• 제목/요약/키워드: titration method

검색결과 258건 처리시간 0.025초

기계적 합금법을 이용한 리튬 2차 전지용 층상 양극물질 $Li[Ni_xCo_{1-2x}Mn_x]O_2$ 의 합성 및 전기화학적 특성에 관한 연구 (Synthesis and electrochemical properties of layered $Li[Ni_xCo_{1-2x}Mn_x]O_2$ materials for lithium secondary batteries prepared by mechanical alloying)

  • 박상호;신선식;선양국
    • 한국결정학회:학술대회논문집
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    • 한국결정학회 2002년도 정기총회 및 추계학술연구발표회
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    • pp.16-16
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    • 2002
  • The presently commercialized lithium-ion batteries use layer structured LiCoO₂ cathodes. Because of the high cost and toxicity of cobalt, an intensive search for new cathode materials has been underway in recent years. Recently, a concept of a one-to-one solid state mixture of LiNO₂ and LiMnO₂, i.e., Li[Ni/sub 0.5/Mn/sub 0.5/]O₂, was adopted by Ohzuku and Makimura to overcome the disadvantage of LiNiO₂ and LiMnO₂. Li[Ni/sub 0.5/Mn/sub 0.5/]O₂ has the -NaFeO₂ structure, which is characteristic of the layered LiCoO₂ and LiNiO₂ structures and shows excellent cycleability with no indication of spinel formation during electrochemical cycling. Layered Li[Ni/sub x/Co/sub 1-2x/Mn/sub x/]O₂ (x = 0.5 and 0.475) materials with high homogeneity and crystallinity were synthesized using a mechanical alloying method. The Li[Ni/sub 0.475/Co/sub 0.05/Mn/sub 0.475/]O₂ electrode delivers a high discharge capacity of 187 mAh/g between 2.8 and 4.6 V at a high current density of 0.3 mA/㎠(30 mA/g) with excellent cycleability. The charge/discharge and differential capacity vs. voltage studies of the Li[Ni/sub x/Co/sub 1-2x/Mn/sub x/]O₂ (x = 0.5 and 0.475) materials showed only one redox peak up to 50 cycles, which indicates that structural phase transitions are not occurred during electrochemical cycling. The magnitude of the diffusion coefficients of lithium ions for Li[Ni/sub x/Co/sub 1-2x/Mn/sub x/]O₂(x = 0.5 and 0.475) are around 10/sup -9/ ㎠/s measured by the galvanostatic intermittent titration technique (GITT).

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동해-삼척지역 석회석의 물리화학적 특성이 탈황성능에 미치는 영향 (Influence of Physicochemical Characteristic of Donghae-Samcheok Limestones on the Performance of Flue Gas Desulfurization (FGD))

  • 서준형;백철승;권우택;조계홍;안지환
    • 자원리싸이클링
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    • 제24권6호
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    • pp.38-44
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    • 2015
  • 동해-삼척지역 석회석을 활용하여 습식배연탈황공정기술에 대한 적용성을 검토하기 위해 석회석의 물리화학적 특성이 탈황성능에 미치는 영향을 연구하였다. 실험은 ASTM 표준 시험방법인 염산적정법을 적용한 실험실 규모의 실험 장치를 이용하여 총중화능력을 측정하였다. 실험결과 총중화능력은 CaO 함량 등의 화학성분 보다 입자크기의 물리적 특성에 더 큰 영향이 있음을 알 수 있었으며, 입자크기가 미립화 될수록 총중화능력의 값은 높아지는 것으로 확인되었다.

란탄족(III)족 이온과 Diaza-18-crown-6-diisopropionic Acid의 착화합물에 관한 연구 (Studies on Complexation of some Lanthanides with Diaza-18-crown-6-diisopropionic Acid)

  • 김정석;이창헌;한선호;서무열;엄태윤;박진하
    • 대한화학회지
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    • 제36권6호
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    • pp.840-848
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    • 1992
  • 이온성 거대고리 리간드, diaza-18-crown-6-diisopropionic acid(K22DAP)를 합성하였다. 이 화합물의 양성자화 상수와 몇 가지 란탄족원소와의 안정도 상수를 전위차적정 방법으로 측정하였다. 양성자화 상수는 log$K_1$ = 9.05, log$K_2$ = 8.37, log$K_3$ = 1.88 및 log$K_4$ = 0.99이고, La(III), Nd(III), Gd(III) 및 Lu(III)와의 안정도 상수 (logKML)는 각각 11.14, 11.43, 11.74 및 10.88이었다. 거대고리 이온운반 물질로서 K22DAP를 사용하고 TTA(thenoyltrifluoroacetone)를 추출제로 하여 란탄(III)족 이온의 추출성질을 연구하였다. pH 8.0의 수상에서 La(III)과 Nd(III)이온은 주로 삼성분착물 Ln(K22DAP)TTA를 형성하였다.

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관능성 단량체로서 Maleic Anhydride를 이용한 Polyolefin의 개질 및 물성 (Modification and Properties of Polyolefin with Maleic Anhydride as a Functional Monomer)

  • 모종헌;이재석;최임철;이원기;박상보;민성기;박찬영
    • Elastomers and Composites
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    • 제47권2호
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    • pp.162-167
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    • 2012
  • 거대분자의 표면개질은 고분자재료의 물성을 향상시키기 위한 점진적이고 바람직한 방안을 제공하며 고분자의 주요 물성을 손상시키지 않고 고분자 표면의 전도도, 젖음성, 안정성, 접착 및 항박테리아성 등을 개선시킨다. PE 또는 PP 등의 polyolefin을 관능성 단량체로서 MAH와 용액상에서 그래프트시켰다. FTIR측정을 통하여 그래프팅이 일어났음을 확인하였다. 그래프팅율은 화학적정에 의하여 결정하였다. MAH량이 많아질수록 접촉각은 낮은 값을 얻었다. 또한 MAH량이 증가함에 따라 polyolefin-g-MAH의 융점($T_m$)은 감소하는 한편 분해온도($T_d$)는 증가하는 경향을 보였다.

Lanthanides-Benzoylformate 착물 형성에 관한 열역학적 연구 (Thermodynamic Properties of Lanthanides Complexes with Benzoylformate Anion)

  • 김영인;박선금
    • 대한화학회지
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    • 제37권4호
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    • pp.442-447
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    • 1993
  • 수용액 내에서 란탄(Ⅲ)-benzoylformate 착물 형성 반응의 열역학적 파라메타들(${\Delta}$G, ${\Delta}$H 및 ${\Delta}$S)을 pH 및 엔탈피 적정 방법을 사용하여 이온세기 $0.1M NaClO_4$, 25$^{\circ}C$ 조건하에서 구하였다. 란탄-benzoylformate 착물의 안정도 상수(1:1) 값으로부터 benzoylformate가 두자리 리간드로 작용함을 알 수 있었다. 열역학적 실험 결과는 카르복실기와 함께 케톤기 산소원자가 결합에 참여하여 킬레이트를형성하는 것으로 판단되었으며, 이는 benzoylformate 리간드 내에 존재하는 벤젠고리의 공액 효과에 의해 케톤기의 산소원자의 전하량이 증가된 결과로 해석되었다. 착물의 안정도는 엔트로피 효과 뿐 아니라, 금속-산소결합 형성에 따른 엔탈피 효과에도 기인하였다.

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Effective Liquid-phase Nitration of Benzene Catalyzed by a Stable Solid Acid Catalyst: Silica Supported Cs2.5H0.5PMo12O40

  • Gong, Shu-Wen;Liu, Li-Jun;Zhang, Qian;Wang, Liang-Yin
    • Bulletin of the Korean Chemical Society
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    • 제33권4호
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    • pp.1279-1284
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    • 2012
  • Silica supported $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ catalyst was prepared through sol-gel method with ethyl silicate-40 as silicon resource and characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy, nitrogen adsorption-desorption and potentiometric titration methods. The $Cs_{2.5}H_{0.5}PMo_{12}O_{40}$ particles with Keggin-type structure well dispersed on the surface of silica, and the catalyst exhibited high surface area and acidity. The catalytic performance of the catalysts for benzene liquid-phase nitration was examined with 65% nitric acid as nitrating agent, and the effects of various parameters were tested, which including temperature, time and amount of catalyst, reactants ratio, especially the recycle of catalyst was emphasized. Benzene was effectively nitrated to mononitro-benzene with high conversion (95%) in optimized conditions. Most importantly, the supported catalyst was proved has excellent stability in the nitration progress, and there were no any other organic solvent and sulfuric acid were used in the reaction system, so the liquid-phase nitration of benzene that we developed was an eco-friendly and attractive alternative for the commercial technology.

Mossbauer Spectroscopic Study of La2-2xSr2xCu1-xFexO4-y(0≤x≤0.5) Solid-solution

  • Park, Jung-Chul;Byeon, Song-Ho;Kim, Don;Lee, Choong-Sub
    • Bulletin of the Korean Chemical Society
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    • 제25권1호
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    • pp.97-100
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    • 2004
  • Tetragonal $K_2NiF_4$-type $La_{2-2x}Sr_{2x}Cu_{1-x}Fe_xO_{4-y}$ solid-solution have been synthesized by citrate based sol-gel method. The valence state of iron was determined by Mossbauer spectroscopy and subsequent iodometric titration clearly showed that the copper ions in this solid-solution are in the mixed valence state Cu(II/III). When x ${\geq}$ 0.3, Fe(III) is competing with the mixture of Cu(II) and Cu(III) and $La_{2-2x}Sr_{2x}Cu_{1-x}Fe_xO_{4-y}$ exhibits a metallic character. No evidence for Cu(II)-O-Fe(IV) ${\leftrightarrow}$ Cu(III)-O-Fe(III) valence degeneracy was observed. In contrast, a small amount of Fe(IV) is observed with increasing x (x = 0.4 and 0.5), revealing a semiconducting behavior. These results suggest that the electronic interaction of Cu(III)-O-Fe(III) contributes greatly to the metallic character, while the electronic interaction of Cu(II)-O-Fe(IV) deteriorates the metallic character of $La_{2-2x}Sr_{2x}Cu_{1-x}Fe_xO_{4-y}$.

pH-Sensitivity Control of PEG-Poly(${\beta}$-amino ester) Block Copolymer Micelle

  • Hwang, Su-Jong;Kim, Min-Sang;Han, Jong-Kwon;Lee, Doo-Sung;Kim, Bong-Sup;Choi, Eun-Kyung;Park, Heon-Joo;Kim, Jin-Seok
    • Macromolecular Research
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    • 제15권5호
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    • pp.437-442
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    • 2007
  • Poly(ethylene glycol) methyl ether (PEG)-poly(${\beta}$-amino ester) (PAE) block copolymers were synthesized using a Michael-type step polymerization, and the construction of pH-sensitive polymeric micelles (PM) investigated. The ${\beta}$-amino ester block of the block copolymers functioned as a pH-sensitive moiety as well as a hydrophobic block in relation to the ionization of PAE, while PEG acted as a hydrophilic block, regardless of ionization. The synthesized polymers were characterized using $^1H-NMR$, with their molecular weights measured using gel permeation chromatography. The $pK_b$ values of the pH-sensitive polymers were measured using a titration method. The pH-sensitivity and critical micelle concentration (CMC) of the block copolymers in PBS solution were estimated using fluorescence spectroscopy. The pH dependent micellization behaviors with various bisacrylate esters varied within a narrow pH range. The critical micelle concentration at pH 7.4 decreased from 0.032 to 0.004 mg/mL on increasing the number of methyl group in the bisacrylate from 4 to 10. Also, the particle size of the block copolymer micelles was determined using dynamic light scattering (DLS). The DLS results revealed the micelles had an average size below 100 nm. These pH-sensitive polymeric micelles may be good carriers for the delivery of an anticancer drug.

Host-Guest Interactions Between Macrocycles and Methylsubstituted Anilinium Ions

  • Lee, Shim-Sung;Jung, Jong-Hwa;Chang, Duk-Jin;Lee, Bu-Yong;Kim, Si-Joong
    • Bulletin of the Korean Chemical Society
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    • 제11권6호
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    • pp.521-527
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    • 1990
  • The binding characteristics and analytical applications of anilinium ion complexes with 18-crown-6 were studied by polarography and NMR. First, the electrochemical reduction of the 10 species of mono and dimethylsubstituted anilinium ion complexes with 18-crown-6 as host in methanol are examined. The addition of 18-crown-6 to anilinium guest solution the polarographic waves remain well defined but shifted toward more negative potentials, indicating the complex formation. The values of formation constants, log Κ for 10 species of methylsubstituted anilinium ion complexes with 18-crown-6 varies from 2.7 to 4.8 in methanol at $25^{\circ}C$. The stability order of complexes for 18-crown-6 is anilinilum > 4-methyl > 3,4-dimethyl > 3-methyl > 3,5-dimethyl > 2,4-dimethyl > 2,5-dimethyl > 2,3-dimethyl > 2-methyl > 2,6-dimethylanilinium ion. The steric hindrance shows significant effect. Second, Proton NMR was used to elucidate their interaction characteristics. From the results of so called NMR titration techniques, the behaviors of binding sites on complexation, and the stoichiometry and stability order of complex were obtained. And the later results show the satisfactory agreement with the quantitative values obtained by polarography. Finally, the individual determinations of anilinium ion mixtures were also accomplished by addition of 18-crown-6. In some mixtures of methyl or dimethylanilinium ions the reduction peaks of differential pulse method appeared into one unresolved wave attributed to the small difference of half-wave potential, ${\Delta}E_{1/2}$. In the presence of 18-crown-6, the polarographic waves were resolved into individual maxima because of the shift toward more negative direction by the difference of selectivity of anilinium ions with 18-crown-6. It may be concluded that quantitative analysis of methylanilinium ion mixture make possible because the half-wave potential shift by the selectivity difference due to the steric hindrance between methyl group and 18-crown-6 on complexation.

해수의 총수소이온농도(pH)와 총알칼리도 측정방법에 대한 선상 비교 연구 (On Board Comparison of Total Hydrogen Ion Concentration (pH) and Total Alkalinity Measurements in Seawater)

  • 강동진;티쉬첸코 파벨;강성현
    • 한국해양환경ㆍ에너지학회지
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    • 제14권3호
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    • pp.205-211
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    • 2011
  • 해수 중의 수소이온농도(pH)와 총알칼리도(TA) 측정 방법에 대한 선상 비교 연구가 동해 표층에서 저층에 이르는 약 550개의 실제 해수 시료에 대해 이루어졌다. 분광광도법과 전위차법에 대한 pH의 비교가 이루어졌으며, 두 방법에 의한 해수의 pH는 전반적으로 잘 일치하였으나, pH가 낮은 심층의 경우 피펫을 사용한 분광법에 의한 값이 전위차법 보다 높은 값을 보였다. 그러나 피펫을 사용하지 않은 분광법과는 두 방법의 정밀도 내에서 동일한 값을 보였다. 이는 피펫에 의해 해수 내의 이산화탄소가 제거되면서 시료 내의 pH를 증가시키는 것으로 판단된다. TA 측정법의 비교를 위해 폐쇄 용기를 이용한 전위차법과 개방 용기를 이용한 전위차법이 사용되었으며, 개방형 용기를 사용했을 때의 값이 폐쇄형 용기를 사용했을 때의 값에 비해 약 5~10 ${\mu}mol\;kg^{-1}$ 작은 값을 보인다. 이는 폐쇄형 용기를 사용했을 때, 적정 도중에 발생하는 이산화탄소가 용액 속에 남아 적정액인 염산 이외의 산을 용액 속에 추가하는 효과를 내기 때문으로 판단된다. 따라서 pH혹은 TA의 분석에 있어서 본 연구에서 비교한 어느 방법을 사용할 수도 있지만 각각의 방법에 대해 특별히 요구되는 주의를 기울일 때 만족할 만한 분석결과를 얻을 수 있다.