• Title/Summary/Keyword: Chemical extraction

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Electrodeposition of some Alpha-Emitting Nuclides and its Isotope Determination by Alpha Spectrometry (몇가지 알파입자 방출 핵종의 전해석출 및 알파 스펙트럼 측정에 의한 그의 동위원소 정량)

  • Key-Suck Jung;In-Suck Suh
    • Journal of the Korean Chemical Society
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    • v.27 no.4
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    • pp.279-286
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    • 1983
  • An apparatus was made for the electrodeposition of alpha emitting actinide nuclides, $^{207}Bi$ and $^{210}Po$. The electrodeposition was made on a polished stainless steel plate cathode. The anode was made of platinum wire and to stir the solution. With the ammonium chloride as electrolyte initial pH = 4, chloride concentration = 0.6M and solution volume = 15ml, a current of 1.5 ampere(current density = 0.59A/$cm^2$) was flowed for 100 minutes for the quantitative recovery of electrodeposition and on average recovery of 98.3% was obtained within ${\pm}$0.7% uncertainty. Alpha spectrometry of the electrodeposited sample showed alpha peaks from $^{210}Po, ^{234}U$ and $^{239}Pu$ having energy resolution (FWHM) of 18.3, 21.8 and 36.0 keV respectively. The electrodeposition and alpha spectrometry for a natural uranium sample of domestic origin gave $^{238}U : ^{234}U = 1 : 6.1{\times}10^{-5}$ and for a neutron-irradiated uranium sample did $^{238}U : ^{239}Pu : ^{241}Am = 100 : 0.0263 : 5.20{times}10^{-5}$. The result of $^{238}U$ determination in the irradiated sample by electrodeposition-alpha spectrometry was in accord within ${\pm}1.6%$ of relative error with the results of solid fluorimetry and mass spectrometry. For $^{239}Pu$ the result of electrodeposition-alpha spectrometry was in accord within ${\pm}$4.0% of relative error with the results of anion exchange separation and the thenoyltrifluoroacetone(TTA) extraction both followed by alpha spectrometries.

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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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Pattern Recognition of the Herbal Drug, Magnoliae Flos According to their Essential Oil Components

  • Jeong, Eun-Sook;Choi, Kyu-Yeol;Kim, Sun-Chun;Son, In-Seop;Cho, Hwang-Eui;Ahn, Su-Youn;Woo, Mi-Hee;Hong, Jin-Tae;Moon, Dong-Cheul
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1121-1126
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    • 2009
  • This paper describes a pattern recognition method of Magnoliae flos based on a gas chromatographic/mass spectrometric (GC/MS) analysis of the essential oil components. The botanical drug is mainly comprised of the four magnolia species (M. denudata, M. biondii, M. kobus, and M. liliflora) in Korea, although some other species are also being dealt with the drug. The GC/MS separation of the volatile components, which was extracted by the simultaneous distillation and extraction (SDE), was performed on a carbowax column (supelcowax 10; 30 m{\time}0.25 mm{\time}0.25{\mu}m$) using temperature programming. Variance in the retention times for all peaks of interests was within RSD 2% for repeated analyses (n = 9). Of the 74 essential oil components identified from the magnolia species, approximately 10 major components, which is $\alpha$-pinene, $\beta$-pinene, sabinene, myrcene, d-limonene, eucarlyptol (1,8-cineol), $\gamma$-terpinene, p-cymene, linalool, $\alpha$-terpineol, were commonly present in the four species. For statistical analysis, the original dataset was reduced to the 13 variables by Fisher criterion and factor analysis (FA). The essential oil patterns were processed by means of the multivariate statistical analysis including hierarchical cluster analysis (HCA), principal component analysis (PCA) and discriminant analysis (DA). All samples were divided into four groups with three principal components by PCA and according to the plant origins by HCA. Thirty-three samples (23 training sets and 10 test samples to be assessed) were correctly classified into the four groups predicted by PCA. This method would provide a practical strategy for assessing the authenticity or quality of the well-known herbal drug, Magnoliae flos.

Functional Cosmetic Characteristics of Momordica charantia Fruit Extract (여주 열매 추출물의 기능성화장품 소재 특성)

  • Kim, Hyun-Woo;Shin, Hyejin;Hwang, Danbi;Lee, Jieun;Jeong, Hyangli;Kim, Donguk
    • Korean Chemical Engineering Research
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    • v.53 no.3
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    • pp.289-294
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    • 2015
  • In this research, water and ethanol extract of Momordica charantia shells, fruits and seeds were tested to see possibility as natural functional cosmetic agent. Water and ethanol extract showed 69.45 mg/g and 70.87 mg/g polyphenol concentration, respectively. Momordica charantia water and ethanol extracts did not indicate cell toxicity up to $1,000{\mu}g/ml$ concentration in MTT assay. Tyrosinase inhibition effects of water and ethanol extract were lower than arbutin, however, ethanol extract showed better DOPA oxidation inhibition effect than arbutin. Elastase inhibition effects of ethanol extract displayed similar efficacy with adenosine at higher concentrations. Solution formulations (5% extract) were stable for 28 days in both extracts, however, lotion formulation (1% extract) showed considerable variation in viscosity whereas ethanol extraction indicated relative stability. In conclusion, water and ethanol extract of Momordica charantia shells, fruits and seeds indicated strong possibility for whitening and antiwrinkle functional cosmetic ingredient.

Quantification of Entacapone in Human Plasma by HPLC Coupled to ESI-MS/MS Detection: Application to Bioequavalence Study (체외에서 ESI-MS/MS 탐지에 연결된 HPLC에 의한 Entacapon의 수량화: 생물학적 동등성 연구에 적용)

  • Balasekhara Reddy., Ch.;Baburao., Ch.;Chandrasekhar., K.B.;Kanchanamala., K.;RihanaParveen., S.K.;Ravikumar., Konda
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.523-532
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    • 2010
  • The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

Determination of PFOS in LDPE and the Result for Proficiency Testing (LDPE 중 PFOS의 분석법 개발과 비교숙련도 결과)

  • Jung, Jae Hak;Lee, Young Kyu;Myung, Seung Woon;Cheong, Nam Yong
    • Journal of the Korean Chemical Society
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    • v.57 no.1
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    • pp.40-51
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    • 2013
  • In order to develop a quantitation method for Perfluorooctanesulfonic acid(PFOS) contained in plastics that are mainly used in electric and electronic equipment, this study consisted of conducting method validations with LDPE samples using soxhlet solvent extraction and LC/MS. As a result, the limits of detection and quantitation (LOD, LOQ) were $2.58{\mu}g/L$ and $7.82{\mu}g/L$, respectively. Additionally, the recovery was 96-102%. For the correlation coefficient of LC/MS, the $r^2$ value was 0.9992 in the concentration range of $7.82-100{\mu}g/L$, which confirmed its linearity. Furthermore, for the standardization of the analysis method for PFOS in electric and electronic equipment to correspond to EU environmental regulations, we conducted a proficiency test with a number of domestic and international testing laboratories. Three of the ten testing laboratories that participated in the proficiency test submitted outliers. Accordingly, we examined the cause of the outliers using the $^{19}F$ NMR, finding that the main cause was an error in the processing of the results for isomers in PFOS that existed in standard solutions and samples.

A Study on Capillary Gas-Liquid Chromatographic Determination of Diosgenin in Costus Speciosus (모세관 기체-액체 크로마토그래피에 의한 Costus Speciosus 중 Diosgenin의 정량에 관한 연구)

  • Taek Jae Kim;Cha Kee Surk;Kim Young Sang
    • Journal of the Korean Chemical Society
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    • v.30 no.4
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    • pp.369-376
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    • 1986
  • Diosgenin in an Indonesian Costus speciosus was determined by capillary gas-liquid chromatography (GLC). The experimental conditions for the hydrolysis, extraction and acetylation of the diosgenin, and the determination by GLC were investigated. 0.20g of dried sample powder was refluxed in the solution of 3N HCI and xylene at 95∼100${\circ}C$ for 4 hours and the xylene layer was separated. The residue evaporated the xylene was refluxed in 20 : 80 acetic anhydride-pyridine for 30 minutes and the diosgenin acetate was extracted with diethyl ether. Dehydrated with anhydrous $Na_2SO_4$ and evaporated the ether, the residue was dissolved in 5.00ml of n-hexane and injected into GLC. Capillary column of SE-30 25m ${\times}$ 0. 33mm was installed in GLC and the column temperature was increased from 180${\circ}$ to 270${\circ}C$ at rate of 10${\circ}C$/min. The flow rate of carrier gas $N_2$ was 2ml/min and FID was used to detect. The analytical result of the diosgenin was 0.281% and relative standard deviation of 5 measures was 1.8%.

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The Effects of Physico-chemical Properties of soils on PCBs Analysis (토양의 이화학적 특성이 PCBs 분석에 미치는 영향)

  • Kim, Tae-Seung;Shin, Sun-Kyoung;Chang, Jun-Young
    • Analytical Science and Technology
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    • v.16 no.1
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    • pp.48-58
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    • 2003
  • The effects of physico-chemical properties of soils on PCBs analysis in Korea was studied Three kinds of extraction solvents(toluene, acetone:hexane, dichloromethane) was selected to apply three different soils. The silicagel, florisil and alumina column cleanup also performed to compare the elution patterns, and three different methods (EPA, Japan, Proposed method in this study) of 62 PCBs also compared the individual peaks recoveries. The solvent average recovery was surveyed the order of toluene, acetone:hexane, dichloromethane as 77.94%, 58.59%, 54.20% for soil A, 53.65%, 80.32%, 68.27% for soil B and 44.52%, 60.35%, 56.36% for soil C, respectively. The average recovery was depended on the soil characters. The highest recoveries of each soil were obtained the toluene for soil A, acetone:hexane for soil B and C. However, the coplanar PCBs was obtained the highest recovery with dichloromethane. Thus, to select the solvent for the analysis of PCBs in solid, the selected compounds have to consider to get good result. The silicagel, florisil, alumina I and alumina II column cleanup process were surveyed the range of 38.73%~98.26%, and the higher chlorinated compounds was obtained the lower recovery compared to the low chlorinated compounds, generally. This results are also consistent with the coplanar PCBs isomers. The compared results of three different countries were obtained the 37.15% for USA, 45.92% for Japan and 44.46% for proposed method in this study.

Herbicidal Activity of Essential Oil from Palmarosa (Cymbopogon martini) (팔마로사 정유의 살초활성)

  • Hong, Su-Young;Choi, Jung-Sup;Kim, Song-Mun
    • Korean Journal of Weed Science
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    • v.31 no.1
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    • pp.96-102
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    • 2011
  • The objective of this study was to find herbicidal compounds in the essential oil of palmarosa (Cymbopogon martini). Of essential oils from basil (Ocimum basilicum), blackpepper (Piper nigrum), clary sage (Salvia sclarea), ginger (Zingiber pfficinale), hyssop (Hyssopus officinalis), nutmag (Myristica fragrance), palmarosa (Cymbopogon martini), fennel (Foeniculum vulgare), sage (Salvia leucantha), and spearmint (Mentha spicta), the herbicidal activity of palmarosa essential oil, which was determined by a seed bioassay using rapeseed (Brassica napus L.), was highest ($GR_{50}$ value, $201{\mu}g\;mL^{-1}$). In palmarosa essential oil, 11 volatile organic chemicals were identified by gas chromatography-mass spectometry with solid-phase micro-extraction apparatus and the major constituents were geraniol (40.23%), geraniol acetate (15.57%), cis-ocimene (10.79%), and beta-caryophyllene (8.72%). The $GR_{50}$ values of geraniol, citral, nerol, and geranyl acetate were 151, 224, 452, and $1,214{\mu}g\;mL^{-1}$, respectively. In greenhouse and field experiments, foliar application of palmarosa essential oil at the level of $80kg\;ha^{-1}$ controlled weeds effectively. Overall results of this study showed that the herbicidal activity of palmarosa essential oil could be due to geraniol and citral which had lower $GR_{50}$ values.

Differentiation of Sorptive Bindings of Some Radionuclides with Sequential Chemical Extractions in Sandstones (순차적화학추출법을 사용한 방사성핵종의 사암에 대한 수착유형 평가)

  • Park, Chung-Kyun;Hahn, Pil-Soo;Park, Hun-Hwee
    • Nuclear Engineering and Technology
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    • v.26 no.4
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    • pp.461-470
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    • 1994
  • Sorption experiments of $^{60}$ Co, $^{85}$ Sr. and $^{137}$ Cs onto sandstone particles in a batch were carried out to investigate the migration mobility. Sorption kinetics and reversibility as well as sorption mechanisms were examined. Sorption reaction occurred mostly within 10 hours on the outer surface of the sandstone particle but diffusion into the inner surface of the mineral has still occurred after that time. In order to distinguish sorption types of radionuclides, a sequential chemical extraction was introduced. The sorbed radionuclides were then extracted by applying different solutions of synthetic groundwater, CaCl$_2$, KCl and KOX-HA Especially KCl is adopted to extract the ion-exchanged cesium. Sorption types considered are reversible sorption under groundwater condition, ion exchange, association with ferro-manganese oxides or oxyhydroxides, and irreversible fixation. Strontium sorbs onto the sandstone surface mainly by fast and reversible ion exchange reaction. However, cobalt and cesium do not sorb by simple process. The main sorptive binding of cobalt was the association with ferro-manganese oxides and the secondary one was irreversible fixation. Diffusion into the lattice of minerals controlled the sorption rate of cobalt The main sorptin type of cesium was irreversible fixation, while ion exchange reaction was the secondary importance. Hence the oreder of migration mobility for the three radionuclides was Sr$^{2+}$ > Co$^{2+}$ > Cs$^{+}$ in the sandstones.

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