• 분석과학
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• 제14권4호
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• pp.306-310
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• 2001

황상용액 매질에서 요오드 음이온을 흡착제에 흡착시킨 후 황산용액에 남아있는 요오드 음이온을 정량하기 위해 이온 크로마토그래피를 적용하였다. 산화제 작용을 하는 황산의 농도를 0.25 M, 0.5 M, 1 M로 변화시키고 요오드 음이온을 각각 첨가한 후 시간변화에 따라 요오드 음이온이 산화되는 정도를 측정하였다. 황산농도가 진할수록 요오드 음이온은 산화되어 휘발하므로 적게 검출되었다. 수산화나트륨 용액을 사용하여 환산매질을 중화하였다. 중화된 0.5 M $Na_2SO_4$ 매질 중 요오드 음이온의 농도범위가 0-20 mg/L인 구간에서 검정곡선의 직선성이 좋게 나타났다(r=0.99999).

• Journal of the Korean Wood Science and Technology
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• 제45권4호
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• pp.471-481
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• 2017

As the molecular weight (MW) of urea-formaldehyde (UF) resins had a great impact on their properties, this work was conducted to study effect of analytical parameters of gel permeation chromatography (GPC) on the MW measurement of UF resins. GPC parameters such as flow rate, column, detector temperature, and sample injection temperature were selected to compare number-average molecular weight (Mn), weight-average molecular weight (Mw), molecular weight distribution (MWD) and polydispersity index (PDI) of two UF resins with different viscosities. As expected, UF resin with higher viscosity resulted in greater Mn and Mw than those of low viscosity UF resin. When the flow rate increased, both Mn and Mw of UF resins decreased and MWD became narrower. By contrast, both Mn and Mw increased and MWD became wide when the column, detector, and sample injection temperature increased. The column, detector, and sample injection temperature of $50^{\circ}C$ at a flow rate of $0.5m{\ell}/min$ resulted in the highest MW and broadest MWD for the GPC analysis. These results suggest that the apparent molecular size or a hydrodynamic radius of UF resin molecules dissolved in the mobile phase affect to Mn, Mw and MWD.

• 한국환경과학회지
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• 제24권12호
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• pp.1569-1582
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• 2015

The analytical method for 16 organophosphorus pesticides was developed in this study. The 16 organophosphorus pesticides were analyzed by liquid chromatography-tandem mass spectrometry (LC/MS/MS) using on-line solid phase extraction (on-line SPE) with PLRP- S cartridge. Analysis of all analytes in the MS/MS was processed in the electrospray ioni-zation (ESI) positive mode. They are Azinphos ethyl, Chlorfenvinphos, Ethion, Famphur, Phosmet, Phosphamidon, Terbufos, Aspon, Chlorpyrifos-methyl, Crotoxyphos, Dichlofenthi-on, Dicrotophos, Fonofos, Thionazin, Dimethoate and Iprobenfos. Limits of detection (LODs) and Limits of quantification(LOQs) were obtained as 0.8~2.0 ng/L and 2.6~6.4 ng/L, respectively. All compounds were not detected at the 8 sampling points of the raw water and clean water.

• 분석과학
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• 제12권2호
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• pp.89-93
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• 1999

적은 양의 시료를 분석할 수 있는 마이크로 컬럼 이온 크로마토그래피용 전도도 셀과 억압컬럼을 개발하였다. 안지름이 작은 모세관 컬럼을 사용하는 경우 이동상의 유속은 보통 $5{\sim}20{\mu}L/min$ 정도 된다. 따라서 이 경우 일반적인 전도도 셀은 사용할 수가 없기에 내부 부피가 작은 모세관 컬럼용 전도도 셀과 억압컬럼을 제작하였다. 전도도 셀은 두 개의 백금 피하주사 바늘을 안지름이 0.010 mm인 튜브 속에 넣어 간격이 $2{\mu}m$ 되게 만들었고, 억압컬럼은 Nafion 튜브를 이용하여 막-억압컬럼 형태로 개발하였다. 이 전도도 셀과 억압컬럼을 이용하여 실제 음이온들(플루오르화물, 아질산염, 질산염, 염소산염)을 분석한 결과 재현성 있고 양호한 크로마토그램을 얻었다.

• 한국축산식품학회지
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• 제29권4호
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• pp.482-486
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• 2009

The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

• 분석과학
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• 제31권3호
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• pp.112-121
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• 2018

The hydrothermal carbonization method has received great attention because of the conversion process from biomass. The reaction produces various products in hydrochar, bio-liquid, and gas. Even though its yield cannot be ignored in amount, it is difficult to find research papers on bio-liquid generated from the hydrothermal carbonization reaction of biomass. In particular, the heterogeneity of feedstock composition may make the characterization of bio-liquid different and difficult. In this study, bio-liquid from the hydrothermal carbonization reaction of food wastes at $230^{\circ}C$ for 4 h was investigated. Among various products, fatty acid methyl esters were analyzed using two different extraction methods: liquid-liquid extraction and column chromatography. Different elutions with various solvents enabled us to categorize the various components. The eluents and fractions obtained from two different extraction methods were analyzed by gas chromatography with a mass spectrometer (GC/MS). The composition of the bio-liquid in each fraction was characterized, and seven fatty acid methyl esters were identified using the library installed in GC/MS device.

• Bulletin of the Korean Chemical Society
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• 제35권11호
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• pp.3280-3288
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• 2014

Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method ($r^2$ > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to $200ng\;mL^{-1}$. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

• KSBB Journal
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• 제25권5호
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• pp.459-465
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• 2010

A simple and efficient analytical method for the simultaneous determination of seven tar color additives was developed using ion pair high performance liquid chromatography. The conditions for HPLC analysis were as follows: column, ${\mu}$-Bondapak C18 (10 ${\mu}m$, 300 ${\times}$ 3.9 mm i.d.); gradient mobile phase, 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrile-methanol (65:25:10) as a mobile for fraction A and 0.025 mol/L ammonium acetate (containing 0.01 mol/L tetrabutylammonium bromide)-acetonitrilemethanol (40:50:10) as a mobile for fraction B; flow rate, 1.0 mL/ min; detection wavelength, 254/520/620 nm. We could attain to the detection limits as 0.01~0.05 ${\mu}$g/mL (254 nm) and 0.005~0.01 ${\mu}$g/mL (520 nm) for six red tar color additives, and 0.05 ${\mu}$g/mL (254 nm) and 0.002 ${\mu}$g/mL (620 nm) for Fast green FCF. This analytical method was applicable to determine the tar color additives contained in several commercial cold syrups.

• Safety and Health at Work
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• 제12권2호
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• pp.209-216
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• 2021

Background: The article presents the results of studies performed in order to develop a new method of airborne potassium bromate(V) determination at workplaces. Methods: The method is based on a collection of the inhalable fraction of potassium bromate(V) using the IOM Sampler, then extraction of bromates with deionized water and chromatographic analysis of the obtained solution. The analysis was performed using ion chromatography with conductometric detection. The tests were performed on a Dionex IonPac®AS22 analytic column (250 × 4 mm, 6 ㎛) with AG22 precolumn (50 × 4 mm 11 ㎛). Results: The method provides for potassium bromate(V) determination within the concentration range of 0.043 ÷ 0.88 mg/m³ for an air sample of 0.72 m³ in volume, i.e., 0.1-2 times the exposure limit value as proposed in Poland. The method was validated in accordance with PN-EN 482. The obtained validation data are as follows: measuring range: 3.1-63.4 ㎍/mL, limit of detection (LOD) = 0.018 ㎍/mL and limit of quantification (LOQ) = 0.053 ㎍/mL. The developed method has been tested in the work environment, on laboratory employees having contact with potassium bromate(V). Conclusion: The analytical method allowed the determination of the inhalable fraction of airborne potassium bromate(V) at workplaces and can be used to assess occupational exposure.

• 분석과학
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• 제35권5호
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• pp.197-204
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• 2022

A gas chromatography-mass spectrometric method was developed for determining 5-chloro-2-methyl-4-isothiazolin-3-one (CMIT), 2-methyl-4-isothiazolin-3-one (MIT), 1,2-benzisothiazolin-3-one (BIT), 3-iodo-2-propynyl butyl carbamic acid (IPBC) and benzoic acid (BA) in household products. A 0.5 g sample was placed in a test tube and dissolved with 5 mL water, 5 mL methylene chloride and 1.0 mL methanol. The solution was extracted by ultra-sonication followed by mechanical shaking using the salting out effect. Under the established condition, the lowest quantification limits of all analytes were in the range of 0.04-10 mg/kg and their relative standard deviations were less than 8.0 %. The method was used to analyze 10 household products. As a result of analyzing 10 household products, MIT was detected in the range of 1.2-3.5 mg/kg in 3 of 10 samples, CMIT was detected in the range of 2.6-8.2 mg/kg in 3 of 10 samples, and BA was detected in the range of 5.0-15 mg/kg in 4 of 10 samples. Meanwhile, BIT and IPBC were not detected in any of the products. It has been shown that this method can be used for the simultaneous determination of biocides with various physical and chemical properties in household products.