• 폴리머
• /
• 제30권3호
• /
• pp.210-216
• /
• 2006

담배 주류연 중 카보닐 화합물의 선택적 감소를 위한 필터 물질을 제조하기 위하여 하이드라존 반응에 있어서 촉진제로 사용되는 과염소산과 인산을 2,4-dinitrophenylhydrazine (2,4-DNPH)와 dansylhydrazine (DAH)과 함께 각각의 흡착제에 첨착시켰다. 제조된 첨착 흡착제의 구조는 FTIR/ATR을 이용하여 확인하였으며 SEM을 이용하여 표면을 관찰하였다. 또한 첨착 시간과 촉진제 그리고 첨착 시약에 따른 첨착량과 담배 주류연 중 카보닐 화합물의 흡착특성을 조사하였다. 첨착량은 첨착 시간에 따라 증가되었으며 2.4-DNPH를 첨착한 흡착제의 경우 다른 흡착제에 비해 카보닐 화합물의 제거 효율이 우수하였다. 또한 폴리아크릴계 흡착제에 2,4-DNPH를 첨착시킬 경우 다른 기재의 흡착제에 비해 우수한 제거 효율을 나타내었는데 이러한 결과들로부터 궐련필터로의 적용 가능성을 확인할 수 있었다.

• 대한화장품학회지
• /
• 제42권1호
• /
• pp.65-73
• /
• 2016

대한민국 식품의약품안전처(식약처)는 포름알데하이드 분석법으로 2,4-dinitrophenylhydrazine(DNPH) 유도체화-고성능액체크로마토그래프법(HPLC)을 고시하고 있다. 본 연구는 고시법의 복잡한 시료 전처리 과정을 개선하여 화장품 분석에 편리하게 사용할 수 있는 유도체화법을 개발하고자 수행되었다. 전처리법을 간단하게 하기 위하여 pH, 시간 및 온도 등 반응조건을 최적화하였다. 이 전처리법은 초산염 완충액(pH 5.0)을 사용한 검액의 pH 조정, 디클로로메탄을 사용한 액-액 분획 그리고 감압농축기를 사용한 증발건조와 같이 식약처 고시법의 복잡한 과정이 필요 없다. 유도체화 과정을 통하여 생성된 formaldehyde dinitrophenylhydrazone(formaldehyde-DNP)는 식약처의 시험방법을 약간 변형한 역상 HPLC법으로 분리하고 정량하였다. 2 ~ 40 ppm 농도 범위의 표준액들을 가지고 수행한 검량선 작성 결과, 본 시험법은 상관계수 값이 0.9999로 좋은 직선성을 보여주었다. 본 실험의 최소검출한계(LOD)와 최소정량한계(LOQ)는 각각 0.2 ppm과 0.5 ppm이었다. 또한 회수율 실험결과는 실험방법이 매우 정확하고 재현성이 높음을 보여주었다. 따라서 본 연구에서 제안된 시험법은 화장품 중 포름알데하이드를 신속하게 분석하는데 적용될 수 있을 것이다.

• 한국대기환경학회지
• /
• 제14권5호
• /
• pp.519-524
• /
• 1998

Formaldehyde is known to have adverse health effects, and is also found to be a product of atmospheric. photochemical reaction%. Several methods have been employed for the measurement of formaldehyde. Among them, two common methods are comparatively evaluated in this study, i.e. the chromotropic acid method and the HPLC method coupled with 2,4- dinitrophenylhydrazine (DNPH) derivatization of carbonyl compounds. Method evaluation and validation were performed with respect to repeatability, linearity, collection efficiency, and recovery efficiency. Comparison of formaldehyde concentrations measured simultaneously in the field using the two (n=20) and 35.8%, respectively. Overall, the measured levels by chromotropic acid method appeared to ice significantly higher than those by DNPH-HPLC method, indicating a positive interference due to the other aldehydes collected together with formaldehyde.

• 약학회지
• /
• 제31권2호
• /
• pp.112-115
• /
• 1987

Gypsogenin was derivatized with 2, 4-dinitrophenylhyclrazine prior to analysis with HPLC. Reversed-phase column (Du pont ODS) was used and the mobile phase was acetonitrile and water (60:40). The effluent was detected at 550nm using an U.V. detector and the retention time was approximately 9.2min. The concentration was quantitated by measuring the area and the detection limit was 0.2$\mu\textrm{g}$.

• 한국연초학회지
• /
• 제27권2호
• /
• pp.178-188
• /
• 2005

To use the filter materials for selective removal of carbonyl compounds in cigarette mainstream smoke, hydrazine such as 2,4-dinitrophenylhydrazine and dansylhydraznie impregnated adsorbents were prepared with perchloric acid or phosphoric acid as a accelerator in hydrazone formation reaction. The change of morphology of adsorbents in various of impregnator were investigated by SEM. Impregnation amount caused by reaction time, acid type and impregnation reagent, and the adsorption properties of carbonyl compounds in cigarette mainstream smoke were investigated. Amounts of impregnation was increased as increasing reaction time. The removal amount for vapor phase carbonyl compounds by 2,4-DNPH impregnated adsorbent was higher than that of dansylhydrazine impregnated adsorbent. The selectivity of 2,4-DNPH impregnated polyacrylic type adsorbent was superior to those of other adsorbents. This results indicated that the 2,4-DNPH impregnated polyacrylic adsorbent was applicable to cigarette filter material because of its fast reactivity and porosity.

• 한국산업보건학회지
• /
• 제10권1호
• /
• pp.126-146
• /
• 2000

To develop and evaluate formaldehyde measurement method using 2,4-dinitro-phenylhydrazine (2,4-DNPH) coated sampler and gas chromatography, laboratory test and field test were conducted. Results of this study are as follows. Limit of detection(LOD) of measurement methods, HPLC-UVD, GC-NPD and GC-FID, is $0.008{\mu}g/m{\ell}$ $0.060{\mu}g/m{\ell}$, $0.472{\mu}g/m{\ell}$ respectively. Coefficiency of measurement methods, HPLC-UVD, GC-NPD and GC-FID, is 0.008, 0.009, 0.020 respectively. Desorption efficiency of sep-pak xposure aldehyde sampler and sorbent sample tube is 1.05(range : 0.99 - 1.12), 1.02(range : 0.99 - 1.06) respectively. Samples of sorbent sample tube and sep-pak xposure aldehyde sampler turned out to be stored at refrigerator, according to storage test results. Measurement methods of HPLC-UVD, GC-NPD, GC-FID, according to results of precision for the combined sampling and analytical procedure, became acceptable to OSHA evaluation standard. Field test using exposure chamber met the NIOSH overall uncertainty recommendation(less than 25%). Overall uncertainty of Sepak-HPLC(UVD), Tube-GC(NPD), Tube-GC(FID) is 11.0% - 17.0%. Consequently gas chromatography(GC-NPD, GC-FID) and high performance liquid chromatography(EPA TO-11) using 2,4-DNPH coated sampler for formaldehyde measurement turned out to be suitable to measure personal formaldehyde exposure at workplaces.

• 한국대기환경학회지
• /
• 제12권2호
• /
• pp.199-209
• /
• 1996

The purpose of this study is to evaluate analytical method for the measurement of carbonyl compounds and to apply method to the measurement of indoor and outdoor concentrations of these compounds at public facilities. For sampling, 2.4-dinitrophenylhydrazine (DNPH) coated DNPH-Silica cartridges were uwed in this study. DNPH reacts with carbonyl compounds and forms carbonyl hydrazone, The carbonyl hydarzone was eluted from the cartridge with acetonitrile and analyzed by reverse-phase HPLC with UV detection. Possible interference caused by ozone during sampling was eliminated by using KI trap commected in series with the DNPH-Silica cartridge. A number of experimental studies were undertaken to evaluate and validate the analytical method, including collection efficiency, recovery, repeatability, lower limits of detection, and effect of ozone. Indoor and outdoor measurements of carbonyl compounds were simultaneously carried out at 14 public facilities located in Taegu city and Kyungsan city from June to July, 1995. Except for one or two sites, the indoor concentrations were found to be higher than the outdoor concentrations for carbonyl compounds. And the concentrations of carbonyl compounds measured in the morning and afternoon were showed higher than the concentrations measured in the evening.

• 한국대기환경학회지
• /
• 제22권2호
• /
• pp.201-208
• /
• 2006

Several carbonyl compounds are important because of their irritant and toxic properties, mutagenicity and carcinogenicity. Therefore, they are regulated in korean odor emission standard. In this study, atmospheric pressure ionization-mass spectrometry(API-MS) is used for the analysis of carbonyl compounds after derivatization with 2, 4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation. In the negative ion mode, the $[M-H]^-$ pseudomolecular ions are most abundant for the carbonyls. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearities ($r^2$) for carbonyls were $0.9977{\sim}0.9999$ when analyte concentration ranges from $25\;to\;250{\mu}g/L$(n=6). The relative standard deviations (%RSD) for carbonyls were $0.55{\sim}3.51%$ for concentration of $100{\mu}g/L$(n=5). The minimum detection limit (MDL) was $1.88{\mu}g/L$(0.27 ppb) for i-valeraldehyde. It was shown that LC-MS method has a great potential for carbonyl compounds analysis.

• Advances in nano research
• /
• 제8권1호
• /
• pp.1-11
• /
• 2020

In order to develop a new adsorbent for removal of formaldehyde from aqueous solution, surface modification of TiO₂ nanoparticles was performed with 2,4-Dinitrophenylhydrazine (DNPH) that have a strong affinity to the formaldehyde. Sodium dodecyl sulfate (SDS) surfactant was used to improve the DNPH grafting to TiO₂ surface. Modified adsorbents were characterized by SEM, TEM, XRD, EDX and FTIR. Since the COD level in wastewaters including formaldehyde is considerable, it is necessary to determine the COD content of the synthetic wastewater. In order to determine the optimal removal conditions, the effect of contact time (60-210 min), pH (4-10) and adsorbent dosage (0.5-1.5 g/L) on adsorption and COD removal efficiencies were studied, using response surface method. EDX and FTIR analysis confirmed the presence of nitrogen-containing functional groups on the modified TiO₂ surface. The maximum formaldehyde adsorption and COD removal efficiencies by modified TiO₂ were about 15.65 and 7.35% higher than the unmodified nanoparticles respectively. Therefore, the grafting of nano-TiO₂ with DNPH would greatly improve its formaldehyde adsorption efficiency. The optimum conditions determined for a maximum formaldehyde removal of 99.904% and a COD reduction of 94.815% by TiO₂/SDS/DNPH nanocomposites were: adsorbent dosage 1.100 g/L, pH 7.424 and the contact time 183.290 min.

• 한국산업보건학회지
• /
• 제30권1호
• /
• pp.58-66
• /
• 2020

Objectives: The objective of this study was to develop formaldehyde samples for quality control (QC) and to test the applicability of proficiency analytical testing in Korea. Methods: We made formaldehyde samples with certified standard solutions (formaldehyde in water or acetonitrile) and 2,4-dinitrophenylhydrazine (2,4-DNPH)-coated silicagel tubes. Four levels of formaldehyde concentration were tested for storage stability at room temperature and at 4℃ over three months. Analytical proficiency testing was performed with four or 36 institutes. Results: Formaldehyde sample tubes were easily made through the injection of standard solutions and the average efficiencies of recovery were 95-101%. The coefficients of variation (CV) of the formaldehyde samples were 1.39-2.55%. The recovery efficiencies fell between 90% and 110% at the concentration range of 1-10 ㎍/sample over three months storage at refrigerated and room temperature. The CVs were less than 5% in the proficiency analytical testing. By adjusted proficient ranges, 64% of the results of the second proficiency analytical testing were acceptable. Conclusions: The formaldehyde samples made by injection on 2,4-DNPH-coated silicagel tubes were stable and applicable for quality control.