• Polymer(Korea)
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• v.30 no.3
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• pp.210-216
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• 2006

To use the filter materials for selective removal of carbonyl compounds in cigarette mainstream smoke, hydrazine such as 2,4-dinitrophenylhydrazine (2,4-DNPH) and dansylhydrazine (DAH) impregnated adsorbents were prepared with perchloric acid or phosphoric acid as an accelerator in hydrazone formation reaction. Changes of molecular structure and morphology of adsorbents in various of impregnator were investigated by FTIR/ATR and SEM. Impregnation amount caused by reaction time, acid type and impregnation reagent, and the adsorption properties of carbonyl compounds in cigarette mainstream smoke were studied. Amounts of impregnation increased with 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 result indicates that the 2,4-DNPH impregnated polyacrylic adsorbent is applicable to cigarette filter material because of its fast reactivity and porosity.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.42 no.1
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• pp.65-73
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• 2016

Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

• Journal of Korean Society for Atmospheric Environment
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• v.14 no.5
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• pp.519-524
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• 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.

• YAKHAK HOEJI
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• v.31 no.2
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• pp.112-115
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• 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$\mu\textrm{g}$.

• Journal of the Korean Society of Tobacco Science
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• v.27 no.2
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• pp.178-188
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• 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.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.10 no.1
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• pp.126-146
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• 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.

• Journal of Korean Society for Atmospheric Environment
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• v.12 no.2
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• pp.199-209
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• 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.

• Journal of Korean Society for Atmospheric Environment
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• v.22 no.2
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• pp.201-208
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• 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
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• v.8 no.1
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• pp.1-11
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• 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.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.30 no.1
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• pp.58-66
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• 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.