• Analytical Science and Technology
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• v.7 no.4
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• pp.441-453
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• 1994

Two extraction methods, liquid-liquid extraction(LLE) and solid-phase extraction(SPE), coupled with GC/MS were compared as preconcentration procedures for priority pollutants in water. Among the semi-volatile priority pollutants, 11 acid and 44 base/neutral compounds were spiked in reagent water. With LLE, which is a modification of EPA Method 625, the overall mean recovery of the 54 compounds was 91% with a mean relative standard deviation(RSD) of 4.6%. With SPE, the overall mean recovery of the 52 compounds was 53% with a mean RSD of 8.9%. The detection limits of both methods were in the range of $1{\sim}5{\mu}g/l$.

• Journal of Radiation Industry
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• v.5 no.2
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• pp.101-106
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• 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
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• v.53 no.11
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• pp.3798-3807
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• 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
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• v.67
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• pp.109-122
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• 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
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• v.47 no.4
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• pp.389-397
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• 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.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.10 no.1
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• pp.208-222
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• 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
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• v.8 no.4
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• pp.90-97
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• 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
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• v.14 no.10
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• pp.1465-1469
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• 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
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• v.18 no.4
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• pp.996-1000
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• 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
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• v.54 no.3
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• pp.374-379
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• 2016

When using an ionic liquid as co-solvent, the extraction efficiency of anticancer agent paclitaxel from biomass was dramatically improved. However, the residual ionic liquid had a significant negative effect on convenient and feasibility of following concentration and drying steps. In this study, a novel method was developed for the effective drying of the crude extract obtained from biomass extraction with ionic liquid. The residual ionic liquid was easily and conveniently removed by drying alone after pre-treatment and additional washing of a sample with water. The optimal crude extract/water ratio and mixing time for pre-treatment and crude extract/water ratio for additional washing were 1:70 (w/v), 4 min, and 1:100 (w/v), respectively. In the microwave-assisted drying process, the drying time was 9-fold shorter than in the vacuum oven drying process.