• Title/Summary/Keyword: Perchlorate ion

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Reaction of Thianthrene Cation Radical Perchlorate with Thioxanthene. Synthesis of Thioxanthene Derivatives (티안트렌 양이온 자유라디칼과 염소산염과 티오크잔틴의 반응. 티오크잔틴 유도체의 합성)

  • Kyongtae Kim
    • Journal of the Korean Chemical Society
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    • v.24 no.1
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    • pp.34-43
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    • 1980
  • The reaction of thianthrene cation radical perchlorate with thioxanthene in acetonitrile gave thianthrene and dark reddish thioxanthylium ion instead of thioxanthene cation radical. Addition of aromatic nucleophiles such as anisole, aniline, N,N-diethylaniline, catechol, ethylbenzene, to the above mixture yielded the corresponding thioxanthenes with substituent at 9 position. Reactions with dibenzo-18-crown-6-ether, diphenylmercury, and triphenylphosphine gave similar products. However, reactions with aromatics with electron-withdrawing group were either too slow or inert to such a reaction.

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Structure of a Copper(Ⅱ) Hexaazamacrotricyclic Complex : (1,3,6,9,11,14-Hexaazatricyclo[12.2.1.16,9]octadecane)-copper(Ⅱ) Perchlorate

  • Cheon Manseog;Suh Paik Myunghyun;Shin Whanchul
    • Bulletin of the Korean Chemical Society
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    • v.13 no.4
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    • pp.363-367
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    • 1992
  • The crystal structure of (1,3,6,9,11,14-hexaazatricycol[12.2.1.$1^{6,9}$]octadecane)copper(Ⅱ) perchlorate, Cu($C_{12}H_{26}N_6$)$(ClO_4)_2$, has been determined by the X-ray diffraction methods. The crystal data are as follows: Mr=516.9, triclinic, ${\alpha}=8.572\;(2)$, b=8.499 (3), c=15.204 (3) ${\AA}$, ${\alpha}=80.42\;(5),\;{\beta}=73.57\;(3),\;{\gamma}=69.82\;(4)^{\circ},\;V=994.2\;{\AA}^3,\;D_C=1.726\;gcm^{-3}$, space group $P{\tilde{1}},\;Z=2,\;{\mu}=21.27\;cm^{-1}&, F(000)=534 and T=297 K. The structure was solved by direct methods and refined by full-matrix least-squares methods to and R value of 0.081 for 1608 observed reflections measured with graphite-mono-chromated Mo Ka radiation on a diffractometer. There are two independent complexes in the unit cell. The two copper ions lie at the special positions (1/2, 0, 0) and (0, 1/2, 1/2)and each complex possesses crystallographic center of symmetry. Each Cu ion is coordinated to four nitrogen donors if the hexaazamacrotricyclic ligand and weakly interacts with two oxygen atoms of the perchlorate ions to form a tetragonally distorted octahedral coordination geometry. The Cu_N (sec), Cu_N(tert) and Cu_O coordination distances are 1.985 (14), 2.055 (14) and 2.757 (13) ${\AA}$ for the complex A and 1.996 (10), 2.040 (11) and 2.660 (13) ${\AA}$ for the complex B, respectively. The macrocycles in the two independent cations assume a similar conformation with the average r.m.s. deviation of 0.073 ${\AA}$. Two 1,3-diazacyclopentane ring moieties of the hexaazamacrotricyclic ligand are placed oppositely and almost perpendicularly to the square coordination plane of the ruffled 14-membered macrocycle. The secondary N atoms are hydrogen-bonded to the perchlorate O atoms with distances of 3.017 (23) and 3.025 (19) ${\AA}$ for the complexes A and B, respectively.

Mass Spectrometric Analysis of Eight Common Chemical Explosives Using Ion Trap Mass Spectrometer

  • Park, Sehwan;Lee, Jihyeon;Cho, Soo Gyeong;Goh, Eun Mee;Lee, Sungman;Koh, Sung-Suk;Kim, Jeongkwon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3659-3664
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    • 2013
  • Eight representative explosives (ammonium perchlorate (AP), ammonium nitrate (AN), trinitrotoluene (TNT), 2,4-dinitrotoluene (DNT), cyclonite (RDX), cyclotetramethylenetetranitramine (HMX), pentaerythritol tetranitrate (PETN), and hexanitrostilbene (HNS)) were comprehensively analyzed with an ion trap mass spectrometer in negative ion mode using direct infusion electrospray ionization. MS/MS experiments were performed to generate fragment ions from the major parent ion of each explosive. Explosives in salt forms such as AP or AN provided cluster parent ions with their own anions. Explosives with an aromatic ring were observed as either $[M-H]^-$ for TNT and DNT or $[M]^{{\cdot}-}$ for HNS, while explosives without an aromatic ring such as RDX, HMX, and PETN were detected as an adduct ion with a formate anion, i.e., $[M+HCOO]^-$. These findings provide a guideline for the rapid and accurate detection of explosives once portable MS instruments become more readily available.

Potential of Perchlorate Ion-Selective Electrode in PVC Membrane and Electrode Characteristics by ac Impedance (과염소산 이온선택성 PVC막 전극전위와 임피던스에 의한 전극특성)

  • 김경민;조경섭;강안수
    • Proceedings of the Membrane Society of Korea Conference
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    • 1998.04a
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    • pp.49-52
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    • 1998
  • 1. 서론 : 화약이나 고체 충진제, 고체로\ulcorner 추진제의 산화제, slurry blasting agent 및 동물사료의 식품첨가제로 사용되고 있는 과염소산은 발화나 폭발성이 매우 강한 산화제로 정확한 순도를 측정하는 것은 중요하다. 용량분석법과 중량분석법에 비교하여 조작이 간단하고 편리한 과염소산이온의 농도를 직접 측정할 수 있는 PVC막 전극에 대한 많은 연구가 진행되고 있다. (생략)

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Urea Receptors which Have Both a Fat Brown RR and a Nitrophenyl Group as a Signaling Group

  • Lee, Sung-Kyu;Kang, Jong-Min
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.3031-3033
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    • 2009
  • A new colorimetric anion sensor 1 has been synthesized based on both Fat brown RR dye and a nitrophenyl group. This new receptor 1 could recognize the presence of fluoride ion effectively and selectively by the change of color of solution. In addition, receptor 1 shows higher affinity for acetate, dihydrogenphosphate, and hydrogensulfate than the other anions such as chloride, bromide, iodide, perchlorate, and nitrate in acetonitrile.

Analysis of Inorganic Acids by Capillary Zone Electrophoresis (Capillary Zone Electrophoresis를 이용한 음이온 동시분석에 관한 연구)

  • Park, Sung-Woo;Jin, Kwang-Ho;You, Jae-Hoon;Kim, Dong-Hwan;Seo, Baeseuk;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.213-221
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    • 1998
  • The determination of inorganic anions by capillary zone electrophoresis is reported. A ten component synthetic mixture of anions of bromide, chloride, fluoride, nitrite, nitrate, sulfite, sulfate, perchlorate, chlorate and chlorite was separated by the capillary column and detected by indirect UV method. The running buffer contained 5 mM ammonium dichromate, 10 mM ammonium acetate, 20 mM diethylenetriamine, 10% methanol solution at pH 9.3. A potential of 15 kV at the cathode (reversed polarity) was utilized for the separation of inorganic anions. A complete separation of anions was achieved in less then 10 min and the applicabilities of the method for the analysis of real samples was demonstrated. We compare the concentration of anions in toluene inhaled humen's urine and in postmortem bloods obtained by capillary zone electrophoresis and ion chromatograph.

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Polymeric Iodide-ion Selective Electrodes Based on Urea Derivative as an Ionophore

  • Jeong, Dae-Cheol;Lee, Hyo-Kyoung;Jeon, Seung-Won
    • Bulletin of the Korean Chemical Society
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    • v.27 no.12
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    • pp.1985-1988
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    • 2006
  • The polymeric membrane electrodes based on urea derivative as an ionophore were prepared and studied for the iodide-ion selective electrode. This membrane exhibits a linear stable response over a wide concentration range ($1.0\;{\times}\;10^{-5}\sim1.0\;{\times}\;10^{-2}$) with a slope of -57.7 mV/decade, a detection limit of log[$I^-$] = -5.63, and a selectivity coefficient for iodide against perchlorate anion (log$K^{pot}_{I^-,j}$ = -1.42). The selectivity series of the membrane gives the follow as $I^-$ > $SCN^-$, $Sal^-$ > $ClO_4^-$ > $NO_3^-$ > $Br^-$ > $NO_2^-$ > $Cl^-$ > $F^-$. The proposed electrode showed good selectivity and response for iodide anion over a wide variety of other anions in pH 5.0 buffer solutions.

A Study on Developing the Draft of International Standard for the Determination of Perchlorate in Soil Using Ion Chromatography (이온크로마토그래피를 이용한 토양 중 퍼클로레이트 정량에 관한 국제표준(안) 연구)

  • Choi, Cheon-il;Lee, Goon-taek;Park, Min-ki;Jeong, Moon-ju;Kim, Ji-yang;Kang, Ji-young;Ryu, Ji-young
    • Journal of Soil and Groundwater Environment
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    • v.20 no.6
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    • pp.55-61
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    • 2015
  • Based on the literature study for the determination of perchlorate in soil we chose the ion chromatography as a measurement method and decided to use 70 mM KOH as an eluent to avoid the interference derived from the co-elution of pyrophosphate (P2O74−), tripolyphosphate (P3O105−). Also we proposed to use air dried soil through 0.15 mm sieve and distilled water as an extractant. Under the these basic concepts, we carried out the experiments to set up the detail procedure like solid to liquid ratio (S/L ratio), extraction time, device for extraction and indicating factors for quality control (e.g. precision, accuracy, MDL, LOQ). In case of time and device for extraction, 5 hours of mechanical shaking or 1 hour of centrifugation showed better precision and accuracy than that of sonication for 1 hour According to these results, we proposed the extraction method combining 5 hours of mechanical shaking with 1 hour of centrifugation. From the aspect of S/L ratio, the ratio of 1/2 or 1/3 showed resonable precision and accuracy. In case of the ratio of 1/2, there would be some problems in the separation process when the proportion of fine particle is high. Therefore, we proposed the extraction ratio of solid to liquid as 1/3 instead of 1/2. With the consideration of cost effectiveness and soil salinity, we proposed the use of cartridge for removing the interfering anions like chloride, sulfate and carbonate in specific sample such as saline soil.

Effect of Polyethylene Glycol on Cu Electrodeposition (구리전해도금에서 폴리에틸렌글리콜(polyethylene glycol)의 영향 연구)

  • An, Eui Gyeong;Choi, Sun Gi;Lee, Jaewon;Cho, Sung Ki
    • Journal of the Korean Electrochemical Society
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    • v.25 no.3
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    • pp.113-118
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    • 2022
  • In this study, the effect of polyethylene glycol (PEG) on Cu electrodeposition was analyzed using cyclic voltammetry. The adsorption of PEG was affected by the specific adsorption of sulfate ion (SO42-) or chloride ion (Cl-). In SO42--based plating solution, the adsorption of PEG was limited by the adsorbed SO42-. Accordingly, the adsorbed PEG could suppress the electron transfer for Cu electrodeposition, but its effect was not significant. Meanwhile, in the plating solution composed of perchlorate ion (ClO4-) which does not specifically adsorb on Cu surface, a strong suppression effect of PEG was observed and it was proportional to the molecular weight of PEG. On the other hand, when Cl- was specifically adsorbed on Cu surface, the suppression effect of PEG was enhanced because PEG and Cl- formed an interrelated adsorbate. The synergetic effect of PEG and Cl- depended on the composition of the plating solution, which means that the synergy between PEG and Cl- is based on the physical interaction. For example, the hydrophobicity of PEG plays an important role in the interaction, as the suppression effect of PEG derivative having a hydrocarbon tail was further enhanced with the addition of Cl-.

Self-assembly Coordination Compounds of Cu(II), Zn(II) and Ag(I) with btp Ligands (btp = 2,6-bis(N'-1,2,4-triazolyl)pyridine):Counteranion Effects

  • Kim, Cheal;Kim, Sung-Jin;Kim, Young-Mee
    • Korean Journal of Crystallography
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    • v.16 no.2
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    • pp.107-127
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    • 2005
  • Five Cu(II) compounds were obtained from different copper salts with btp ligands, and their structures were determined by X-ray crystallography. The structure of coordination polymer 2 contains btp-bridged tetranuclear Cu(II) units weakly connected by nitrate ions, and the structure of a discrete Cu(II) molecule 1 contains acetates and btp ligands. With perchlorate anions, two btp ligands bridge Cu(II) ions to form a double zigzag chain 3, while a single zigzag chain 4 is created with sulfate anions. The reaction of $Cu(NO_{3})_{2}$ containing $NH_{4}PF_{6}$ with btp ligands also produced a polymeric compound 5 containing $Cu(H_{2}O)_{2}^{2+}$ and $Cu(NO_{3})_{2}$ units alternatively bridged by btp ligands with H-bonds between copper bonded water and nitrate oxygen atoms. Five Zn(II) compounds were obtained from different zinc salts with btp ligands, and the structures of polymeric compounds (6, 7 and 8) and monomeric compounds (9 and 10) were determined by X-ray crystallography. With nitrate, chloride and bromide anions, btp ligands bridge Zn(II) ions to form polymeric compounds (6, 7 and 8), but btp ligands coordinate to a Zn(II) ion to form monomeric complexes (9 and 10) with $PF_{6}^{-}$ and perchlorate anions. Four silver salts and btp ligands produced two kinds of structures, dinuclear 20-membered rings and one-dimensional zigzag chain depending on different anions. For $ClO_{4}^{-}$ and OTf anions, weak interactions between Ag(I) and anions make dinuclear 20-membered rings construct polymeric compounds (11 and 13). For $PF_{6}^{-}$ anion, there are also weak interactions between Ag(I) and $F(PF_{6}^{-})(12)$, but they do not construct a polymeric compound. For $O_{2}CCF_{3}^{-}$ anion, btp ligands bridge Ag(I) atoms to make one-dimensional zigzag chain (14), and there are also interactions between Ag(I) and anions.