• Title/Summary/Keyword: liquid recovery

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Sample Pretreatment and HRGC/HRMS Analysis for Determination of Dioxins in Environmental Samples (환경시료 중 다이옥신류의 정량을 위한 시료전처리방법의 개선 및 고분해능 GC/MS 분석에 관한 연구 Ⅰ)

  • Kim, Jin Yeong;Jang, Yun Seok;Lee, Dae Un
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.819-826
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    • 1994
  • This study described a simple, rapid and cost effective analytical technique for the ultra-trace analysis of dioxins in environmental samples. Liquid-Liquid extraction methods were used for the initial extraction and enrichment of the analyte. Subsequent clean-up procedures were achieved by using strong cation exchanger, silica and Florisil cartridges. Extracts were analysed by HRGC/HRMS-SIM. The efficiency of these analytical methods was tested by recovery and selectivity for elimination of interferences such as phenols, pesticides and PCBs in each step. The mean recovery of 1,2,3,4-TCDD spiked at 10 ppt in sea water was about 92(${\pm}$1.6)%. This analytical method was applied to Kwangyang sea water and 4.5pg/L of 2,3,7,8-TCDD was determined.

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Study on Subcritical Water Degradation of RDX Contaminated Soil in Batch and Dynamic Mode (배치형과 연속흐름형에 의한 토양 중 RDX의 아임계 분해특성 비교연구)

  • Choi, Jae-Heon;Lee, Hwan;Lee, Cheol-Hyo;Kim, Ju-Yup;Park, Jeong-Hun;Jo, Young-Tae
    • Journal of Soil and Groundwater Environment
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    • v.20 no.6
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    • pp.95-102
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    • 2015
  • The purpose of this study is to compare the degradation characteristics by subcritical water of RDX contaminated soil using batch mode and dynamic mode devices. First, upon application of RDX contaminated soil, RDX treatment efficiency was increased with increasing the temperature in both modes. At 150℃, the treatment efficiency was 99.9%. RDX degradation efficiency got higher with lower ratio of solid to liquid. However, the treatment efficiency in the dynamic mode tended to be decreased at a certain ratio of solid to liquid or lower. The treatment efficiency was increased when it took longer time for the reactions in both modes. As the results of analysis on concentration of treated water after subcritical water degradation, the RDX recovery rate of dynamic and batch modes at 150℃ was 10.5% and 1.5%, respectively. However, both modes showed very similar recovery rates at 175℃ or higher. RDX degradation products were analyzed in treated water after it was treated with subcritical water. According to the results, RDX degradation mechanism was mostly oxidation reaction and reduction reaction was partially involved. Therefore, it suggested that most of RDX in soil was degraded by oxidation of subcritical water upon extraction. According to this result, it was found that both batch and dynamic modes were very effectively applied in the treatment of explosive contaminated soil.

Validation of an HPLC Analytical Method for Determination of Biogenic Amines in Agricultural Products and Monitoring of Biogenic Amines in Korean Fermented Agricultural Products

  • Yoon, Hyeock;Park, Jung Hyuck;Choi, Ari;Hwang, Han-Joon;Mah, Jae-Hyung
    • Toxicological Research
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    • v.31 no.3
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    • pp.299-305
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    • 2015
  • An HPLC analytical method was validated for the quantitative determination of biogenic amines in agricultural products. Four agricultural foods, including apple juice, Juk, corn oil and peanut butter, were selected as food matrices based on their water and fat contents (i.e., non-fatty liquid, non-fatty solid, fatty liquid and fatty solid, respectively). The precision, accuracy, recovery, limit of detection (LOD) and quantification (LOQ) were determined to test the validity of an HPLC procedure for the determination of biogenic amines, including tryptamine, ${\beta}$-phenylethylamine, putrescine, cadaverine, histamine, tyramine, spermidine and spermine, in each matrix. The LODs and LOQs for the biogenic amines were within the range of 0.01~0.10 mg/kg and 0.02~0.31 mg/kg, respectively. The relative standard deviation (RSD) of intraday for biogenic amine concentrations ranged from 1.86 to 5.95%, whereas the RSD of interday ranged from 2.08 to 5.96%. Of the matrices spiked with biogenic amines, corn oil with tyramine and Juk with putrescine exhibited the least accuracy of 84.85% and recovery rate of 89.63%, respectively, at the lowest concentration (10 mg/kg). Therefore, the validation results fulfilled AOAC criteria and recommendations. Subsequently, the method was applied to the analysis of biogenic amines in fermented agricultural products for a total dietary survey in Korea. Although the results revealed that Korean traditional soy sauce and Doenjang contained relatively high levels of histamine, the amounts are of no concern if these fermented agricultural products serve as condiments.

High Performance Liquid Chromatographic Method for Determination of Metazosulfuron Residue in Representative Crops

  • Lee, Hyeri;Kim, Eunhye;Lee, Young Deuk;Kim, Jeong-Han
    • Korean Journal of Environmental Agriculture
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    • v.32 no.2
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    • pp.128-135
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    • 2013
  • BACKGROUND: This study was performed to develop a single residue analytical method for new herbicide metazosulfuron in crops. METHODS AND RESULTS: Brown rice, apple, mandarin, Kimchi cabbage and soybean were selected as representative crops, and clean-up system, partition solvent and extraction solvent were optimized. Instrumental limit of quantitation (ILOQ), linearity of calibration curve and method limit of quantitation (MLOQ) were determined based on the chromatography and whole procedures. For recovery tests, brown rice, apple, mandarin, Kimchi cabbage and soybean samples were macerated and fortified with metazosulfuron standard solution at three levels (MLOQ, 10 MLOQ and 100 MLOQ). And then those were extracted with acetonitrile, concentrated, and partitioned with ethyl acetate. Then the extracts were concentrated again and cleaned-up through $NH_2$ (aminopropyl) SPE cartridge with acetone : dichloromethane (1% acetic acid) (20 : 80, v/v) before concentration and analysis with HPLC. CONCLUSION(S): ILOQ of metazosulfuron was 2 ng (S/N${\geq}$10) and good linearity was achieved between 0.05 and 12.5 mg/Kg of metazosulfuron standard solutions, with coefficients of determination of 0.9999. MLOQ was 0.02 mg/Kg. Good recoveries from 74.1 to 116.9% with coefficients of variation (C.V.) of less than 10% were obtained, regardless of sample type, which satisfies the criteria of Korea Food and Drug Administration (KFDA). Those results were reconfirmed with LC-MS (SIM). The method established in this study is simple, economic and efficient to be applied to most of crops as an official and general method for residue analysis of metazosulfuron.

Application of Solvent Extraction to the Treatment of Industrial Wastes

  • Shibata, Junji;Yamamoto, Hideki
    • Proceedings of the IEEK Conference
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    • 2001.10a
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    • pp.259-263
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    • 2001
  • There are several steps such as slicing, lapping, chemical etching and mechanical polishing in the silicon wafer production process. The chemical etching step is necessary to remove damaged layer caused In the slicing and lapping steps. The typical etching liquor is the acid mixture comprising nitric acid, acetic acid and hydrofluoric acid. At present, the waste acid is treated by a neutralization method with a high alkali cost and balky solid residue. A solvent extraction method is applicable to separate and recover each acid. Acetic acid is first separated from the waste liquor using 2-ethlyhexyl alcohols as an extractant. Then, nitric acid is recovered using TBP(Tri-butyl phosphate) as an extractant. Finally hydrofluoric acid is separated with the TBP solvent extraction. The expected recovered acids in this process are 2㏖/l acetic acid, 6㏖/1 nitric acid and 6㏖/l hydrofluoric acid. The yields of this process are almost 100% for acetic acid and nitric acid. On the other hand, it is important to recover and reuse the metal values contained in various industrial wastes in a viewpoint of environmental preservation. Most of industrial products are made through the processes to separate impurities in raw materials, solid and liquid wastes being necessarily discharged as industrial wastes. Chemical methods such as solvent extraction, ion exchange and membrane, and physical methods such as heavy media separation, magnetic separation and electrostatic separation are considered as the methods for separation and recovery of the metal values from the wastes. Some examples of the application of solvent extraction to the treatment of wastes such as Ni-Co alloy scrap, Sm-Co alloy scrap, fly ash and flue dust, and liquid wastes such as plating solution, the rinse solution, etching solution and pickling solution are introduced.

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Organosolv Pretreatment of Slurry Composting and Biofiltration of Liquid Fertilizer-Treated Yellow Poplar for Sugar Production

  • Kim, Ho-Yong;Gwak, Ki-Seob;Jang, Soo-Kyeong;Ryu, Keun-Ok;Yeo, Hwanmyeong;Choi, In-Gyu
    • Journal of the Korean Wood Science and Technology
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    • v.43 no.5
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    • pp.578-590
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    • 2015
  • The present study examines the influence of slurry composting and biofiltration liquid fertilizer (SCBLF) treatment on the biomass characteristics of yellow poplar, and the optimization of organosolv pretreatment for sugar production. After SCBLF treatment, total exchangeable cation contents of yellow poplar was increased from $3.1g\;kg^{-1}$ to $4.4g\;kg^{-1}$, and as a result, biomass production of yellow poplar was also enhanced by 82.3%. Organosolv pretreatment was conducted with three independent variables: 1) reaction temperature: $133.2^{\circ}C$ to $166.8^{\circ}C$; 2) acid concentration: 0.2% to 1.8%; and 3) reaction time: 1.6 min to 18.4 min. Reaction temperature was the most significant variable in water insoluble solid (WIS) recovery rate. High overall sugar yield was attained from pretreatment conditions approximately 50% of WIS recovery rate, and the highest overall glucose yield (44.0%) was achieved from pretreatment at $140^{\circ}C$ with 1.5% acid concentration for 5 min. Consequently, 21.1% of glucose and 5.8% of xylose were produced from the organosolv pretreatment of SCBLF-treated 8-year-old yellow poplar.

A Study on the Simultaneous Determination of Residual Zeranol, Zearalenone and Their Metabolites in Beef by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry에 의한 우육 중의 잔류 Zeranol, Zearalenone 및 그 대사산물들의 동시 분석법에 대한 연구)

  • 이은섭;이용욱
    • Journal of Food Hygiene and Safety
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    • v.9 no.1
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    • pp.1-13
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    • 1994
  • A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

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The effect of relative humidity on the performance of DNPH-cartridge sampling for odorous aldehydes (악취성 Carbonyl 화합물의 카트리지 채취 분석: 습도가 채취효율에 미치는 영향)

  • Lee, Min-Hee;Kim, Ki-Hyun
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.50-59
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    • 2012
  • In this study, the effect of humidity change on DNPH cartridge sampling efficiency for carbonyl compounds (CCs) has been investigated. For this analysis, gaseous standard of 6 different CCs (formaldehyde (FA), acetaldehyde (AA), propionaldehyde (PA), butyraldehyde (BA), isovaleraldehyde (IA), and valeraldehyde (VA)) was calibrated after derivatization with three types of DNPH cartridge products. Their calibration results derived at RH values between 0 and 80% were then compared against liquid phase standards. If the results of our analysis are compared by the RH values between 20 and 80%, the effect of RH can be distinguished between light and heavy CCs. For lighter CCs (like FA and AA), there was no significant change. However, for the ones heavier than PA, there was fairly noticeable increase in relative recovery ratio in RH value between 20 and 80%. Such patterns are seen consistently from all three DNPH products tested for comparison. The results of our analysis suggest that proper correction for RH change may be needed for heavier CCs by the cartridge method.

Analytical Method for Triazine Herbicide Cyanazine Residues in Major Medicinal Crops (주요 약용작물에 대한 Cyanazine 제초제의 잔류 분석법)

  • Hwang, Young Sun;Lim, Jung Dae;Choung, Myoung Gun
    • Korean Journal of Medicinal Crop Science
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    • v.24 no.3
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    • pp.237-245
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    • 2016
  • Background: Cyanazine is used as a pre-emergent herbicide once during the growing season to control weeds of many upland crops worldwide. This study aimed to establish a method to determined cyanazine residue levels in major medicinal crops by using high performance liquid chromatography-UV detection/mass spectometry (HPLC-UVD/MS). Methods and Results: Cyanazine residue was extracted with acetone from the raw products of four representative medicinal plants - Scutellaria baicalensis, Paeonia lactiflora, Platycodon grandiflorum and Angelica gigas. The extract was diluted with a large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. It was then purifined using optimized Florisil column chromatography. HPLC analysis conducted using an octadecylsilyl column allowed the successful separation of cyanazine from co-extractives of the samples, and the amount was sensitively quantified by ultraviolet absorption at 225 nm with no interference. The accuracy and precision of the proposed method were validated by conducting recovery experiments on each medicinal crop sample fortified with cyanazine at two concentration levels per crop in triplicate. Conclusions: The mean recoveries ranged from 91.2% to 105.3% for the four representative medicinal crops. The coefficients of variation were less than 10%, irrespective of the sample types and fortification levels. The limit of quantification of cyanazine was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method was performed by liquid chromatography/MS using selected-ion monitoring technique to clearly identify the suspected residue.

Preculture Condition for Stable Recovery of Strawberry (Fragaria × ananassa Duch.) Shoot Tips after Cryopreservation Using Droplet Vitrification

  • Lee, Young-Yi;Lee, Sun-Yi;Song, Jae-Young;Yoon, Munsup;Yi, Jung-Yoon;Lee, Jung-Ro;Kim, Haeng-Hoon
    • Korean Journal of Plant Resources
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    • v.33 no.6
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    • pp.675-681
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    • 2020
  • This study describes an efficient and stable droplet vitrification following cryopreservation of strawberry shoot tip (Fragaria × ananassa Duch.) accessions 'Massey' and 'MDUS3816'. The shoot tips were precultured in Murashige and Skoog (MS) liquid medium supplemented with sucrose (0.3-0.7M). Precultured explants were osmoprotected with loading solution (LS, C4) containing 17.5% glycerol and 17.5% sucrose for 40 min and exposed to dehydration solution (B1) containing 50% glycerol and 50% sucrose for 40 min at 25oC. Subsequently, the explants were transferred onto droplets containing 2.5 µL PVS3 on sterilized aluminum foils (4 cm× 0.5 cm) prior to direct immersion in liquid nitrogen (LN) for 1 h. The highest regrowth rate (%) in both the cultivars was obtained when the shoot tips were precultured with 0.3M sucrose for 30 h + 0.5M sucrose for 16 h at 25oC. The cryopreserved shoots tips exhibited 57.8 % recovery rate by culturing in NH4NO3-free MS medium supplemented with 3% sucrose, 1.0 g/L casein, 1.0mg/L GA3, and 0.5 mg/L BA for 5 weeks and in MS medium supplemented with 0.5 mg/L GA3 for 8 weeks. Variation was not observed in both of ploidy analysis and morphological investigation on plantlets of two accessions cryopreserved under variable preculture conditions.