• Analytical Science and Technology
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• v.26 no.4
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• pp.287-297
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• 2013

The optimization of analytical method for the thermal desorption of seven VOCs (volatile organic compounds) by TD-GC/MS (thermal desorption-gas chromatograph-mass spectrometer) with solid phase sorbent tube, and comparative analysis for the determination of VOCs plotted by standard sorbent tubes prepared using both gas phase and liquid phase materials were investigated. The result of paired t-test showed that a liquid phase standard sorbent tube method was in agreement with a gas phase standard sorbent tube method for six species of VOCs including benzene, toluene, ethylbenzene, o-, m-, and p-xylene except for styrene at the significance level (${\alpha}=0.01$), while the 15.6% of difference in response factor between both of gas phase and liquid phase standard plotting for the determination of styrene showed that both methods were significantly different at the significance level. Therefore, the liquid phase standard plotting method was employed to reduce erroneous data for the determination of styrene including BTEX. Under the optimized analytical method by liquid phase standard sorbent tube, recovery was between $100{\pm}5%$ for 7 species of VOCs, reproducibility ranged from 0.3 to 7.7%, and method detection limit (MDL) ranged from $0.01{\mu}g/m^3$ for o-xylene to $0.27{\mu}g/m^3$ for toluene. The optimized standard method was applied to determine VOCs VOCs from indoor air of of dormitory, one bedroom apartment, and a new car.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.9 no.1
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• pp.173-186
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• 1999

To utilize diffuse sampling of formaldehyde in air, a new sampler was designed. A glass fiber filter was impegnated with 2,4-dinitrophenylhydrazine(DNP) and phosphoric acid and mounted 37mm cassette. The formaldehyde vapor was sampled in the dynamic chamber and measured by high performance liquid chromatograph and compared with solid sorbent tube. The results were as follows ; 1. The desorption efficiencies of diffusive sampler between 97.0% and 100%. 2. the sampling rate is constant as in $58{\sim}61.8m{\ell}/min$ when sampling times are between 120 and 360 min. 3. There was a significant relationship between concentrations of diffusive samples and active samples with the coefficient of determination(R2) of 0.92. 4. Desorbed amount of formaldehyde diffusive sampler was increased by high relative humidity. 5. Wheth diffusive samplers were stored at room temperature or at refrigerator there was no statistically significant difference in the accuracy of result. 6. When the diffusive samplers, which collected formaldehyde vapor, were exposed to clean air for three hours, there was no significant loss of formaldehyde due to reverse diffusion. In conclusion, this study suggest that developed diffusive samplers will be a reasonable substitute for the solid sorbent tube for sampling formaldehyde and practical comparative study of developed diffusive sampler should be performed at workplaces of manufacturing industry.

• Korean Chemical Engineering Research
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• v.50 no.3
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• pp.492-498
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• 2012

In this study, hydrodynamics such as solid circulation rate and voidage in the desulfurizer and the reaction characteristics of Zn-based solid sorbents were investigated using lab-scale high pressure and high temperature desulfurization process. The continuous HGD (Hot Gas Desulfurization) process consist of a fast fluidized bed type desulfurizer (6.2 m tall pipe of 0.015 m i.d), a bubbling fluidized bed type regenerator (1.6 m tall bed of 0.053 m i.d), a loop-seal and the pressure control valves. The solid circulation rate was measured by varying the slide-gate opening positions, the gas velocities and temperatures of the desulfurizer and the voidage in the desulfurizer was derived by the same way. At the same gas velocities and the same opening positions of the slide gate, the solid circulation rate, which was similar at the temperature of $300^{\circ}C$ and $550^{\circ}C$, was low at those temperatures compared with a room temperature. The voidage in the desulfurizer showed a fast fluidized bed type when the opening positions of the slide gate were 10~20% while that showed a turbulent fluidized bed type when those of slide gate were 30~40%. The reaction characteristics of Zn-based solid sorbent were investigated by different desulfurization temperatures at 20 atm in the continuous operation. The $H_2S$ removal efficiency tended to decrease below the desulfurization temperature of $450^{\circ}C$. Thus, the 10 hour continuous operation has been performed at the desulfurization temperature of $500^{\circ}C$ in order to maintain the high $H_2S$ removal efficiency. During 10 hour continuous operation, the $H_2S$ removal efficiency was above 99.99% because the $H_2S$ concentration after desulfurization was not detected at the inlet $H_2S$ concentration of 5,000 ppmv condition using UV analyzers (Radas2) and the detector tube (GASTEC) which lower detection limit is 1 ppmv.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.6 no.1
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• pp.17-27
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• 1996

This study was designed to survey exposure levels of formaldehyde among workplaces in some plywood industries and to compare three sampling methods including the impinger method(IM, NIOSH method No. 3500), the solid sorbent tube method(SS, NIOSH method No. 2541), and the passive bubbler monitor method(PB, SKC). The survey was conducted in seven particle board manufacturing factories, two resin manufacturing factories and two plywood manufacturing factories in Incheon area during the period from March 6 to April 20, 1995. The workplaces included were the hot/cold press, the roller/spreader, the soaking/drying, and the reaction/mixing areas. The results were as follows; 1. The average(GM, GSD) concentrations of formaldehyde by sampling methods were 0.11(4.43) ppm by IM, 0.27(2.03) ppm by SS, and 0.29(2.04) ppm by PB, respectively. The concentrations by 1M method were statistically very significantly lower than those of SS and PB methods, particularly at low air borne concentrations of formaldehyde (p<0.001). 2. The area average concentrations of formaldehyde by workplaces measured with PB bubblers were 0.23(2.08) ppm from the press, 0.23(1.77) ppm from the spreader, 0.24(1.51) ppm from the soaking, and 0.46(1.96) ppm from the reaction areas, respectively. The personal average concentrations of formaldehyde by workplaces measured with PB bubblers were 0.30(1.77) ppm from the press, 0.33(1.54) ppm from the spreader, 0.36(1.46) ppm from the soaking, and 0.84(1.19) ppm from the reaction areas, respectively. 3. No statistically significant differences of formaldehyde concentrations among workplaces except the reaction area(p<0.001) were found. 4. Formaldehyde concentrations from personal samples were higher than those of from area sam pies in all workplaces studied. But no statistically significant differences of formaldehyde concentrations both area and personal samples were found. In conclusion, this study found that although formaldehyde concentrations in some plywood industries in Incheon area were below the regulatory limit of 1 ppm, they were over the limits recommended by NIOSH and ACGIH. This study also suggests that the impinger method may underestimate true formaldehyde concentrations. It implies that there will be more workplaces not meeting current regulatory limit if either the solid sorbent or passive bubbler methods were used instead of the impinger method. It is suggested that passive monitors will be a reasonable alternative for area and personal sampling of formaldehyde if the accuracy and validity of passive monitors be verified before use.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.11 no.3
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• pp.241-248
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• 2001

The main factors of breakthrough are known to sampling time, flow rate, concentration of the sample, temperature, humidity, and the physical characteristics of the solid sorbent tube. However, no study has been reported the effect of temperature and sampling volume on the breakthrough of acharcoal tube during vinyl chloride monomer (VCM) sampling. The objective of this study is to suggest the optimal sampling condition during VCM sampling based on National Institute for Occupational Safety and Health (NIOSH) method. To evaluate adequate sampling volume for VCM without breakthrough, volume of 1, 2, 3, 4, and 5 L each from VCM of 1, 5, 10, 15, and 20ppm at flow rate of 0.05 L/min were sampled in $22^{\circ}C$ and $40^{\circ}C$. At $22^{\circ}C$, in the case of 1, 5, 10, and 15ppm, VCM was adsorbed completely in first section of charcoal tube regardless of sampling volume. But in 20ppm, detection rates are 99.56% in first section and 0.44% in second section. At $40^{\circ}C$ of 1ppm, VCM was adsorbed completely in first section. In 10, 15, and 20ppm, detection rates of second, third, and forth sections were decreased significantly by reduction of sampling volume. In determination of breakthrough based on NIOSH method, no breakthrough was occurred in 20ppm at $22^{\circ}C$. At $40^{\circ}C$, breakthrough was occurred in 10, 15, and 20ppm when sampling volume was 5L. Although no breakthrough was occurred when sampling volume was 3L. Finally, in environment of temperature around $22^{\circ}C$, breakthrough may not occurred up to 20ppm during sampling for VCM. During sampling for VCM in environment of temperature around $40^{\circ}C$, no breakthrough occurred in 1-5ppm and 10-20ppm when sampling volume is 5L and 3L respectively. This result suggests that the sampling volume should be considered when VCM sampling under hot conditions (> $22^{\circ}C$) by the NIOSH method No. 1007.

• Journal of Korean Society for Atmospheric Environment
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• v.30 no.6
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• pp.586-599
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• 2014

During the last two decades, indoor air quality and volatile organic compounds (VOCs) have been of concern in Korean society due to their nature of potential health impacts. In order to investigate the pollution levels of VOCss in indoor environments, establishment of a solid test method for monitoring the airborne VOCss is essential. In Korea, a method based on adsorbent sampling and GC analysis coupled with thermal desorption was proclaimed as the Korea Standard Method for Indoor Air Quality Test. This study was carried out to examine some inherent problems of the VOCs measurement method. The VOCs method does not describe in detail preparing the standard samples. The standard samples may be prepared by impregnation of either liquid standard solutions or a mixture of standard gases. In this study, we investigated the optimal temperature condition for transferring the liquid standards onto a standard adsorbent tube. As a result, keeping the impregnation temperature at $250^{\circ}C$ will be recommended in regard of the boiling points of multiple target analytes and the thermal stability of the adsorbent. We also demonstrated some problems associated with handling of a syringe used for transferring the standard solutions onto the adsorbent tubes, and a best way to get rid of the syringe problems was suggested. Finally, a number of field works were conducted to evaluate the performance of adsorbent sampling methods. Comparison of different adsorbent tubes, i.e. tube packed with single sorbent (Tenax) and double sorbents (Tenax with Carbotrap), revealed that 30 to 40% differences between the two groups, implying that sampling efficiency is depending on the volatility and the strength of adsorbents. However, duplicate precisions for VOCs sampling with a same type of adsorbent and at same flow rates appeared to be satisfactory to be all within 20%, which is a quality control guideline. Distributed volume precisions were also found to be within a guideline value, 25%, although the precision was in general inferior to the duplicate precision. The Korea indoor VOCs test method should be more refined and improved in many aspects, particularly procedure and instrumentation for preparing the standard samples and specification of quality control assessment.

• Analytical Science and Technology
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• v.24 no.3
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• pp.200-211
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• 2011

In this study, 13 compounds including four volatile fatty acids (VFA) and nine volatile organic compounds (VOC) were analyzed by cryogenic trapping-thermal desorption technique. In order to evaluate the analytical method for VFA, calibration experiments were performed using five different sorbent materials. When the calibration results are compared between different sorbents, sampling tube filled with Carbopack X showed the highest response factor (RF) for both VFA and VOC. To validate this new analytical method for VFA using cryogenic trapping-thermal desorption technique, this method was compared with alkali absorption method recommended by the odor prevention law of the Korea Ministry of Environment (KMOE). For this purpose, unknown samples were analyzed by two different methods, i.e., cryogenic trapping-thermal desorption (TD) and alkali absorption with solid phase microextraction (SPME). When the results of two different methods were compared, ratios of concentrations determined by the two analytical methods (TD/SPME) was found as 0.46 (valeric acid) ~ 0.71 (isovaleric acid). Therefore, additional study is required to properly establish and find stable analytical conditions for VFA analysis. Furthermore, comparison between two different methods should be made with more reliable calibration approaches.