• Environmental Analysis Health and Toxicology
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• 제17권2호
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• pp.95-107
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• 2002

This study was designed to investigate the characteristics of atmospheric concentrations of toxic volatile organic compounds (VOCs) in Korea. Target compounds included 1,3-butadiene, aromatics such as BTEX, and a number of carbonyl compounds. In this paper, as the first part of the study, the performance of sampling and analytical methods was evaluated for the measurement of selected VOCs and carbonyl compounds in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/MSD analysis, while carbonyls by the DNPH-silica cartridge sampling with HPLC analysis. The methodology was investigated with a wide range of performance criteria such as repeatability, linearity. lower detection limits, collection efficiency, thermal conditioning, breakthrough volume and calibration methods using internal standards. In addition, the sampling and analytical methods established in this study were applied to real field samples duplicately collected in various ambient environments. Precisions for the duplicate samples appeared to be comparable with the performance criteria recommended by USEPA TO-17. The overall precision of the sampling and analytical methods was estimated to be within 20 ∼ 30% for major aromatic VOCs such as BTEX, whereas the precision for major carbonyl compounds such as formaldehyde and acetaldehyde was within 10 ∼ 20% for field samples. This study demonstrated that the adsorbent sampling and thermal desorption method can be reliably applied for the measurement of BTEX in ppb levels frequently occurred in common indoor and ambient environments.

• 한국환경보건학회지
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• 제28권2호
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• pp.109-116
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• 2002

The purpose of this study was to evaluate a new sampling and analytical method for the determination of airborne hexavalent chromium, Cr(Ⅵ), in a field plating operation. The procedures of this new method (Shin & Paik's Method) are as the following: Airborne hexavalent chromium is collected on polyvinyl chloride (PVC) filter according to the National Institute iota Occupational Safety and Health (NIOSH) Method 7600, and the filler sample is placed in a screw-capped vial and soaked with 2% NaOH/3% Na₂CO₃ solution immediately after sampling. The Cr(Ⅵ) sample is analyzed by ion chromatography/visible spectrophotometry (IC/VS) according to the U.S. Environmental Protection Agency (EPA) Method 218.6. The airborne Cr(Ⅵ) concentrations measured by this method were compared with those determined by three reference methods: One (NIOSH/EPA Method) consisted of sampling airborne Cr(Ⅵ) on PVC filters and storing the sample filters in strew-capped vials according to the NIOSH method, and analyzing Cr(Ⅵ) in samples using IC/VS according to the EPA method. The second method (Impinger Method/NaHCO₃) consisted of absorbing airborne Cr(Ⅵ) into 0.02 M NaHCO₃ solution in midget impinger, and analyzing the Cr(Ⅵ) in samples using IC/VS. The third method was the OSHA Method ID-215. Using these four different methods, lour replicates of air samples were collected at an electroplating process and analyzed simultaneously. Two-way ANOVA and paired t-test were used to test difference among values determined by the methods. There was no significant difference and a strong correlation (r²:0.99) between Cr(Ⅵ) concentrations measured by the Shin & Paik's Method and an impinger method (p>0.05). However, Cr(Ⅵ) concentrations determined by Shin & Paik's Method were significant1y different from those by the NIOSH/EPA Method (p<0.05) or the OSHA method (p<0.05). The Cr(Ⅵ) concentrations of Shin & Paik's Method were significantly higher than those of the NIOSH/EPA Method or the OSHA method. This result indicated that the Shin & Paik's Method may prevent Cr(Ⅵ) losses caused by reduction and give more reliable results of airborne Cr(Ⅵ) concentrations in work environments.

• Geomechanics and Engineering
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• 제9권6호
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• pp.743-755
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• 2015

It is well known that the quality of sample significantly determines the accuracy of soil parameters for laboratory testing. Although sampling disturbance has been studied over the last few decades, the theoretical investigation of soil disturbance due to sampling penetration has been rarely reported. In this paper, an analytical solution for estimating the soil disturbance due to sampling penetration was presented using cavity expansion method. Analytical results in several cases reveal that the soil at different location along the sample centerline experiences distinct phases of strain during the process of sampling penetration. The magnitude of induced strain is dependent on the position of the soil element within the sampler and the sampler geometry expressed as diameter-thickness ratio D/t and length-diameter ratio L/D. Effects of sampler features on soil disturbance were also studied. It is found that the induced maximum strain decreases exponentially with increasing diameter-thickness ratio, indicating that the sampling disturbance will reduce with increasing diameter or decreasing wall thickness of sampler. It is also found that a large length-diameter ratio does not necessarily reduce the disturbance. An optimal length-diameter ratio is suggested for the further design of improved sampler in this study.

• 한국산업보건학회지
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• 제33권4호
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• pp.455-463
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• 2023

Objectives: The aim of this study was to develop an air sampling and analytical method for estimating worker exposure to linear carbonate solvents and to evaluate the method. Methods: The target substances were three linear carbonates: DMC, DEC, EMC. GC/FID was used for sample analysis. Laboratory experiments were conducted to determine desorption solvents and sample capacity, and to evaluate storage stability, accuracy, and precision. Results: Coconut Shell Charcoal (CSC, 100/50 mg) was used as the air sampling media, and a desorption solvent of 5% methanol/95% dichloromethane was selected. Recommended sampling capacities were 1~11 ℓ for DMC, 1~18 ℓ for DEC, and 1~24 ℓ for EMC. The stability of three linear carbonates was demonstrated over 30 days in a refrigerator (4℃). Detection limits were determined as follows: DMC 0.26 ㎍/sample, DEC 0.24 ㎍/sample, and EMC 0.25 ㎍/sample. The total coefficient of variation was calculated as DMC 0.064, DEC 0.079, and EMC 0.07. Conclusions: This sampling and analysis method is suitable for estimating personal exposure to linear carbonates in the workplace.

• 한국대기환경학회지
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• 제18권1호
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• pp.39-49
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• 2002

In this study, limits of detection (LOD), accuracy and precision of four sampling/ analytical methods were evaluated and compared for the determination of airborne hexavalent chromium, Cr (VI). The methods include : (1) a combination of the National Institute for Occupational Safety and Health (NIOSH) Method 7600/U. S. Environmental Protection Agency (EPA) Method 218.6 (NIOSH/EPA Method) proposed by Shin and Paik, 2) two impinger methods using 2% NaOH/3% Na$_2$CO$_3$. (3) same as (2) but with 0.02 N NaHCO$_3$absorbing solution, and (4) the Occupational Safety and Health (OSHA) Method ID-215. An ion chromatograph/visible absorbance detector was used for the analysis of Cr (VI) in sample solution. Limit of detection (LOD) , analytical accuracy, and precision were also tested using Cr (VI) spike samples. Recoveries (as index of accuracy) and coefficient of variation (CV) (as a index of precision) were determined. Two-way ANOVA and Turkey's test were performed to test the significance in differences among recoveries and CVs of the methods. In all the methods, the peaks of Cr (VI) were separated sharply on chromatograms and exhibited a strong linearity with Cr (VI) concentrations in solution. The correlation coefficients of calibration curves typically ranged from 0.9997 to 0.9999, and the analytical LODs from 0.025 to 0.1$\mu\textrm{g}$/sample. All the method had good sensitivities and linearities between Cr (VI) levels and peak areas. The accuracies (% mean recoveries) of the methods ranged from 80.1 to 104.2%, while the precisions (pooled coefficient of variation) ranged from 3.16 to 4.43%. The impinger methods showed higher recoveries ( > 95%) than those of the PVC filter methods (the OSHA Method and the NIOSH/EPA Method). It was assumed that Cr (VI) on PVC filter was exposed to air and reduced to trivalent chromium, Cr (III), whereas it was stabilized in alkali solution contained in impinger. Thus, a special treatment of Cr (VI) samples collected on PVC filters may be required.

• 한국산업보건학회지
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• 제16권2호
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• pp.91-100
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• 2006

The purpose of this study was to validate alternative method by using non-carcinogenic, and less toxic solvents than NIOSH analytical method 5524 for measuring the airborne MWFs in workplaces. In laboratory tests, the ETM solvents(mixture of same volume for ethyl ether, toluene, and ethanol) were selected. The alternative method of analyzing MWFs, referred to as the ETM solvent extraction method, showed 0.04 mg/sample as LOD, and 0.15 mg/sample as LOQ. The analytical precision (pooled CV, coefficient of variation) of the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was 1.5%, 2.0%, 2.6%, 1.6%, respectively, which was similar to the precision (2.6%) of NIOSH analytical method (NIOSH 0500) for total dust. The analytical accuracy by recovery test, spiked mass calculated as extractable mass, was almost 100%. As the result of storage stability test, metalworking fluid samples should be stored in refrigerated condition, and be analyzed in two weeks after sampling. The 95% confidence limit of the estimated total standard error for the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was ${\pm}12.6%$, ${\pm}12.5%$, ${\pm}14.0%$, and ${\pm}13.6%$, respectively, which satisfied the OSHA sampling and analytical criteria.

• 한국산업보건학회지
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• 제19권2호
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• pp.96-101
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• 2009

The purpose of this study was to conduct the field validation of alternative method(ETM method) by using non-carcinogenic, and less toxic solvents than NIOSH (National Institute for Occupational Safety and Health) analytical method 5524 for measuring the airborne metalworking fluids in workplaces. We carried out the field validation test by using the exposure chamber, guaranteeing the air sampling homogeneously in a machining environment. The ETM mixed solvent presented the complete solubility of MWFs used in test field. Based on the field test data, the bias of the ETM method from reference method, NIOSH analytical method 5524, was from -7.0% to 5.1%. The overall uncertainty of the ETM nethod was 21.6%, which satisfied the NIOSH criteria for the sampling and analytical criteria.

• 분석과학
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• 제8권4호
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• pp.739-744
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• 1995

The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

• 분석과학
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• 제18권4호
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• pp.344-354
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• 2005

최근 들어 실내공기질 악화의 주 오염원인 건축자재에 대한 관심이 고조되면서 건축자재 오염물질 방출시험 자료 구축이 중요하게 됨에 따라, 신뢰성 있는 자료 확보를 위해 건축자재 방출시험 정도 관리에 대한 필요성이 대두되었다. 이에 본 연구는 건축자재 방출시험 성능에 대한 정도관리를 위해 총 휘발성 유기화합물과 포름알데히드에 대하여 기기분석 재현성, 회수율, 검출한계, 중복 및 반복채취 재현성, 파과용량 평가 등을 실시하였다. 기기분석 및 시료채취에 대한 재현성은 20~30% 이내의 양호한 결과를 보였으며, 회수율은 80% 이상으로 나타났으며, 파과 역시 일어나지 않아 소형챔버법에 의한 성능은 전반적으로 만족할 만한 수준을 보였다. 따라서, 소형챔버를 이용한 건축자재 오염물질 방출시험방법은 신뢰성있는 자료를 제공해 줄 수 있을 것으로 판단된다.

• 한국산업보건학회지
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• 제16권4호
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• pp.346-355
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• 2006

The purpose of this study was conducted to ascertain the difference between impinger and passive sampling methods in the process of sampling and analyzing on airborne formaldehyde. Formaldehyde generating workplaces included in this study comprised four types of manufacturing industry such as two workplaces of products of wood, cork, straw and plaiting materials manufacturing industries, one casting metal manufacturing industry, and one parts and accessories for motor vehicles and it′s engines manufacturing industry. Workplaces contained in this study were located in some manufacturing area of Busan industrial complex and this study was carried out during a period from January 2003 to December 2004. Analytical accuracy, precision and detection limit of two methods was compared. Exposure level of its airborne concentration was evaluated in formaldehyde generating workplaces those were classified by types of industry, working process, and time. The results were as follows ; 1. A rate of recovery was 107.1% in impinger method and 101.8% in passive method, and precision was 7.79% in impinger method and 4.40% in passive method. There was no statistical significance in analytical accuracy and precision between two methods. A limitation of detection was 0.011 ppm in passive method which was lower than that of impinger method (0.020 ppm) by 1.8 times. 2. Airborne formaldehyde concentration of impinger method was different from passive method. It′s concentration by passive method was higher by 5.1 times than that by impinger method in the parts and accessories for motor vehicles and it′s engines manufacturing industry (P<0.05). Only in molding process among several types of processes, formaldehyde concentration in passive method was higher by 5.1 times than that in impinger method (P<0.05). Furthermore, formaldehyde concentration in passive method was higher by 1.7 times than that in impinger method (P<0.05) in the first half of year 2003. 3. The geometric mean of formaldehyde concentration in impinger method was lower than that in passive method, but there was no statistical significance of formaldehyde concentration by the difference of sampling method. In conclusion, it is difficult to conclude which is better between the two sampling methods because of no statistical significance for the difference of concentration. Because of lacks of certified passive sampling and analytical method, at present situation, studies on verification of accuracy and precision, obstructive reaction against validity on its exposure assessment, and research to develop domestically manufactured passive sampler in terms of cost-effectiveness should be continuously carried out.