, Jung Ran;Cheong, Hae-Kwan;Lim, Hyun-Sul;Paik, Nam-Won
Journal of Korean Society of Occupational and Environmental Hygiene
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v.7
no.2
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pp.209-222
/
1997
Authors surveyed the ground water near the waste disposed from a fiberglass production factory to confirm the presence of glassfiber in the water and to determine the effect of sampling conditions and storage on the recovery of fibrous materials in the ground water. Sample was collected at every 4 hours for 48 hours consecutively. After finishing the 48 hours sample, water sampling was done from each tap after repeated turning on and off the water for 30 seconds at each time. Sample was collected in the two 1.5 liter polyethylene bottle after vigorously shaking the bottle with the same water several times with the flowing tap water. At each paired sample, one bottle was stored stand still at room temperature, and the other sample was filtered immediately after sampling. Water was filtered on the Mixed Cellulose Ester filter with negative pressure. Each sample was divided into upper and lower layer. The other bottle was stored at room temperature standstill for 7 days and filtered in the same fashion as the other pair of sample did. Each MCE filter was divided into 4 pieces and one piece was treated with acetone to make it transparent. Each prepared sample was observed by two researchers under the light and polarizing microscopy, scanning electron microscopy and energy dispersive X-ra microanalysis. Fibers were classified by the morphology and polarizing pattern under the polarizing microscope, and count was done. 1. There was a significant fluctuation in number of the fibers, but there was no specific demonstrable pattern. 2. Non-polarizing fibers frequently disappeared after 7 days's storage. But cluster of fibers were found at the wall of the same container by scratching technique. 3. Polarizing fibers were usually found in between the filter and the manicure pasted area. Possible explanations for this phenomenon will be that either these fibers are very light or have electronic polarity. Hence, these fibers are not able to be attached on the surface of slide glass. 4. Under the scanning electron microscopic examination, the fibers which are not refractive under the light microscopy were identified as glassfiber. Other fibers which is refractive under the polarizing microscopy were identified as magnesium silicate fibers. It is strongly suggested that development of standardized method of sample collection and measurement of fibrous material in the water is needed.
Journal of the Korean Society for Marine Environment & Energy
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v.8
no.4
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pp.213-219
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2005
In this study, we try to Quantitatively assess the micropollutants in Gwangyang bay, Gamag bay and Yeoa bay, using simultaneous analytical method fir 310 chemicals. In the results, several dozen organic pollutants were detected in sampling sites, and the major chemicals detected were CH type chemicals, such as aliphatic and polycyclic compounds, and CHN(O) type chemicals, such as aromatic ammines and nitro compounds. The concentration of organic pollutants was higher in summer than in winter. However, there was no association of species of organic pollutants with season. The total concentration of pesticides at each sampling site was measured within the range of $ND{\sim}9.11{\mu}g/L$. Insecticides and fungicides of pesticide type were detected in Gwangyang bay and Gamag bay, while six kinds of endocrine disrupter were detected in southern coastal waters. From the results of this study, we should estimated that the insecticides, the fungicides, and a few of the endocrine disrupters are major pollutant factors in southern coastal waters.
The article presents a theoretical-experimental approach developed for modeling the coefficient of sliding friction in the dynamic system tool-workpiece in slide diamond burnishing of low-alloy unhardened steels. The experimental setup, implemented on conventional lathe, includes a specially designed device, with a straight cantilever beam as body. The beam is simultaneously loaded by bending (from transverse slide friction force) and compression (from longitudinal burnishing force), which is a reason for geometrical nonlinearity. A method, based on the idea of separation of the variables (time and metric) before establishing the differential equation of motion, has been applied for dynamic modeling of the beam elastic curve. Between the longitudinal (burnishing force) and transverse (slide friction force) forces exists a correlation defined by Coulomb's law of sliding friction. On this basis, an analytical relationship between the beam deflection and the sought friction coefficient has been obtained. In order to measure the deflection of the beam, strain gauges connected in a "full bridge" type of circuit are used. A flexible adhesive is selected, which provides an opportunity for dynamic measurements through the constructed measuring system. The signal is proportional to the beam deflection and is fed to the analog input of USB DAQ board, from where the signal enters in a purposely created virtual instrument which is developed by means of Labview. The basic characteristic of the virtual instrument is the ability to record and visualize in a real time the measured deflection. The signal sampling frequency is chosen in accordance with Nyquist-Shannon sampling theorem. In order to obtain a regression model of the friction coefficient with the participation of the diamond burnishing process parameters, an experimental design with 55 experimental points is synthesized. A regression analysis and analysis of variance have been carried out. The influence of the factors on the friction coefficient is established using sections of the hyper-surface of the friction coefficient model with the hyper-planes.
Journal of Korean Society for Atmospheric Environment
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v.23
no.5
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pp.547-556
/
2007
The release, sampling and analytical methods have been developed and tested for perfluorocarbons (PFCs) atmospheric tracers in order to gain insight into the atmospheric transport and dispersion over the urban conditions of Seoul, Korea. Although PFCs tracer experiments provide unique opportunities to test local and urban scale of transport and dispersion, no previous experiment with PFCs has been conducted in Korea. PMCH and PDCH were chosen as targeted tracers in our study due to their extreme low ambient concentrations and great sensitivities among various PFCs. For PFCs release system, a set of micro-metering pump, electronic balance, vaporizing furnace and high speed blower was constructed for precise and accurate release of tracers. The precision of released rate by this system was estimated to be 1%. Samplings of PFCs were carried out by fabricated portable air samplers with micro pumps and rotameters into glass tubes packed with 150 mg of Carboxen-569. The uncertainty of these sampling system was maintained below 14%. PMCH and PDCH were quantified in GC/ECD with preconditioned injection system to eliminate the interference compounds using traps and subsequent catalytic conversion system prior to column separation. Three intensive field test were undertaken during the springtime of 2002 to 2004 in eastern part of Seoul. Daily background samples were collected to characterize the background levels of PMCH and PDCH prior to their release. The observed background concentrations of PMCH ranged from 3.5 to 10.1 fL/L and varied randomly in location and time in this study. Its mean and standard variation of background concentration ($6.8{\pm}1.9\;fL/L$) are higher than those ($3.2{\sim}5.8\;fL/L$) of other historic tracer studies. Identified uncertainty for background PMCH was $1.7{\sim}2.0\;fL/L$ using this analytical system. Combined relative uncertainty in determining the tracer's concentrations was estimated as 17%. However, its background concentrations and uncertainty in concentration determination were found to be low and stable enough for tracer study.
Kim, Jin-Young;Jeong, Jae-Chul;Suh, Sung-Ill;Suh, Yong-Jun;Lee, Jeong-Jik;Kim, Jong-Sang;In, Moon-Kyo
YAKHAK HOEJI
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v.52
no.6
/
pp.480-487
/
2008
We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH), the major metabolite of ${\Delta}^9$-tetrahydrocannabinol, in urine sample by solid-phase extraction (SPE) and GC/MS detection. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day and inter-person validation were performed using statistical analysis of several indicative factors. Measurement uncertainty associated with target analyte in real forensic samples was estimated using quality control (QC) data. Traceability of measurement was established through traceable standards, calibrated volumetric glassware and volume measuring device. The major factors of contribution to combined standard uncertainty, were calibration linearity, inter-day repeatability and inter-person reproducibility, while those associated with preparation of analytical standards and sampling volume were not so important considering the degree of contribution. Relative combined standard uncertainties associated with the described method was 12.05% for THCCOOH.
Kang, Sam Woo;Kim, In Yong;Han, Hong Seok;Lee, Seung Seok
Analytical Science and Technology
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v.6
no.1
/
pp.57-63
/
1993
Spectrophotometric determination of cobalt by flow injection method is described. 2-(5-Bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino) aniline rapidly forms a water-soluble complex with cobalt in $NH_3-NH_4Cl$ buffer solution at pH 10.5. The absorption maxima of this complex is at 545 nm with molar absorptivity of $58000L\;mol^{-1}\;cm^{-1}$. The calibration curve of cobalt is linear over the range of 0.1 to 0.6ppm and the detection limit is 25ppb. The relative standard deviation is ${\pm}0.72%$ for 0.5ppm and the sampling rate is $60samples\;hr^{-1}$. The interfering effect of some cations and anions was investigated. Ni(II), Cu(II), Fe(III) and $CN^-$ interfered severely. The interfering effect of these matallic ions could be decreased by adding $1.0{\times}10^{-3}M$ EDTA solution to the carrier stream.
Different isolation methods for the volatile components of Anise(Pimpinella anisum L.) are compared in terms of the difference of components obtained with each analytical procedure. These methods include headspace(purge & trap) sampling procedure, simultaneous distillation extraction(SDE), steam distillation and solvent extraction. Total 43 components were identified by? comparing gas chromatography retention time and mass spectral data. Different isolation techniques result in compositionally different isolates. The headspace(purge & trap) sampling procedure was found to be the best method of choice for a qualitative analysis of the volatile components.
The energy recovery rate estimation method proposed through the Waste Control Act does not take into account the energy used in practice. In addition, the method for measuring a lower heating value, which is the main factor of the energy recovery rate, was carried out through a small sampling amount, and thus the representative value of the waste was not reflected. With the revised estimation method (Notification No. 2015-215 of the Ministry of Environment), the energy recovery rate should be estimated based on the actual amount of energy used, and a heat balance method was proposed as a way to estimate the lower heating value. In this study, the lower heating value was estimated for seven industrial waste incineration facilities according to the revised estimation method. All data used in the estimations were achieved from measurement instruments applied to each of the incinerators and through direct measurements taken by the operators for the purposes of calculation. As a result, the lower heating value was estimated to be about 3,404.7 kcal/kg for the seven industrial waste incineration facilities.
CFC(CFC-12, CFC-11 and CFC-113) analytical system for air and water was constructed using a customized purge and trap extraction device and a gas chromatograph with an electron capture detector. Sampling methods of air and water for CFCs were also established. The analytical system was experimentally optimized to result in reproducibilities of triplicates less than 2% for current air samples and less than 5% for groundwater samples with CFC-12 concentration of 160 to 180 pg/kg, and verified with respect to the CFC system in USGS, which showed analytical results were in agreement within 10%. CFCs in air were monitored at three sites over 19-month period in the central part of South Korea, and the result indicates no significant local sources of CFCs in those areas. For groundwater in Jeju Island, CFCs were measured over a year with a two-month interval. The time-series data showed seasonal fluctuations which could be interpreted by the effect of recharge pulse derived from large amount of rainfall during monsoon period with a few month delay, which indicates high permeability of basaltic rocks in Jeju Island.
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