• 분석과학
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• 제34권3호
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• pp.128-133
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• 2021

적정 화학반응에는 화학종의 전위차 변화뿐만 아니라 지시약의 색깔 변화도 포함된다. 전위차 적정에서는 종말점에서 전위의 급격한 변화를 측정하여 적정 곡선을 얻는다. 산-염기 적정은 일반적으로 지시약의 색 변화를 관찰하여 종말점을 결정함으로써 수행된다. 전위차를 측정하여 종말점을 결정하는 방법은 잘 확립 되어 상용화되어 있지만 색의 변화를 관찰하여 종말점을 얻는 장치는 많지 않은 실정이다. 적외선 광원과 감지기로 적정액 방울을 계수하고, 백색광원과 광 검출기로 종말점의 변색을 감지하여 아날로그-디지털 변환기인 아두이노 (Arduino)가 적용된 간단하고 정밀한 스펙트럼 종말점 검출 기구를 제작하였다. Spectrator는 지시약으로 티몰 블루를 사용한 산-염기 적정에서 재현성 측면에서 우수한 결과를 보였다. Spectrator 제작 과정과 이를 사용한 실험결과를 공유한다.

• Journal of Photoscience
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• 제9권2호
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• pp.305-307
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• 2002

Spectroscopic titration of D 193N and D 193E mutants of pharaonis phoborhodopsin (ppR) were performed to evaluate the pK$_{a}$ of the Schiff base Asp 193 corresponds to Glu204 of bacteriorhodopsin (bR). The pK$_{a}$ of the Schiff base (SBH$^{+}$) of D193N was 10.1~10.0 (at XH$^{+}$) and 11.4~11.6 (at X) depending on the protonation state of a certain residue (designated by X) and independent on CI$^{[-10]}$ , while those of the wild-type and D193E were> 12. pK$_{a}$ of XH$^{+}$ were; 11.8~11.2 at the state of SB, 10.5 at SBH$^{+}$ state in the presence of CI$^{[-10]}$ , and 9.6 at SBH$^{+}$ without CI$^{[-10]}$ These imply the presence of a long-range interaction in the extracellular channel.r channel.

• Bulletin of the Korean Chemical Society
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• 제27권9호
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• pp.1397-1400
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• 2006

A detailed spectroscopic study ($^1H$ NMR, COSY, ROESY) of complexation of venlafaxine hydrochloride (VEN) with $\beta$-cyclodextrin ($\beta$--CD) was carried out in solution. The stoichiometry of the complex was determined to be 1 : 1 and penetration of aromatic ring into $\beta$-Cyclodextrin cavity was confirmed from primary rim side, with the help of ROESY spectral data. The structure of the venlafaxine hydrochloride-$\beta$-CD complex has been proposed. The association constant was determined to be 234 $M^{-1}$.

• 분석과학
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• 제34권6호
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• pp.267-274
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• 2021

분광학적 검출에 의해 종말점을 확인하는 적정기(Spectrator; SPT)와 기존 적정기(automatic burette; ABT, autotitrator; ATT)를 사용한 분석 결과를 비교하기 위하여 동일한 시료에 대한 산-염기 적정 실험을 수행하였다. 각기 다른 적정장치를 사용하여 얻어진 측정값(종말점)의 직진성, 동등성, ANOVA, F-테스트, t-테스트 등을 통하여 차이점을 통계학 분석을 수행하였으며, 직진성에서 확인된 결정계수는 모두 0.999 이상이고 통계적으로 분석된 결과에 의하여 측정값에 차이가 없다는 귀무가설은 채택되었다. 새로운 실험방법에 대한 일치성을 확인하는 Bland-Altman 분석을 통하여 본 연구에서 사용한 적정장치에서 얻어진 측정값에서 불일치 양상이 확인되지 않았다.

• Macromolecular Research
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• 제12권6호
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• pp.586-592
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• 2004

Poly(glycidyl methacrylate)-grafted polyethylene microbeads (POPM) presenting epoxy groups were prepared by radiation-induced graft polymerization of glycidyl methacrylate on the polyethylene microbead. The obtained POPM was characterized by IR spectroscopic, X-ray photoelectrons spectroscopy (XPS), scanning electron microscope (SEM), and thermal analyses. Furthermore, the abundance of epoxy groups on the POPM was determined by titration and elemental analysis after amination. The epoxy group content was calculated to be in the range 0.29-0.34 mmol/g when using the titration method, but in the range 0.53-0.59 mmol./g when using elemental analysis (EA) after amination. The lipase was immobilized to the epoxy groups of the POPM under various experi­mental conditions, including changes to the pH and the epoxy group content. The activity of the lipase-immobilized POPM was in the range from 160 to 500 unit/mg-min. The activity of the lipase-immobilized POPM increased upon increasing the epoxy group content. The lipase-immobilized POPM was characterized additionally by SEM, elec­tron spectroscopy for chemical analysis (ESCA), and EA.

• Tribology and Lubricants
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• 제35권3호
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• pp.151-157
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• 2019

Insulated oil degradation produces charged by-products, such as acids and hydro-peroxides, which tend to reduce the insulating properties of the oil. In this study, UV-vis spectroscopy measurement technology is developed and experimentally compared with other measurement methods, such as the titration method and IR spectroscopy, to validate its ability to monitor the degradation of electrical insulating paper. The degradation characteristics of the insulating paper are appropriately represented through various types of measurement methods, such as the Tan (delta) method, $CO_2$ gas production measurement, the titration method, and IR spectroscopy. The results are demonstrated to be well comparable to a change in the fluorescence emission ratio (FER), which is defined as the shift in fluorescence intensity in the measured wavelength range, and also to the chromatic ratio, which is defined as a color shift to longer wavelength ranges. The results also show that, by using UV-vis spectroscopy, it is possible to detect the degradation of the insulating paper. This study suggests that UV-vis spectroscopy can be applied as an alternative to high-performance liquid chromatography, which is the internationally recognized measurement technology for cellulose paper degradation. The FER detector is also verified to be useful as an effective condition-monitoring device for power transformers.

• Bulletin of the Korean Chemical Society
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• 제32권3호
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• pp.793-799
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• 2011

We report the complexation behavior of calix[4]arenemonoquinone-triacid (CTAQ), which is an electroactive and water-soluble receptor for calcium ion. UV-visible and NMR spectroscopic studies revealed that CTAQ in aqueous media forms 1:2 as well as 1:1 (metal ion:CTAQ) stoichiometric complexes with $Ca^{2+}$, $Sr^{2+}$, and $Ba^{2+}$ ions. The nonlinear fitting of titration curves based on UV-visible absorption spectra showed that the binding constants of CTAQ for $Ca^{2+}$ ion are 4 $({\pm}2){\times}10^6\;M^{-1}$ for 1:1 and 1.4 $({\pm}0.5){\times}10^{11}\;M^{-2}$ for 1:2 complex. NMR conformational studies and the titration curves corroborate that the $Ca^{2+}$:CTAQ complex in aqueous solution is not present in the form of merely 1:1 one, being consistent with UV-visible spectrophotometric results. The Monte Carlo simulation supports the presence of a stable conformer of 1:2 complexes in which a $Ca^{2+}$ ion is interposed between two CTAQs at the global minimum. This is the first model of 1:2 stoichiometric complex of calix[4]arene and alkaline earth ions in aqueous media.

• Bulletin of the Korean Chemical Society
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• 제18권9호
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• pp.916-922
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• 1997

A superconducting phase La2CuO4+δ (Tc=44 K) has been prepared by electrochemical oxidation which allows the oxygen to intercalat into the La2O2 layers. According to the Cu K-edge X-ray absorption near edge structure spectroscopic analysis, the oxidized phase shows an overall spectra shift of about 0.5 eV to a higher energy region compared to the as sintered one with the occurrence of an additional peak corresponding to the transition to the |1s13dn+1L-14pσ1 > final state, indicating the oxidation of CuO2 layer. From the X-ray photoelectron spectroscopic studies, it is found that the binding energy of La 3d5/2 is significantly shifted from 834.3 eV (as sintered La2CuO4) to 833.6 eV (as electrochemically oxidized La2CuO4+δ), implying that the covalency of the (La-O) bond is decreased due to the oxygen intercalation. The O 1s spectra do not provide an evidence of the superoxide or peroxide, but the oxide (O2-) with the contaminated carbonate (CO32-) based on the peaks at 529 eV and 532 eV, respectively, which is clearly confirmed by the Auger spectroscopic analysis. Oxygen contents determined by iodometric titration (δ=0.07) and thermogravimetry (δ=0.09) show good coincidence each other, also giving an evidence for the "O2-" nature of excess oxygen. From the above results, it is concluded that "O2-" appeared as O 1s peak at 528.6 eV is responsible for superconductivity of La2CuO4+δ.

• International Journal of Safety
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• 제9권1호
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• pp.43-46
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• 2010

In the recycle process of organic solvent, the atmospheric oxygen can cause autoxidation and product peroxide. The time-saving method to evaluate the hazards has been required. In this study, oxygen pressure monitoring experiment was proposed as a new method to evaluate autoxidative resistances of solvents. Some of organic solvents were pressurized by oxygen and kept under isothermal condition. At the same time, the pressure in the vessel tracked. Iodometrical titration, thermal analysis and spectroscopic analysis were performed to measure peroxide concentration, the heat of reaction and chemical bonding change. From the results that THF has larger oxygen consumption rate than CPME, it is considered that autoxidative resistance of THF is lower than that of CPME. This method enables to obtain results in shorter time than other methods. These experimental results were consistent with the previous research with longer test durations [1-2].

• Bulletin of the Korean Chemical Society
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• 제15권11호
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• pp.1001-1003
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• 1994

A series of phosphodiesters of p-nitrophenyl phosphoryl derivatives were synthesized and used as a model substrate for phospholipase D (PLD). The phosphodiester substrates were synthesized from p-nitrophenyl phosphorodichloridate and corresponding alcohols with different chain lengths and polar groups. To measure the activity of PLD, either spectroscopic method for p-nitrophenol or pH-stat titration method was employed. For each substrate, effects of substrate concentration, pH, and $Ca^{2+}$ ion were examined. The kinetic parameters $V_{max}$ for the different substrates were varied depending on the chain lengths or charge of the alcohols. No calcium effect was observed in the hydrolysis of neutral and negatively charged alcohol derivatives, while positively charged choline derivative showed a strong $Ca^{2+}$ ion dependence.