GC/NPD 방식에 기초한 아민류 악취물질의 분석특성 비교 Detection Properties of Malodorous Ami ne Compounds by the Gas Chromatography/Nitrogen Phosphorous Detector (GC/NPD) Method
본 연구에서는 악취성 아민류 화합물에 대한 GC/NPD 방식의 기본적인 검량특성을 평가하고자 하였다. 이를 위해, 3종의 아민화합물들(methyl amine, dimethyl amine, trimethyl amine)을 선정하였다. 그리고 5가지 농도대로 액상표준시료를 준비하여, 검량선을 확보하였다. 이때, 이들 결과를 내부검량방식으로 보기 위하여 pyridine, nitrobenzene, nicotine을 내부표준시료로 첨가하여 활용하였다. 우선, 외부검량방법 중, 부피고정방식(FSV)으로 검량선을 작성한 결과, 분석감도는 TMA > DMA > MTA 순으로 높게 나타나는 것을 확인하였다. 그리고 상관계수 값(r)이 0.97 이상으로 높은 직선성을 보였다. 검량선을 작성할 때, 시료 주입부피의 감소에 따라서 기기분석감도는 matrix 영향으로부터 자유로운 경향(감도증가)을 확인하였다. 반면, 농도고정방식(FSC)으로 구한 검량선에서는 MTA, DMA, TMA 모두 FSV 방법에 대비하여 검량결과의 안정도가 떨어지는 경향을 확인하였다. FSV의 결과를 다시 내부검량방법을 적용한 결과, pyridine 성분을 내부표준물질로 적용하였을 때, 외부검량에 비해 분석의 재현성이 향상하는 것을 확인하였다(예: DMA 75%만큼 향상).
본 연구에서는 악취성 아민류 화합물에 대한 GC/NPD 방식의 기본적인 검량특성을 평가하고자 하였다. 이를 위해, 3종의 아민화합물들(methyl amine, dimethyl amine, trimethyl amine)을 선정하였다. 그리고 5가지 농도대로 액상표준시료를 준비하여, 검량선을 확보하였다. 이때, 이들 결과를 내부검량방식으로 보기 위하여 pyridine, nitrobenzene, nicotine을 내부표준시료로 첨가하여 활용하였다. 우선, 외부검량방법 중, 부피고정방식(FSV)으로 검량선을 작성한 결과, 분석감도는 TMA > DMA > MTA 순으로 높게 나타나는 것을 확인하였다. 그리고 상관계수 값(r)이 0.97 이상으로 높은 직선성을 보였다. 검량선을 작성할 때, 시료 주입부피의 감소에 따라서 기기분석감도는 matrix 영향으로부터 자유로운 경향(감도증가)을 확인하였다. 반면, 농도고정방식(FSC)으로 구한 검량선에서는 MTA, DMA, TMA 모두 FSV 방법에 대비하여 검량결과의 안정도가 떨어지는 경향을 확인하였다. FSV의 결과를 다시 내부검량방법을 적용한 결과, pyridine 성분을 내부표준물질로 적용하였을 때, 외부검량에 비해 분석의 재현성이 향상하는 것을 확인하였다(예: DMA 75%만큼 향상).
In this study, calibration characteristics of odorous amine compounds were investigated by gas chromatography (GC)-nitrogen phosphorous detector (NPD). To this end, three different amine compounds (methyl amine (MTA), dimethyl amine (DMA), and trimethyl amine (TMA)) were analyzed in a series of cali...
In this study, calibration characteristics of odorous amine compounds were investigated by gas chromatography (GC)-nitrogen phosphorous detector (NPD). To this end, three different amine compounds (methyl amine (MTA), dimethyl amine (DMA), and trimethyl amine (TMA)) were analyzed in a series of calibration experiments. As the first step, the liquid phase standards of these amines were calibrated at 5 concentration levels with the fixed standard volume (FSV) method. The results showed that response factors of three amines were in the order of TMA ＞ DMA ＞ MTA with their correlation coefficients (r) above 0.97. The results of FSV calibration also indicated that the analytical sensitivity of amines increased with reducing injection volume due to the decrease in matrix effect. However, when these compounds were calibrated by the fixed standard concentration (FSC) method, the results were not stable under most circumstances. In addition, the reliability of internal calibration approach was also tested using pyridine, nitrobenzene, and nicotine. When pyridine was used as internal standard of these amines, analytical reproducibility of amines was improved greatly compared to external calibration results (e.g., an improvement of 75% for DMA).
In this study, calibration characteristics of odorous amine compounds were investigated by gas chromatography (GC)-nitrogen phosphorous detector (NPD). To this end, three different amine compounds (methyl amine (MTA), dimethyl amine (DMA), and trimethyl amine (TMA)) were analyzed in a series of calibration experiments. As the first step, the liquid phase standards of these amines were calibrated at 5 concentration levels with the fixed standard volume (FSV) method. The results showed that response factors of three amines were in the order of TMA ＞ DMA ＞ MTA with their correlation coefficients (r) above 0.97. The results of FSV calibration also indicated that the analytical sensitivity of amines increased with reducing injection volume due to the decrease in matrix effect. However, when these compounds were calibrated by the fixed standard concentration (FSC) method, the results were not stable under most circumstances. In addition, the reliability of internal calibration approach was also tested using pyridine, nitrobenzene, and nicotine. When pyridine was used as internal standard of these amines, analytical reproducibility of amines was improved greatly compared to external calibration results (e.g., an improvement of 75% for DMA).
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