• 공업화학
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• 제4권4호
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• pp.721-730
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• 1993

$Cu_xH_3-2_xPMo_{12}O_{40}{\cdot}_nH_2O$에서 구리의 치환양 x를 변화시켜 여러 가지의 헤테로폴리산 동염 촉매를 제조하고, 열분석, X-선 회절분석, 적외선 분광분석, 비표면적 측정, 전자현미경 분석, 암모니아의 승온탈착법 등으로 촉매의 특성을 조사하였다. 아크롤레인의 산화반응에 대한 이 촉매계의 반응특성은 고정층 연속반응기에서 조사하였다. 이 촉매들은 $200^{\circ}C$ 근처에서 결정수의 탈리가 일어났고 구리의 치환에 따른 구조수의 탈리는 $300{\sim}400^{\circ}C$ 사이에서 관찰되었다. 이들 촉매는 Keggin 구조를 가짐을 확인할 수 있었고, 구리의 치환양이 증가함에 따라 Keggin 음이온인 $(PMo_{12}O_{40})^{3-}$의 분해 정도가 증가하였으며, 이때 분해 생성물로 소량의 $MoO_3$와 $P_2O_5$가 관찰되었다. x가 증가할수록 아크롤레인의 전화율이 감소하였는데 이것은 비표면적과 전체 산점의 양이 감소하였기 때문인 것으로 판단된다. 그러나 단위면적당 반응속도와 아크릴산의 선택도는 x=1.0에서 가장 높게 나타났으며 이 촉매는 독특한 산점분포를 나타내었다.

• 한국대기환경학회지
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• 제21권2호
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• pp.191-204
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• 2005

Building and furnishing materials and consumer product are important sources of volatile organic compounds(VOCs) and other aldehydes in the indoor environment. Some available evidence indicates that VOCs can cause adverse health effects to the building occupants and contribute to some of the symptoms of what we call, 'Sick House Syndrome' in Korea. The aims of this study were to evaluate the efficiency of emission system and to investigate comparison of the emission characteristics of different building materials such as wall-papers, paints, and adhesives. The emission of VOCs from building materials were determined in the small chambers defining the temperature, relative humidity, and ventilation rate in this study. VOCs were sampled for 20 minutes using Tenax-TA tubes and analysed by GC-MS with thermal desorption. The stability of conditions for temperature and relative humidity in this small chamber system showed that the fluctuation of temperature was between 25.4$\pm$0.3$^{\circ}C$ and that of relative humidity was 50.2$\pm$0.6$\%$ under the airflow rate of 167 mL/min. The emission tests from building materials resulted in TVOC emission rates of 0.011 $\~$ 3.108 mg/m$^{2}$h after 7 days. The general wall-papers emitted toluene abundantly and the natural wall-papers mainly emitted n-butanol and a minor amount of alkanes compound such as n -tetradecane. The remainder consisted of toluene, m,p -xylene, and styrene. The paints mainly emitted toluene and the adhesives mainly emitted chloroform as well as toluene. As a result, this study is expected to suggest meaningful data for future studies in exposure control through selecting healthy building materials and for the establishment of guidelines for various building materials in Korea.

• 한국지하수토양환경학회지:지하수토양환경
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• 제21권6호
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• pp.179-191
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• 2016

In addition to the measurement of the concentration of soil contaminants, the new idea of indicative parameters was proposed to validate the remedial works through the monitoring for the changes of soil characteristics after applying the clean up technologies. The parameters like CFU (colony forming unit), pH and soil texture were recommended as indicative parameters for land farming. In case of soil washing, water content and the particle size distribution of the sludge were recommended as indicative parameters. The sludge is produced through the particle separation process in soil washing and it is usually treated as a waste. The parameters like water content, organic matter content, CEC (cation exchange capacity) and CFU were recommended as indicative parameters for the low temperature thermal desorption method. Besides the indicative parameter, sampling methods in stock pile and the optimal minimum amount of composite soil sample were proposed. The rates of sampling error in regular grid, zigzag, four bearing, random grid methods were 17.3%, 17.6%, 17.2% and 16.5% respectively. The random grid method showed the minimum sampling error among the 4 kinds of sampling methods although the differences in sampling errors were very little. Therefore the random grid method was recommended as an appropriate sampling method in stock pile. It was not possible to propose a value of optimal minimum amount of composite soil sample based on the real analytical data due to the dynamic variation of $CV_{fund{\cdot}error}$. Instead of this, 355 g of soil was recommended for the optimal minimum amount of composite soil sample under the assumption of ISO 10381-8.

• 분석과학
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• 제18권1호
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• pp.66-73
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• 2005

본 연구에서는 주요 환원황 화합물에 해당하는 4가지 황성분, $H_2S$, $CH_3SH$, DMS, DMDS을 이용하여, 이들의 주요 검출방법에 해당하는 GC/PFPD 방식의 검출특성을 대부분의 환경시료의 분석에 활용할 수 있는 두 가지 기준에서 비교 분석하였다. 우선 수 십 ppb 단위의 고농도 시료들에 대한 분석특성을 이해하기 위해, GC/PFPD에 루프주입장치를 결합한 고농도 모드 시스템을 구성하고, 이에 대한 평가를 시도하였다. 그리고 이에 대비하여, 열탈착 시스템을 연계한 저농도 모드 시스템을 이용하여, 환경대기와 같이 극단적으로 낮은 농도 (ppt 수준)로 존재하는 시료들의 분석기법을 평가하였다. 양 분석방식의 비교에 의하면, 개별 황성분들의 검출특성은 대단히 규칙적인 특성을 유지하는 것으로 나타났다. 고농도모드를 이용한 비교결과에 의하면, 황화수소의 경우 가장 약한 감도를 보인 반면, 황원소를 두개 함유한 DMDS는 가장 민감한 감도를 보였다. 고농도 모드에 대비하여 저농도 모드의 감도를 비교할 경우, 감도가 수십 배 수준으로 감소하는 것으로 나타났다. 양 방식의 뚜렷한 감도차이에도 불구하고, 선택한 모드에 상관없이 황성분들의 상대적인 검량특성은 비교적 규칙적인 경향성이 유지되는 것으로 나타났다. 이들 성분에 대한 정확한 검량을 위해서는 다양한 관점에서 검출특성을 정의하기 위한 노력이 수반되어야 할 것으로 사료된다.

• 한국대기환경학회지
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• 제25권6호
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• pp.523-538
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• 2009

Recently, there has been a keen demand for real-time automatic monitoring of VOCs not only in Korea but other developed countries. We carried out this study to evaluate and to optimize the performance of a continuous automatic monitoring system for hazardous VOCs (HVOCs) in the ambient atmosphere, using an on-line GC system. The online system normally consisted of a Nafion dryer prior to a cold trap of an automatic thermal desorption apparatus and a GC system equipped with two detectors, i.e. PID and ECD. Preliminary tests conducted to check out any contamination of the system revealed an evidence of significant artifact formation of benzene, and it was found that the Nafion dryer (even brand new one) is the source of the benzene artifact. Thus, all the subsequent experiments in this study was carried out inevitably by removing the Nafion dryer. The on-line GC method was investigated with a variety of QC/QA performance criteria such as repeatability, linearity, lower detection limits, and accuracy. In order to find out the best operating condition for the on-line GC system, three different types (in terms of adsorption strength) of cold trap combinations were tested, i.e. (i) Tenax-TA and Carbopack-B combination (weak and hydrophobic); (ii) Tenax-TA, Carbopack-X and Carboxen-1000 combination (strong and hydrophilic); and (iii) Tenax-TA and Carbopack-X combination (medium and hydrophobic/hydrophilic). The USEPA TO-17 manual method was selected as a reference method to evaluate the performance of the on-line method. A series of experiments revealed that the system performance was superior to others when a cold trap packed with hydrophilic adsorbents (Tenax-TA/Carbopack-X/Carboxen-1000 combination) was used and operated at $25^{\circ}C$. However, the system with a cold trap packed with a combination of Tenax-TA and Carbopack-X is more recommended for field applications since the carboxen-1000 adsorbent is too sensitive to water vapor, and hence the performance of the system might be very unstable to humid samples or during rainy days. Furthermore, the precision and accuracy criteria of the Tenax-TA/ Carbopack-X combination were generally compatible with the triple adsorbents cold trap. The continuous automatic monitoring method is, thus, considered very useful to real-time monitoring to understand the variations of VOCs concentrations in ambient air, as it adopts much simpler procedures in sampling, analysis, and data integration steps than manual monitoring methods. However, it should be noted that there is a high possibility of benzene artifacts formation through the Nafion dryer, which is often installed to remove water vapor in air samples before being adsorbed onto the cold trap. Therefore, if a Nafion dryer is used in any studies of monitoring VOCs, the benzene contamination should be carefully examined before carrying out obtaining the data.

• 분석과학
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• 제14권5호
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• pp.432-441
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• 2001

본 연구에서는 Tenax-GR을 이용한 고체흡착관과 curie-point식 열탈착 장치로 구성된 농축장치와 자동시료채취장치를 short column GC/PID의 주입구에 연결하여 대기압 이하에서 작동되는 자동화된 휴대용 농축-기체 크로마토그래프 시스템을 개발하였다. 이 시스템은 농축-열탈착-분석 및 세정의 3과정이 한 단위로 작동되며 1~2 min 주기로 연속적인 단위조작이 가능하였다. 톨루엔 표준기체로 검토한 농축장치는 $0.405{\sim}4.05mg/m^3$의 농도범위에서 $94.7{\pm}6.6{\sim}103.8{\pm}3.1$의 높은 회수율을 나타냈고, 7% 이내의 RSD로 좋은 재현성을 나타냈다. 4 m의 짧은 모세관 컬럼을 사용한 본 시스템에서는 벤젠, 톨루엔 및 자일렌(BTX)의 혼합표준기체를 30 sec 이내에 신속하게 분리할 수 있었다. 그리고 컬럼출구의 압력이 입구보다 낮은 진공 GC로 작동되기 때문에 일반 GC에 비해 컬럼의 단위길이당 분리능을 높일 수 있었다. 본 시스템의 벤젠, 톨루엔, o-자일렌 표준기체의 검출한계는 각각 41, 49, $472ng/m^3$로 나타났다. 따라서, 본 시스템은 환경대기 중 저농도의 BTX를 수 분 이내의 주기로 연속모니터링하는 장치로 현장에 적용할 수 있을 것이라 생각된다.

• 분석과학
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• 제23권1호
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• pp.24-35
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• 2010

본 연구에서는 GC-PFPD와 열탈착 분석기법을 이용한 환원 황화합물(reduced sulfur compounds: RSC)에 대한 열탈착 검량방식의 시간적 재현성을 기존의 외부 검량기법에 덧붙여, 내부표준시료 기법을 연계하여 평가하고자 하였다. 이를 위하여, 4종류의 악취성 황화합물질($H_2S$, $CH_3SH$, DMS, DMDS)과 이들에 대한 내부 표준시료로 CS2를 준비하였다. 이들 표준시료는 저농도(10, 20, 50, 100 ppb)와 고농도 그룹(100, 200, 500, 1000 ppb)을 대표할 수 있게 넓은 범위로 준비하였다. 그리고 외부검량(external calibration)방식의 분석 결과를 부피고정방식(fixed standard volume: FSV)과 농도고정방식(fixed standard concentration: FSC)로 비교하였다. 또한, 2차적으로 FSV 방식의 결과에 외부 및 내부 검량기법을 동시에 적용하여 검량방식의 경시변화(안정도)를 평가하였다. 본 실험의 결과, 감도에 대한 경시변화는 FSC 방식에 비해 FSV 방식에서 작게 나타났다. 따라서 RSC 분석에서 FSV방식이 경시변화를 줄여주는데 상대적으로 효과적이라는 것을 알 수 있었다. 2차적으로 FSV 방식의 결과에 대해 외부 및 내부방식의 감도(기울기 값)를 비교하였다. 이러한 비교를 상대표준편차(RSD)값으로 평가하면, GC-PFPD-TD 시스템의 감도가 비교적 강한 경시변화를 보인다는 것을 알 수 있다. 따라서 이러한 분석기법의 시간적 재현성을 확보하기 위해서는 여러 가지 검정노력이 필요한 것으로 사료된다.

• 한국환경보건학회지
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• 제46권2호
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• pp.150-158
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• 2020

Objective: This study is designed to measure the concentration of DBPs (disinfection by-products) in pool water and in air and to estimate the carcinogenic potential through the evaluation of inhalation exposure. Methods: The subjects were six indoor swimming pools with many users in Gwangju. Samples of pool water and indoor air were taken every one month from August 2018 to August 2019 and analyzed for eight swimming pool standards. Three-liter air samples were collected and the VOCs were analyzed using GC/MS directly connected to thermal desorption. Results: pH was 6.8-7.5 and the concentration of free residual chlorine in pool water was 0.40-0.96 ?/ℓ. Physicochemical test items such as KMnO₄ consumption and heavy metal items such as Aluminum met existing pool hygiene standards. No VOC materials were detected except for the DBPs. The concentration of THMs in the pool water was 11.05-41.77 ㎍/L and the THMs mainly consist of Chloroform (63-97%) and BDCM (3-31%). The concentration of indoor air THMs is 13.24-32.48 ㎍/㎥ and consists of Chloroform. The results of carcinogenic assessment of chloroform in the indoor swimming pool via inhalation exposure were 2.0 to 6.4 times higher than the 'acceptable risk level' suggested by the US EPA. Conclusions: The concentration of THMs in the pool water is 11.05-41.77 ㎍/L, most of which is chloroform. In addition, the concentration of indoor air THMs is 13.24-32.48 ㎍/㎥. The result of carcinogenic assessment of chloroform was 2.0 to 6.4 times higher than the 'acceptable risk level' suggested by the US EPA.

• 공업화학
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• 제10권2호
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• pp.304-309
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• 1999

한국산 벤토나이트에 0.2 M $AlCl_3{\cdot}6H_2O$ 수용액과 0.5 M NaOH 수용액을 혼합하여 제조한 수산화 알루미늄 올리고머를 층간 삽입시켜 다공성의 Al-pillared clay를 합성하여 특성 분석 및 열 안정성을 조사하였다. 합성한 aluminum-pillared clay는 수산화 알루미늄 올리고머의 OH/Al의 몰비가 0.25~2.25로 증가할수록 비표면적은 $104{\sim}228m^2/g$으로 증가하였고, 미세세공 면적과 미세세공 부피도 비표면적과 함께 증가하였다. 또한 BJH식으로 계산된 기공분포로부터 약 $40{\AA}$ 정도의 mesopore도 많이 생성되었음을 알 수 있었다. 이 결과는 수산화 알루미늄 올리고머가 층간 삽입되어 층간 공간을 확장하고 알루미늄 산화물이 층간에 지주가 되어 기공이 잘 발달하였기 때문인 것으로 생각된다. 또한 OH/Al 몰비가 클수록 층간기둥이 잘 발달되어 기공이 더욱 증가되었음을 알 수 있었다. OH/Al의 비가 큰 수산화 알루미늄 올리고머 용액으로 제조된 Al-pillared clay는 층간 지주들이 많이 생성되므로서 층간 기둥 밀도를 증가시켜 열안정성을 향상시킨 것으로 생각된다.

• 한국대기환경학회지
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• 제26권6호
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• pp.633-648
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• 2010

The study was performed to elucidate the characteristics of VOCs at distinct monitoring sites in urban atmosphere; one is at a roadside in downtown inland city of Jeonju, and the other is at an industrial site in Gunsan near coastal area. The ambient samples were collected for 24 hours in two-bed adsorbent tubes by using MTS-32 sequential tube sampler equipped with Flex air pump every 16 days in a roadside and a industrial complex from February to November in 2009. VOCs were determined by thermal desorption coupled with GC/MSD. Major individual VOCs in roadside samples were shown as following order in magnitude: toluene>m,p-xylene>ethyl benzene>decanal; and those in the industrial complex samples were as follows: toluene>ethanol>ethyl acetate>decanal>m,pxylene. High benzene concentration in the roadside was more frequently occurred than in the industrial complex. However ambient level of toluene in the industrial complex was higher than that in the road side. Results from roadside sample analysis showed that nonane and 1,2,4-trimethylbenzene were very frequently observed with higher concentrations than those in the industrial complex. It seems that nonane and 1,2,4-trimethylbenzene could be the source characteristics for the roadside air. From the diurnal variation, it was found that concentrations of benzene, ethylbenzene, xylene, nonane and 1,2,4-trimethylbenznene in the roadside were higher during rush hours; but those in the industrial complex were higher from 10 to 16 LST when the industrial activities were animated. On weekly base, the concentration of benzene, toluene, ethylbenzene and m,p-xylene in the roadside were higher specifically on Wednesday, but those in the industrial complex were higher on Sunday. It was found that the general trends of VOCs levels at both sites significantly influence on seasonal changes. The results of factor analysis showed that the VOCs in the roadside were mainly affected by the emission of vehicles and the evaporation of diesel fuel, meanwhile those in the industrial complex were influenced by the evaporation of solvents and vehicular emission.