• 분석과학
• /
• 제7권4호
• /
• pp.441-453
• /
• 1994

수질에서 유해물질을 농축하는 방법으로 액체 추출법과 고체상 추출법을 GC/MS를 검출기로 사용하여 비교하였다. 비휘발성 유해물질 중 11종의 산과 44종의 염기/중성 화합물들을 reagent water에 첨가하여 분석한 결과, 액체추출법은 54종의 화합물에 대해 91%의 평균회수율과 4.6%의 평균상대표준편차를 나타내었으며, 고체상 추출법은 52종의 화합물에 대해 63%의 평균회수율과 8.9%의 평균상대표준편차를 보였다. 두 방법의 검출한계는 $1{\sim}5{\mu}g/l$였다.

• 방사선산업학회지
• /
• 제5권2호
• /
• pp.101-106
• /
• 2011

The separation of germanium and gallium ion with metal oxide was introduced into the development of $^{68}Ge/^{68}Ga$ generator. Germanium and gallium within mixed solution were respectively separated by using a liquid-liquid extraction and a column chromatographic method. The separation of Ge within high concentrated hydrochloric and sulfuric acid was conducted by the extraction to $CCl_4$ and the back-extraction to 0.05 M HCl. An optimum condition of the extraction by $CCl_4$ was in 5~7 M HCl and efficiency was around 80%. The gallium was selectively separated by using $Al_2O_3$ among metal oxides as sorbents from the mixed solution in 0.04~0.10 M HCl condition.

• Nuclear Engineering and Technology
• /
• 제53권11호
• /
• pp.3798-3807
• /
• 2021

Tritium extraction from radioactively contaminated cement mortar samples was performed using heating and liquid scintillation counting methods. Tritiated water molecules (HTO) can be present in contaminated water along with water molecules (H₂O). Water is one of the primary constituents of cement mortar dough. Therefore, if tritium is present in cement mortar, the buildings and structures using this cement mortar would be contaminated by tritium. The radioactivity level of the materials in the environment exposed to tritium contamination should be determined for their disposal in accordance with the criteria of low-level radioactive waste disposal facility. For our experiments, the cement mortar samples were heated at different temperature conditions using a high-temperature combustion furnace, and the extracted tritium was collected into a 0.1 M nitric acid solution, which was then mixed with a liquid scintillator to be analyzed in a liquid scintillation counter (LSC). The tritium extraction rate from the cement mortar sample was calculated to be 90.91% and 98.54% corresponding to 9 h of heating at temperatures of 200 ℃ and 400 ℃, respectively. The tritium extraction rate was close to 100% at 400 ℃, although the bulk of cement mortar sample was contaminated by tritium.

• Journal of Industrial and Engineering Chemistry
• /
• 제67권
• /
• pp.109-122
• /
• 2018

This work highlights extraction and removal of Lignosulfonate using sunflower oil-Tri-n-octylamine (TOA) system in bulk liquid membrane transport. Maximum extraction and recovery percentages of 92.4% and 75.2% were achieved. Optimum manifold operating conditions were: 4 vol.% TOA, $2{\pm}0.1$ feed phase pH, 300 rpm stirring speed, at $40^{\circ}C$ with 0.2 (M) $Na_2SO_4$ solution. 1:2 (organic/aqueous) and 1:1 (aqueous/aqueous) phase ratios produced best results. Extraction (36.85 kJ/mol) was found to be intermediate controlled and stripping (54.79 kJ/mol) was chemical reaction controlled. Kinetic estimation of data with higher rate constants for stripping vis-${\grave{a}}$-vis extraction showed latter to be rate determining.

• Nuclear Engineering and Technology
• /
• 제47권4호
• /
• pp.389-397
• /
• 2015

The effects of mixing vanes (MVs) attached to a grid spacer on the characteristics of air-water annular flows were experimentally investigated. To know the effects, a grid spacer with or without MV was inserted in a vertical circular pipe of 16-mm internal diameter. For three cases (i.e., no spacer, spacer without MV, and spacer with MV), the liquid film thickness, liquid entrainment fraction, and deposition rate were measured by the constant current method, single liquid film extraction method, and double liquid film extraction method, respectively. The MVs significantly promote the re-deposition of liquid droplets in the gas core flow into the liquid film on the channel walls. The deposition mass transfer coefficient is three times higher for the spacer with MV than for the spacer without MV, even for cases 0.3-m downstream from the spacer. The liquid film thickness becomes thicker upstream and downstream for the spacer with MV, compared with the thickness for the spacer without MV and for the case with no spacer.

• 한국산업보건학회지
• /
• 제10권1호
• /
• pp.208-222
• /
• 2000

This study was conducted to supplement limit of previous study, The objectives of this study were to select optimal conditions of high performance liquid chromatography(HPLC) operation for detecting urinary 2-thiothiazolicline-4-carboxylic acid(TTCA) and thiocarbamide simultaneously, and to evaluate recovery rates for various liquid-liquid extration method of these metabolites, The results are as follows : 1. The urinary TTCA and thiocarbamide were separate sharply when flow rate is $0.7m{\ell}/min$, using a series $C_8$ and $C_{18}$ column, 50 mM $KH_2PO_4$ : acetonitrile (93.5 : 6.5) and pH 3.5 as a mobile phase. The retention time was TTCA, $12.07{\pm}0.11$(mean${\pm}$SD, n=06), thiocarbamide, $7.85{\pm}0.01$ (mean${\pm}$SD, n=6), respectively. The calibration curve for TTCA and thiocarbamide was linear within the range 0.05 to $30{\mu}g/m{\ell}$. 2. By the liquid-liquid extration, butanol extration with $(NH_4)_2$ as a salting-out reagent was used as a simultaneous extration method for these metabolites in acid state, and recovery rates of this method are urinary TTCA, $49.6{\pm}17.7$ (mean${\pm}$SD, n=16), thiocarbamide, $43,9{\pm}5.50$ (mean${\pm}$SD, n=16), respectively 3. The precision(pooled coefficients of variation for 4 concentration) of the urinary thiocarbamide analysis was 0.03754 by butanol liquid-liquid extraction with $(NH_4)_2$ as a salting-out reagent, and TTCA was 0.04082 by ethyl acetate liquid-liquid extration with $(NH_4)_2$ as a salting out reagent The above results show that the butanol liquid-liquid extraction with $(NH_4)_2$ as a salting-out reagent in acid state, and using a series $C_8$ and $C_{18}$ column, 50 mM $KH_2PO_4$ : acetonitrile (93.5 : 6.5) and pH 3.5 as a mobile phase are suitable for the analysis of urinary TTCA and thiocarbamide simultaneously. The detection limit of TTCA and thiocarbamide was about $0.17{\mu}g/m{\ell}$, $0.07{\mu}g/m{\ell}$.

• Mass Spectrometry Letters
• /
• 제8권4호
• /
• pp.90-97
• /
• 2017

Androgenic anabolic steroids (AASs) are synthetic derivatives of testosterone with a common structure containing cyclopentanoperhydrophenanthrene nucleus. Their use enhances the muscle building capacity and is beneficial during performance. The AASs are one of the most abused group of substances in horse doping. Liquid chromatography tandem mass spectrometry ($LC/MS^n$) has been successfully applied to the detection of anabolic steroids in biological samples. However, the saturated hydroxysteroids viz: nandrolone, $5{\alpha}-estrane-3{\beta}$, $17{\alpha}-diol$ exhibit lower detection responses in electrospray ionisation (ESI) because of their poor ionisation efficiency. To overcome this limitation pre-column chemical derivatization has been introduced to enhance their detection responses in $LC-ESI-MS^n$ analysis. The aim of present study was to develop a sensitive method for identification and confirmation of nandrolone and its metabolite in horse urine incorporating pre-column derivatization using picolinic acid. The method consists of extraction of targeted steroid conjugates by solid phase extraction (SPE). The eluted steroid conjugates were hydrolysed by methanolysis and free steroids were recovered with liquid-liquid extraction. The resulting steroids were derivatized to form picolinoyl esters and identification was done using LC-ESI-MS/MS in positive ionization mode. The picolinated steroid adduct enhanced the detection levels in comparison to underivatized steroids.

• Asian-Australasian Journal of Animal Sciences
• /
• 제14권10호
• /
• pp.1465-1469
• /
• 2001

A sensitive high-performance liquid chromatographic method was developed to determine the content of cholesterol in milk and dairy products. To optimize separation of cholesterol, mobile phases including acetonitrile:2-propanol (8:1, v/v), acetonitrile:methanol (3:1, v/v), and acetonitrile:methanoI:2-propanol (7:3: I, v/v/v) were compared. Acetonitrile/methanol/2-propanol was superior to the other mobile phase systems for separating cholesterol. Liquid-liquid extraction (LLE) of cholesterol was simplified using a non-polar solvent, hexane, to remove interfering compounds, and had an excellent recovery $(100{\pm}1.0%)$ of cholesterol. A solid phase extraction (SPE) method using Sep-pak $C_{18}$ was developed and compared with LLE. The SPE method was rapid and highly reproducible. Both extraction methods were useful when used in combination with saponification of esterified cholesterol to facilitate total cholesterol determination. The detection limit of cholesterol was $0.01{\mu}g$. The newly developed HPLC method was rapid, simple, and accurate, and has advantages over the many methods commonly used.

• Food Science and Biotechnology
• /
• 제18권4호
• /
• pp.996-1000
• /
• 2009

Sapium japonicum was extracted by a pressurized liquid. Operating parameters such as the type and the ratio of solvent to water, temperature, pressure, and number of extractions were investigated as the main variables that influence the extraction efficiencies of total phenolics (TP). MeOH extracted the highest level of TP as 50.4 mg GAE/g compared to 48.8 and 27.2 mg GAE/g with $H_2O$ and EtOH, respectively. $EtOH:H_2O$ (40:60, v/v) was found to be the best solvent for TP extraction as 90.3 mg GAE/g compared to 85.0 and 84.3 mg GAE/g in 40:60 and 60:40 of $MeOH:H_2O$, respectively. TP were increased with the increase of the number of extraction steps. TP content was increased by 11% as the extraction temperature was increased from 40 (97.4) to $50{\circ}C$ (108.3 mg GAE/g). The optimum extraction conditions of TP were; extraction solvent, $EtOH:H_2O$ (40:60, v/v); temperature, $50{\circ}C$; pressure, 10.2 MPa; 2 extraction steps.

• Korean Chemical Engineering Research
• /
• 제54권3호
• /
• pp.374-379
• /
• 2016

이온성 액체를 보조용매로 이용할 경우 바이오매스로부터 파클리탁셀의 추출 효율은 획기적으로 개선되지만 잔류 이온성 액체로 후속 농축 및 건조에 많은 어려움이 따른다. 따라서 본 연구에서는 공정 효율 향상을 위하여 이온성 액체를 이용한 바이오매스 추출물을 효과적으로 건조할 수 있는 새로운 방법을 개발하였다. 추출물을 물로 전처리하고 추가적으로 세척함으로써 잔류 이온성 액체 제거를 통해 효과적으로 건조할 수 있었다. 물 전처리을 위한 최적의 시료/물 비, 혼합시간 및 추가세척을 위한 최적의 시료/물 비는 각각 1:70 (w/v), 4분, 1:100 (w/v)이었다. 또한 진공 건조보다 마이크로웨이브를 이용한 건조의 경우 건조시간을 9배 정도 단축 가능하여 공정 효율이 획기적으로 개선될 것으로 판단된다.