• Title/Summary/Keyword: Phosphate determination

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Separation and Determination of Acteoside in Pedicularis resupinata var. oppositifolia by Ion Pair Liquid Chromatography (이온쌍 액체 크로마토그래피에 의한 마주송이풀 중의 Acteoside의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Analytical Science and Technology
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    • v.8 no.2
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    • pp.161-166
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    • 1995
  • Determination of acteoside in Pedicularis resupinata var. oppositifolia has been studied using ion pair liquid chromatography. Sample was extracted with 40mL methanol for 4 hrs. The extract was cleaned up by using Sep-Pak $C_{18}$ catridge and 8mL aqueous methanol eluent(methanol 50%, water 50%, phosphate buffer pH=8.0). Its determination was performed by means of IP-HPLC with a Hamilton PRP-1 polystyrene-divinylbenzene reversed phase column($15cm{\times}4.6mm$ i. d., $5{\mu}m$) and an aqueous methanol eluent(methanol 60%, water 40% phosphate buffer pH=8.2) containing of $5.0{\times}10^{-3}M$ tetrabutylammonium bromide. The established method was applied to the sample that was collected in area of Pyung Chang gun. As a result, its content ranges showed to be 0.062~0.076%.

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Determination of Tributyl Phosphate Degradation Products by Ion Chromatography (이온크로마토그래피에 의한 Tributyl Phosphate(TBP) 분해산물의 정량)

  • Han, Sun Ho;Lee, Hyo Jin;Yang, Han Beom;Park, Yang Soon;Joe, Kih Soo
    • Analytical Science and Technology
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    • v.15 no.4
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    • pp.329-334
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    • 2002
  • Tributyl phosphate(TBP) is used in solvent extraction process for radioactive waste. This compound may be degraded to dibutyl phosphate($DBP^-$), monobutyl phosphate($MBP^{2-}$) and ${PO_4}^{3-}$ by radioactive material. Amount of $DBP^-$ and $MBP^{2-}$ in TBP must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for $DBP^-$, $MBP^{2-}$, $F^-$, $Cl^-$, ${NO_2}^-$, ${NO_3}^-$, ${SO_4}^{2-}$ and ${PO_4}^{3-}$ are studied with AS4A-SC(Dionex) analytical column and $Na_2CO_3$/NaOH eluent by Ion chromatography. Optimum condition for these anions is 2 mM $Na_2CO_3$/1 mM NaOH eluent. All anions by this condition is well separated within 15min. Dynamic range is $10{\mu}g/mL$ - $100{\mu}g/mL$ for DBP and $5{\mu}g/mL$ - $50{\mu}g/mL$ for $MBP^{2-}$, respectively. The Detection limit for AS4A-SC are $1{\mu}g/mL$ for $DBP^-$ and $0.5{\mu}g/mL$ for $MBP^{2-}$ in this system with a $25{\mu}L$ sample loop.

Spectrophotometric Determination of Submicrogram Amounts of Orthophosphate Suitable for Water Analysis (水質分析을 目的한 極微量燐酸鹽의 高感度比色定量法)

  • Chong Hun Won
    • Journal of the Korean Chemical Society
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    • v.8 no.3
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    • pp.113-120
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    • 1964
  • The critical examination of the spectrophotometric method for determining microgram quantities of phosphate by the n-butyl acetate extraction as molybdophosphoric acid and subsequent development of the molybdenum blue has been made. In this procedure from 2 to 8 ${\mu}g$. of phosphate-phosphorus can be determined under optimum conditions. The final concentration of ammonium molybdate and the final acidity of perchloric acid for the formation of heteropoly acid are suitable to be ranges of 0.5 to 1.1% and 0. 5 to 1. 1 N respectively, and subsequently extracted with 10 ml. of n-butyl acetate. The extract is developed to molybdenum blue with 5.0 ml. of 1. 3% stannous chloride in 1N hydrochloric acid. The color is stable for at least one hour in the use of perchloric acid for the condensation. In order to determination of submicrogram amounts of phosphate, the sensitivity of the molybdenum blue method is hardly sufficient, a sensitive and stable molybdenum(V)-thiocyanate complex method has been investigated. By the procedure less than 1.2 ${\mu}g$. of phosphate-phosphorus can be determined with an accuracy of less than 5% the relative error. The molybdenum(Ⅵ) extracted by the above procedure is reduced to molybdenum(V) in the extract directly with a solution of 4 to 10% of stannous chloride, 0.5 to 1.5 mM of copper, and 0.1 to 0.9 N of perchloric acid as final concentration in 4.3 to 6.3 N of hydrochloric acid or 9.0 to 13.0 N of sulfuric acid by heating for one minute in boiling water, after cooling, the molybdenum(V)-thiocyanate complex color is developed by adding 6.0 M ammonium thiocyanate solution making the final concentration to be in a range of 0.4 to 0.9 M. This procedure the very sensitive, reliable, and stable can be applied to determining submicrogram amounts of phosphate in natural waters with a precision of 1.6 ${\times}\;10^{-2}$ the standard deviation as absorbance.

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Achiral and Chiral Determination of Benzophenanthridine Alkaloids from Methanol Extracts of Hylomecon Species by High Performance Liquid Chromatography

  • Kang, Jong-Seong;Long, Pham-Hoai;Lim, Hwan-Mi;Kim, Young-Ho;Gottfried-Blaschke
    • Archives of Pharmacal Research
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    • v.26 no.2
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    • pp.114-119
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    • 2003
  • A high performance liquid chromatographic (HPLC) method was developed for the qualitative and quantitative determination of benzophenanthridine alkaloids from the methanol extracts of Hylomecon hylomeconoides and H. vernale (Papaveraceae). Achiral and chiral methods were adapted for the separation of 6-methoxydihydrosanguinarine (1), 6-acetonyldihydrosanguinarine (2) and dihydrosanguinarine (3). The achiral reversed phase HPLC method made it possible the simultaneous separation and determination of 1, 2 and 3 within 20 min on ODS column using acetonitrile-phosphate buffer (50 mM, pH 7.0) (50 : 50, v/v). The separation and determination of 1 and 2 enantiomers was available using chiral columns. The same amount of (+) and (-)-enantiomers of 1 was found from the methanol extract of specimen, indicated that 1 could be the artifact produced by the reaction of sanguinarine with methanol. H. hylomeconoides showed higher level of 1 and 3 in compared with H. vernale, especially in root samples permitting the possibility of chemical discrimination between two species.

Adsorption characteristic of Cu(II) and phosphate using non-linear and linear isotherm equation for chitosan bead (비선형과 선형 등온흡착식을 이용한 키토산비드의 구리와 인산염의 흡착특성)

  • Kim, Taehoon;An, Byungryul
    • Journal of Korean Society of Water and Wastewater
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    • v.34 no.3
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    • pp.201-210
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    • 2020
  • 2 (Langmuir, Freundlich, Elovich, Temkin, and Dubinin-Radushkevich) and 3 (Sips and Redlich-Peterson)-parameter isotherm models were applied to evaluated for the applicability of adsorption of Cu(II) and/or phosphate isotherm using chitosan bead. Non-linear and linear isotherm adsorption were also compared on each parameter with coefficient of determination (R2). Among 2-parameter isotherms, non-linear Langmuir and Freundlich isotherm showed relatively higher R2 and appropriate maximum uptake (qm) than other isotherm equation although linear Dubinin-Radushkevich obtained highest R2. 3-parameter isotherm model demonstrated more reasonable and accuracy results than 2-parmeter isotherm in both non-linear and linear due to the addition of one parameter. The linearization for all of isotherm equation did not increase the applicability of adsorption models when error experiment data was included.

Studies on Equilibria and Analytical Applications of Synergistic Solvent Extraction(II). Determination of Trace Lithium in Sea Water using TTA and TOPO

  • Kim, Yeong Sang;Choe, Jong Mun;Lee, Chi U
    • Bulletin of the Korean Chemical Society
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    • v.21 no.9
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    • pp.855-859
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    • 2000
  • An application of synergistic solvent extraction for the etermination of trace lithium in sea water has been studied by forming an adduct complex of thenoyltrifluoroacetone (TTA) and trioctylphosphine oxide (TOPO) in a solvent. The interference by major constituents in sea water was eliminated by phosphate precipitation. Ex-perimental conditions such as solution pH, concentrations of TTA and TOPO etc. were optimized in synthetic sea water with similar compositionto its natural counterpart. To eliminate the interference, 1.38g of ammoni-um dihydrogen phosphate and 2.5 mL of ammonia water were added into 100 mL of thediluted solution at $60^{\circ}C$ to form the phosphate precipitates of Ca2+ and Mg2+ ions. After the pH of this filtrate was adjusted to 8.0, 10.0 mL of m-xylene containing 0.1 M TTA and 0.05 M TOPO was added to the solution in a separatory funnel, and the solution was shaken vigorously for 20 minutes. The solvent was separated from the aqueous solution, and 20 uL of m-xylene solution was injected into a gaphite tube to measure the absorbance by GF-AAS. The detection limit was 0.42 ng/mL. Lithium was determined within the range of 146 to 221 ng/mLin Korean coast-al sea waters, and the recoveries in the spiked samples were 94 to 106%.

The Amounts of the Available Phosphorus in Soils of Kwang-nung Forest (광릉삼림토양의 유효인산량에 관하여)

  • 장남기
    • Journal of Plant Biology
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    • v.11 no.3
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    • pp.18-22
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    • 1968
  • Determination of the pH value and analyses of the available phosphorus of some soils under the forest and grassland Kwang-nung have been examined to study the relationship between the soil pH and available phophorus. The results might be summarized as follows: 1) The available phosphorus decrease steadily as the pH goes up to 5.2. However, at the pH 5.2∼6.3, it shows an increase and decreases again as the rise above pH 6.3. 2) There is a significant difference in the amounts of the soil phosphate among the areas sampled. 3) The statistical analysis of the data obtained shows that soil phosphate is limiting factor governing the distribution of natural vegetal pattern.

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Determination of Epinephrine Using Sodium Iodate in Chemiluminescence

  • Lee, J.S.;Lim, H.B.
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2315-2318
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    • 2007
  • Epinephrine was determined using a lab-made chemiluminescence (CL) system with air pump. Luminolsodium IO4? chemiluminescence system was employed to produce the luminescence of epinephrine. In the reaction, epinephrine was oxidized to produce superoxide or singlet oxygen by periodate in alkaline solution, which enhanced CL of luminol. For optimization, various buffers, such as phosphate, borate, and tris, were studied in this experiment. Compared to NaOH, the phosphate and borate buffer showed better reproducibility with similar sensitivity. Small amount of sample, 22 μL, was required for a measurement. The limit of quantification for epinephrine was obtained to be ~10?9 g/mL after optimization.

Electrochemical Behavior and Differential Pulse Polarographic Determination of Piperacillin Sodium

  • Hahn, Young-hee;Son, Ean-ji
    • Archives of Pharmacal Research
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    • v.23 no.3
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    • pp.197-201
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    • 2000
  • In an aqueous piperacillin sodium solution, a well-defined single wave or single peak was observed by direct current(DC) polarography or differential pulse polarography(DPP). The peak potential change per pH unit was -54 mV in the phosphate buffer at $18^{\circ}C$, which indicated that protons were involved in the electrochemical reduction of the 2,3-dioxopiperazine moiety of piperacillin sodium with a $H^{+}e^{-}$ ratio of one. Using a phosphate buffer of pH 4.3, the $1.0{times}10^{-7}$ M piperacillin sodium single peak could be determined by DPP with relative standard deviation of 1.6 %(n=3). Piperacillin sodium could be analyzed with-out interference from penicillin G-potassium, which enabled the employment of DPP as a fast and simple technique for monitoring the synthetic process of the antibiotic.

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Time-dependent Degradation of Polyphenol Oxidase in Perilla Fructescens Leaves

  • Kim, An-Keun;Kim, Yoo-Kyung
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.142.3-143
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    • 2003
  • Time-dependent PPO activity was determined at $4^\times$C and $30^\times$C. The result of activity determination, PPO extracted by phosphate buffer containing triton x-1l4(tPPO) was more stable than PPO by phosphate buffer(bPPO). The result of electrophoresis, at first a band was appeared at 48kd. After 1-3days a partial degrade band was appeared in bPPO and three partial degrade bands in tPPO. No activity band was appeared in PPOs at $30^\times$C and bPPO at $4^\times$C after 4 days. (omitted)

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