Sample records for solvent extraction operations

  1. SOLVENT EXTRACTION PROCESSES: A SURVEY OF SYSTEMS IN THE SITE PROGRAM

    EPA Science Inventory

    Solvent extraction of contaminated soils, sludges and sediments has been successfully completed at a number ofSuperfund sites. Each commercialized process uses a unique operating system to extract organic contaminants from solids. These operating systems may be classified by the ...

  2. Infusion extractor

    NASA Technical Reports Server (NTRS)

    Chang-Diaz, Franklin R. (Inventor)

    1986-01-01

    This invention relates to an apparatus and method of removing desirable constituents from an infusible material by infusion extraction. A piston operating in a first chamber draws a solvent into the first chamber where it may be heated, and then moves the heated solvent into a second chamber containing the infusible material, where infusion extraction takes place. The piston then moves the solvent containing the extract through a filter into the first chamber, leaving the extraction residue in the second chamber. The method is applicable to operation in low or micro-gravity environments.

  3. Environmental life cycle assessment on the separation of rare earth oxides through solvent extraction.

    PubMed

    Vahidi, Ehsan; Zhao, Fu

    2017-12-01

    Over the past decade, Rare Earth Elements (REEs) have gained special interests due to their significance in many industrial applications, especially those related to clean energy. While REEs production is known to cause damage to the ecosystem, only a handful of Life Cycle Assessment (LCA) investigations have been conducted in recent years, mainly due to lack of data and information. This is especially true for the solvent extraction separation of REEs from aqueous solution which is a challenging step in the REEs production route. In the current investigation, an LCA is carried out on a typical REE solvent extraction process using P204/kerosene and the energy/material flows and emissions data were collected from two different solvent extraction facilities in Inner Mongolia and Fujian provinces in China. In order to develop life cycle inventories, Ecoinvent 3 and SimaPro 8 software together with energy/mass stoichiometry and balance were utilized. TRACI and ILCD were applied as impact assessment tools and LCA outcomes were employed to examine and determine ecological burdens of the REEs solvent extraction operation. Based on the results, in comparison with the production of generic organic solvent in the Ecoinvent dataset, P204 production has greater burdens on all TRACI impact categories. However, due to the small amount of consumption, the contribution of P204 remains minimal. Additionally, sodium hydroxide and hydrochloric acid are the two impactful chemicals on most environmental categories used in the solvent extraction operation. On average, the solvent extraction step accounts for 30% of the total environmental impacts associated with individual REOs. Finally, opportunities and challenges for an enhanced environmental performance of the REEs solvent extraction operation were investigated. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Intensification of extraction of curcumin from Curcuma amada using ultrasound assisted approach: Effect of different operating parameters.

    PubMed

    Shirsath, S R; Sable, S S; Gaikwad, S G; Sonawane, S H; Saini, D R; Gogate, P R

    2017-09-01

    Curcumin, a dietary phytochemical, has been extracted from rhizomes of Curcuma amada using ultrasound assisted extraction (UAE) and the results compared with the conventional extraction approach to establish the process intensification benefits. The effect of operating parameters such as type of solvent, extraction time, extraction temperature, solid to solvent ratio, particle size and ultrasonic power on the extraction yield have been investigated in details for the approach UAE. The maximum extraction yield as 72% was obtained in 1h under optimized conditions of 35°C temperature, solid to solvent ratio of 1:25, particle size of 0.09mm, ultrasonic power of 250W and ultrasound frequency of 22kHz with ethanol as the solvent. The obtained yield was significantly higher as compared to the batch extraction where only about 62% yield was achieved in 8h of treatment. Peleg's model was used to describe the kinetics of UAE and the model showed a good agreement with the experimental results. Overall, ultrasound has been established to be a green process for extraction of curcumin with benefits of reduction in time as compared to batch extraction and the operating temperature as compared to Soxhlet extraction. Copyright © 2017. Published by Elsevier B.V.

  5. Method of infusion extraction

    NASA Technical Reports Server (NTRS)

    Chang-Diaz, Franklin R. (Inventor)

    1989-01-01

    Apparatus and method of removing desirable constituents from an infusible material by infusion extraction, where a piston operating in a first chamber draws a solvent into the first chamber where it may be heated, and then moves the heated solvent into a second chamber containing the infusible material, and where infusion extraction takes place. The piston then moves the solvent containing the extract through a filter into the first chamber, leaving the extraction residue in the second chamber.

  6. Extraction, scrub, and strip test results for the salt waste processing facility caustic side solvent extraction solvent example

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, T. B.

    An Extraction, Scrub, and Strip (ESS) test was performed on a sample of Salt Waste Processing Facility (SWPF) Caustic-Side Solvent Extraction (CSSX) solvent and salt simulant to determine cesium distribution ratios (D(Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams; this data will be used by Parsons to help determine if the solvent is qualified for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations. The extraction D(Cs) measured 12.9, exceeding the required value of 8. This value is consistent with results from previousmore » ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges.« less

  7. Recovery of catechin compounds from Korean tea by solvent extraction.

    PubMed

    Row, Kyung Ho; Jin, Yinzhe

    2006-03-01

    Catechin compounds from Korean green tea as potential sources of anticancer and antioxidant components were target materials in this work. The methodologies of solvent extraction and partition were utilized to recover catechin compounds from green tea. The optimum experimental condition was obtained by optimizing operating factors, such as, the extraction solvent, extraction time and operating temperature. After extracting the green tea with water at 80 degrees C for 40 min, the extract was partitioned with water/chloroform, which was best suited to remove caffeine impurity from the extract. Further, the resulting extract was partitioned water/ethyl acetate to deeply purify the catechin compounds of EGC, EC, EGCG and ECG. The experimental result in this work could be extended to preparative HPLC to obtain EGCG on commercial scale.

  8. Next Generation Solvent Performance in the Modular Caustic Side Solvent Extraction Process - 15495

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Smith, Tara E.; Scherman, Carl; Martin, David

    Changes to the Modular Caustic Side Solvent Extraction Unit (MCU) flow-sheet were implemented in the facility. Implementation included changing the scrub and strip chemicals and concentrations, modifying the O/A ratios for the strip, scrub, and extraction contactor banks, and blending the current BoBCalixC6 extractant-based solvent in MCU with clean MaxCalix extractant-based solvent. During the successful demonstration period, the MCU process was subject to rigorous oversight to ensure hydraulic stability and chemical/radionuclide analysis of the key process tanks (caustic wash tank, solvent hold tank, strip effluent hold tank, and decontaminated salt solution hold tank) to evaluate solvent carryover to downstream facilitiesmore » and the effectiveness of cesium removal from the liquid salt waste. Results indicated the extraction of cesium was significantly more effective with an average Decontamination Factor (DF) of 1,129 (range was 107 to 1,824) and that stripping was effective. The contactor hydraulic performance was stable and satisfactory, as indicated by contactor vibration, contactor rotational speed, and flow stability; all of which remained at or near target values. Furthermore, the Solvent Hold Tank (SHT) level and specific gravity was as expected, indicating that solvent integrity and organic hydraulic stability were maintained. The coalescer performances were in the range of processing results under the BOBCalixC6 flow sheet, indicating negligible adverse impact of NGS deployment. After the Demonstration period, MCU began processing via routine operations. Results to date reiterate the enhanced cesium extraction and stripping capability of the Next Generation Solvent (NGS) flow sheet. This paper presents process performance results of the NGS Demonstration and continued operations of MCU utilizing the blended BobCalixC6-MaxCalix solvent under the NGS flowsheet.« less

  9. Solvent extraction: the coordination chemistry behind extractive metallurgy.

    PubMed

    Wilson, A Matthew; Bailey, Phillip J; Tasker, Peter A; Turkington, Jennifer R; Grant, Richard A; Love, Jason B

    2014-01-07

    The modes of action of the commercial solvent extractants used in extractive hydrometallurgy are classified according to whether the recovery process involves the transport of metal cations, M(n+), metalate anions, MXx(n-), or metal salts, MXx into a water-immiscible solvent. Well-established principles of coordination chemistry provide an explanation for the remarkable strengths and selectivities shown by most of these extractants. Reagents which achieve high selectivity when transporting metal cations or metal salts into a water-immiscible solvent usually operate in the inner coordination sphere of the metal and provide donor atom types or dispositions which favour the formation of particularly stable neutral complexes that have high solubility in the hydrocarbons commonly used in recovery processes. In the extraction of metalates, the structures of the neutral assemblies formed in the water-immiscible phase are usually not well defined and the cationic reagents can be assumed to operate in the outer coordination spheres. The formation of secondary bonds in the outer sphere using, for example, electrostatic or H-bonding interactions are favoured by the low polarity of the water-immiscible solvents.

  10. Infusion Extractor

    NASA Technical Reports Server (NTRS)

    Chang-Diaz, Franklin R.

    1988-01-01

    Apparatus and method of removing desirable constituents from an infusible material by infusion extraction, where a piston operating in a first chamber draws a solvent into the first chamber where it may be heated, and then moves the heated solvent into a second chamber containing the infusible material, and where infusion extraction takes place. The piston then moves the solvent containing the extract through a filter into the first chamber, leaving the extraction residue in the second chamber.

  11. Process for removing halogenated aliphatic and aromatic compounds from petroleum products

    DOEpatents

    Googin, J.M.; Napier, J.M.; Travaglini, M.A.

    1983-09-20

    A process is described for removing halogenated aliphatic and aromatic compounds, e.g., polychlorinated biphenyls, from petroleum products by solvent extraction. The halogenated aliphatic and aromatic compounds are extracted from a petroleum product into a polar solvent by contacting the petroleum product with the polar solvent. The polar solvent is characterized by a high solubility for the extracted halogenated aliphatic and aromatic compounds, a low solubility for the petroleum product and considerable solvent power for polyhydroxy compound. The preferred polar solvent is dimethylformamide. A miscible compound, such as, water or a polyhydroxy compound, is added to the polar extraction solvent to increase the polarity of the polar extraction solvent. The halogenated aliphatic and aromatic compounds are extracted from the highly-polarized mixture of water or polyhydroxy compound and polar extraction solvent into a low polar or nonpolar solvent by contacting the water or polyhydroxy compound-polar solvent mixture with the low polar or nonpolar solvent. The halogenated aliphatic and aromatic compounds and the low polar or nonpolar solvent are separated by physical means, e.g., vacuum evaporation. The polar and nonpolar solvents are recovered from recycling. The process can easily be designed for continuous operation. Advantages of the process include that the polar solvent and a major portion of the nonpolar solvent can be recycled, the petroleum products are reclaimable and the cost for disposing of waste containing polychlorinated biphenyls is significantly reduced. 1 fig.

  12. Process for removing halogenated aliphatic and aromatic compounds from petroleum products

    DOEpatents

    Googin, John M.; Napier, John M.; Travaglini, Michael A.

    1983-01-01

    A process for removing halogenated aliphatic and aromatic compounds, e.g., polychlorinated biphenyls, from petroleum products by solvent extraction. The halogenated aliphatic and aromatic compounds are extracted from a petroleum product into a polar solvent by contacting the petroleum product with the polar solvent. The polar solvent is characterized by a high solubility for the extracted halogenated aliphatic and aromatic compounds, a low solubility for the petroleum product and considerable solvent power for polyhydroxy compound. The preferred polar solvent is dimethylformamide. A miscible compound, such as, water or a polyhydroxy compound, is added to the polar extraction solvent to increase the polarity of the polar extraction solvent. The halogenated aliphatic and aromatic compounds are extracted from the highly-polarized mixture of water or polyhydroxy compound and polar extraction solvent into a low polar or nonpolar solvent by contacting the water or polyhydroxy compound-polar solvent mixture with the low polar or nonpolar solvent. The halogenated aliphatic and aromatic compounds and the low polar or nonpolar solvent are separated by physical means, e.g., vacuum evaporation. The polar and nonpolar solvents are recovered from recycling. The process can easily be designed for continuous operation. Advantages of the process include that the polar solvent and a major portion of the nonpolar solvent can be recycled, the petroleum products are reclaimable and the cost for disposing of waste containing polychlorinated biphenyls is significantly reduced.

  13. Process for removing halogenated aliphatic and aromatic compounds from petroleum products. [Polychlorinated biphenyls; methylene chloride; perchloroethylene; trichlorofluoroethane; trichloroethylene; chlorobenzene

    DOEpatents

    Googin, J.M.; Napier, J.M.; Travaglini, M.A.

    1982-03-31

    A process for removing halogenated aliphatic and aromatic compounds, e.g., polychlorinated biphenyls, from petroleum products by solvent extraction. The halogenated aliphatic and aromatic compounds are extracted from a petroleum product into a polar solvent by contracting the petroleum product with the polar solvent. The polar solvent is characterized by a high solubility for the extracted halogenated aliphatic and aromatic compounds, a low solubility for the petroleum product and considerable solvent power for polyhydroxy compound. The preferred polar solvent is dimethylformamide. A miscible polyhydroxy compound, such as, water, is added to the polar extraction solvent to increase the polarity of the polar extraction solvent. The halogenated aliphatic and aromatic compounds are extracted from the highly-polarized mixture of polyhydroxy compound and polar extraction solvent into a low polar or nonpolar solvent by contacting the polyhydroxy compound-polar solvent mixture with the low polar or nonpolar solvent. The halogenated aliphatic and aromatic compounds in the low polar or nonpolar solvent by physical means, e.g., vacuum evaporation. The polar and nonpolar solvents are recovered for recycling. The process can easily be designed for continuous operation. Advantages of the process include that the polar solvent and a major portion of the nonpolar solvent can be recycled, the petroleum products are reclaimable and the cost for disposing of waste containing polychlorinated biphenyls is significantly reduced. 2 tables.

  14. Remediating pesticide contaminated soils using solvent extraction

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Sahle-Demessie, E.; Meckes, M.C.; Richardson, T.L.

    Bench-scale solvent extraction studies were performed on soil samples obtained from a Superfund site contaminated with high levels of p,p{prime}-DDT, p,p{prime}-DDE and toxaphene. The effectiveness of the solvent extraction process was assessed using methanol and 2-propanol as solvents over a wide range of operating conditions. It was demonstrated that a six-stage methanol extraction using a solvent-to-soil ratio of 1.6 can decrease pesticide levels in the soil by more than 99% and reduce the volume of material requiring further treatment by 25 times or more. The high solubility of the pesticides in methanol resulted in rapid extraction rates, with the systemmore » reaching quasi-equilibrium state in 30 minutes. The extraction efficiency was influenced by the number of extraction stages, the solvent-to-soil ratio, and the soil moisture content. Various methods were investigated to regenerate and recycle the solvent. Evaporation and solvent stripping are low cost and reliable methods for removing high pesticide concentrations from the solvent. For low concentrations, GAC adsorption may be used. Precipitating and filtering pesticides by adding water to the methanol/pesticide solution was not successful when tested with soil extracts. 26 refs., 10 figs., 6 tabs.« less

  15. Extraction, scrub, and strip test results for the solvent transfer to salt waste processing facility

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, T.

    The Savannah River National Laboratory (SRNL) prepared approximately 240 gallons of Caustic-Side Solvent Extraction (CSSX) solvent for use at the Salt Waste Processing Facility (SWPF). An Extraction, Scrub, and Strip (ESS) test was performed on a sample of the prepared solvent using a salt solution prepared by Parsons to determine cesium distribution ratios (D(Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams. This data will be used by Parsons to help qualify the solvent for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations.more » The extraction D(Cs) measured 15.5, exceeding the required value of 8. This value is consistent with results from previous ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges.« less

  16. Extracting organic matter on Mars: A comparison of methods involving subcritical water, surfactant solutions and organic solvents

    NASA Astrophysics Data System (ADS)

    Luong, Duy; Court, Richard W.; Sims, Mark R.; Cullen, David C.; Sephton, Mark A.

    2014-09-01

    The first step in many life detection protocols on Mars involves attempts to extract or isolate organic matter from its mineral matrix. A number of extraction options are available and include heat and solvent assisted methods. Recent operations on Mars indicate that heating samples can cause the loss or obfuscation of organic signals from target materials, raising the importance of solvent-based systems for future missions. Several solvent types are available (e.g. organic solvents, surfactant based solvents and subcritical water extraction) but a comparison of their efficiencies in Mars relevant materials is missing. We have spiked the well characterised Mars analogue material JSC Mars-1 with a number of representative organic standards. Extraction of the spiked JSC Mars-1 with the three solvent methods provides insights into the relative efficiency of these methods and indicates how they may be used on future Mars missions.

  17. METAL EXTRACTION PROCESS

    DOEpatents

    Lewis, G.W. Jr.; Rhodes, D.E.

    1957-11-01

    An improved method for extracting uranium from aqueous solutions by solvent extraction is presented. A difficulty encountered in solvent extraction operations using an organic extractant (e.g., tributyl phosphate dissolved in kerosene or carbon tetrachloride) is that emulsions sometimes form, and phase separation is difficult or impossible. This difficulty is overcome by dissolving the organic extractant in a molten wax which is a solid at operating temperatures. After cooling, the wax which now contains the extractant, is broken into small particles (preferably flakes) and this wax complex'' is used to contact the uranium bearing solutions and extract the metal therefrom. Microcrystalline petroleum wax and certain ethylene polymers have been found suitable for this purpose.

  18. Extraction, Scrub, and Strip Test Results for the Salt Waste Processing Facility Caustic Side Solvent Extraction Solvent Sample

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, T. B.

    An Extraction, Scrub, and Strip (ESS) test was performed on a sample of Salt Waste Processing Facility (SWPF) Caustic-Side Solvent Extraction (CSSX) solvent and salt simulant to determine cesium distribution ratios (D( Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams; this data will be used by Parsons to help determine if the solvent is qualified for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations. The extraction D( Cs) measured 12.5, exceeding the required value of 8. This value is consistent with resultsmore » from previous ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges. This revision was created to correct an error. The previous revision used an incorrect set of temperature correction coefficients which resulted in slight deviations from the correct D( Cs) results.« less

  19. Optimization of solvent extraction of shea butter (Vitellaria paradoxa) using response surface methodology and its characterization.

    PubMed

    Ajala, E O; Aberuagba, F; Olaniyan, A M; Onifade, K R

    2016-01-01

    Shea butter (SB) was extracted from its kernel by using n-hexane as solvent in an optimization study. This was to determine the optima operating variables that would give optimum yield of SB and to study the effect of solvent on the physico-chemical properties and chemical composition of SB extracted using n-hexane. A Box-behnken response surface methodology (RSM) was used for the optimization study while statistical analysis using ANOVA was used to test the significance of the variables for the process. The variables considered for this study were: sample weight (g), solvent volume (ml) and extraction time (min). The physico-chemical properties of SB extracted were determined using standard methods and Fourier Transform Infrared Spectroscopy (FTIR) for the chemical composition. The results of RSM analysis showed that the three variables investigated have significant effect (p < 0.05) on the %yield of SB, with R(2) - 0.8989 which showed good fitness of a second-order model. Based on this model, optima operating variables for the extraction process were established as: sample weight of 30.04 g, solvent volume of 346.04 ml and extraction time of 40 min, which gave 66.90 % yield of SB. Furthermore, the result of the physico-chemical properties obtained for the shea butter extracted using traditional method (SBT) showed that it is a more suitable raw material for food, biodiesel production, cosmetics, medicinal and pharmaceutical purposes than shea butter extracted using solvent extraction method (SBS). Fourier Transform Infrared Spectroscopy (FTIR) results obtained for the two samples were similar to what was obtainable from other vegetable oil.

  20. Green ultrasound-assisted extraction of carotenoids from pomegranate wastes using vegetable oils.

    PubMed

    Goula, Athanasia M; Ververi, Maria; Adamopoulou, Anna; Kaderides, Kyriakos

    2017-01-01

    The objective of this work was to develop a new process for pomegranate peels application in food industries based on ultrasound-assisted extraction of carotenoids using different vegetable oils as solvents. In this way, an oil enriched with antioxidants is produced. Sunflower oil and soy oil were used as alternative solvents and the effects of various parameters on extraction yield were studied. Extraction temperature, solid/oil ratio, amplitude level, and extraction time were the factors investigated with respect to extraction yield. Comparative studies between ultrasound-assisted and conventional solvent extraction were carried out in terms of processing procedure and total carotenoids content. The efficient extraction period for achieving maximum yield of pomegranate peel carotenoids was about 30min. The optimum operating conditions were found to be: extraction temperature, 51.5°C; peels/solvent ratio, 0.10; amplitude level, 58.8%; solvent, sunflower oil. A second-order kinetic model was successfully developed for describing the mechanism of ultrasound extraction under different processing parameters. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Re-refining of waste petroleum by competing solubility characteristics

    NASA Astrophysics Data System (ADS)

    Byars, Michael Steven

    1998-11-01

    The United States produces over 1.3 billion gallons of used oil per year. Of the 1.3 billion gallons about 60% is used as fuel, nearly 20% is dumped into the environment, 13% is placed in landfills, 2% is re-refined into lube oil, and the remaining is either used for other purposes or incinerated. This is a great potential source of lubricating oil. The work presented here is a solvent extraction process using a solvent (highly miscible with the oil) and a co-solvent (slightly miscible with the oil). Extractions using isopropanol, ethanol, methyl tert-butylether and methanol are presented. The criteria used for evaluation of the extraction processes are yield, product viscosity index, and ash percent. The solvent/co-solvent combinations of MTBE and ethanol performed best and had the advantage of a common solvent/co-solvent in all extraction steps. The extraction process that provided the best results was a two step process using a combination solvent of MTBE and ethanol. The used oil was first extracted using MTBE/ethanol. The extracted oil was then contacted with a solvent combination composed of 80% ethanol. This solvent combination extracted the remaining additives from the oil. The recovered oil was nearly 60% by weight with a high viscosity index and no ash content. A preliminary battery limits design and economic analysis of the process was performed. A 500 bbl/day plant would have a capital cost of 1.9 million and an annual operation cost of 310,000. The plant as designed would produce 300 bbl/day of lube feedstock and have an ROI of 19%.

  2. Evaluation of a heat exchanger for use in the Integrated Equipment Test facility solvent-extraction system

    NASA Astrophysics Data System (ADS)

    Lewis, B. E.

    1982-12-01

    The primary decontamination extraction section product (HAP) heat exchanger will be located between the extracting section (HA) and scrubbing section (HS) of centrifugal solvent extraction contactors in the Integrated Equipment Test (IET) facility. The heat exchanger is required to raise the temperature of the organic product stream from the HA contactor from 40 to 500 C. Tests were conducted under prototypic IET operating conditions to determine the head requirements for gravity flow and the overall heat transfer coefficient for the heat exchanger. Results from the tests indicated that the specified heat exchanger would perform satisfactorily under normal operating conditions.

  3. Novel Fluorinated Tensioactive Extractant Combined with Flotation for Decontamination of Extractant Residual during Solvent Extraction

    NASA Astrophysics Data System (ADS)

    Wu, Xue; Chang, Zhidong; Liu, Yao; Choe, Chol Ryong

    2017-12-01

    Solvent-extraction is widely used in chemical industry. Due to the amphiphilic character, a large amount of extractant remains in water phase, which causes not only loss of reagent, but also secondary contamination in water phase. Novel fluorinated extractants with ultra-low solubility in water were regarded as effective choice to reduce extractant loss in aqueous phase. However, trace amount of extractant still remained in water. Based on the high tensioactive aptitude of fluorinated solvent, flotation was applied to separate fluorinated extractant remaining in raffinate. According to the data of surface tension measurement, the surface tension of solution was obviously decreased with the addition of fluorinated extractant tris(2,2,3,3,4,4,5,5-octafluoropentyl) phosphate (FTAP). After flotation, the FTAP dissolved in water can be removed as much as 70%, which proved the feasibility of this key idea. The effects of operation time, gas velocity, pH and salinity of bulk solution on flotation performance were discussed. The optimum operating parameters were determined as gas velocity of 12ml/min, operating time of 15min, pH of 8.7, and NaCl volume concentration of 1.5%, respectively. Moreover, adsorption process of FTAP on bubble surface was simulated by ANSYS VOF model using SIMPLE algorithm. The dynamic mechanism of flotation was also theoretically investigated, which can be considered as supplement to the experimental results.

  4. Effect of the type and level of hydration of alcoholic solvents on the simultaneous extraction of oil and chlorogenic acids from sunflower seed press cake.

    PubMed

    Scharlack, Nayara K; Aracava, Keila K; Rodrigues, Christianne Ec

    2017-10-01

    The present study aimed to evaluate the replacement of hexane by alcoholic solvents in oil extraction from sunflower seed press cake. The use of ethanol and isopropanol has important advantages, including low toxicity and good operational safety. Thus, in the present study, solid-liquid extractions were performed in a single stage from 60 to 90 °C and in consecutive extractions in three stages at 90 °C. Solvent hydration negatively affected the extraction of oil but favored the extraction of chlorogenic acids (CAs), especially when ethanol was used. Regarding oxidative stability, the oils extracted using ethanol presented long induction times, which could be related to the high levels of not only CAs and tocopherols, but also phospholipids. Alcoholic solvents can be used for extraction to produce sunflower seed oil containing minor compounds that give it greater oxidative stability. In addition, the results obtained using hydrous ethanol showed that this solvent can yield defatted sunflower seed meal with a low content of CAs, enabling future use of the protein fraction. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  5. Liquefaction process wherein solvents derived from the material liquefied and containing increased concentrations of donor species are employed

    DOEpatents

    Fant, B. T.; Miller, John D.; Ryan, D. F.

    1982-01-01

    An improved process for the liquefaction of solid carbonaceous materials wherein a solvent or diluent derived from the solid carbonaceous material being liquefied is used to form a slurry of the solid carbonaceous material and wherein the solvent or diluent comprises from about 65 to about 85 wt. % hydroaromatic components. The solvent is prepared by first separating a solvent or diluent distillate fraction from the liquefaction product, subjecting this distillate fraction to hydrogenation and then extracting the naphthenic components from the hydrogenated product. The extracted naphthenic components are then dehydrogenated and hydrotreated to produce additional hydroaromatic components. These components are combined with the solvent or diluent distillate fraction. The solvent may also contain hydroaromatic constituents prepared by extracting naphthenic components from a heavy naphtha, dehydrogenating the same and then hydrotreating the dehydrogenated product. When the amount of solvent produced in this manner exceeds that required for steady state operation of the liquefaction process a portion of the solvent or diluent distillated fraction will be withdrawn as product.

  6. Pressurized liquid extraction of ginger (Zingiber officinale Roscoe) with bioethanol: an efficient and sustainable approach.

    PubMed

    Hu, Jiajin; Guo, Zheng; Glasius, Marianne; Kristensen, Kasper; Xiao, Langtao; Xu, Xuebing

    2011-08-26

    To develop an efficient green extraction approach for recovery of bioactive compounds from natural plants, we examined the potential of pressurized liquid extraction (PLE) of ginger (Zingiber officinale Roscoe) with bioethanol/water as solvents. The advantages of PLE over other extraction approaches, in addition to reduced time/solvent cost, the extract of PLE showed a distinct constituent profile from that of Soxhlet extraction, with significantly improved recovery of diarylheptanoids, etc. Among the pure solvents tested for PLE, bioethanol yield the highest efficiency for recovering most constituents of gingerol-related compounds; while for a broad concentration spectrum of ethanol aqueous solutions, 70% ethanol gave the best performance in terms of yield of total extract, complete constituent profile and recovery of most gingerol-related components. PLE with 70% bioethanol operated at 1500 psi and 100 °C for 20 min (static extraction time: 5 min) is recommended as optimized extraction conditions, achieving 106.8%, 109.3% and 108.0% yield of [6]-, [8]- and [10]-gingerol relative to the yield of corresponding constituent obtained by 8h Soxhlet extraction (absolute ethanol as extraction solvent). Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Hydrometallurgical recovery of germanium from coal gasification fly ash: pilot plant scale evaluation

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Arroyo, F.; Fernandez-Pereira, C.; Olivares, J.

    2009-04-15

    In this article, a hydrometallurgical method for the selective recovery of germanium from fly ash (FA) has been tested at pilot plant scale. The pilot plant flowsheet comprised a first stage of water leaching of FA, and a subsequent selective recovery of the germanium from the leachate by solvent extraction method. The solvent extraction method was based on Ge complexation with catechol in an aqueous solution followed by the extraction of the Ge-catechol complex (Ge(C{sub 6}H{sub 4}O{sub 2}){sub 3}{sup 2-}) with an extracting organic reagent (trioctylamine) diluted in an organic solvent (kerosene), followed by the subsequent stripping of the organicmore » extract. The process has been tested on a FA generated in an integrated gasification with combined cycle (IGCC) process. The paper describes the designed 5 kg/h pilot plant and the tests performed on it. Under the operational conditions tested, approximately 50% of germanium could be recovered from FA after a water extraction at room temperature. Regarding the solvent extraction method, the best operational conditions for obtaining a concentrated germanium-bearing solution practically free of impurities were as follows: extraction time equal to 20 min; aqueous phase/organic phase volumetric ratio equal to 5; stripping with 1 M NaOH, stripping time equal to 30 min, and stripping phase/organic phase volumetric ratio equal to 5. 95% of germanium were recovered from water leachates using those conditions.« less

  8. Subcritical n-hexane/isopropanol extraction of lipid from wet microalgal pastes of Scenedesmus obliquus.

    PubMed

    Bian, Xiaoyu; Jin, Wenbiao; Gu, Qiong; Zhou, Xu; Xi, Yuhe; Tu, Renjie; Han, Song-Fang; Xie, Guo-Jun; Gao, Shu-Hong; Wang, Qilin

    2018-02-19

    Subcritical co-solvents of n-hexane/isopropanol were primarily utilized to extract lipid from wet microalgal pastes of Scenedesmus obliquus. The effects of key operational parameters were investigated, and the optimal parameters were obtained: solvent ratio of n-hexane to isopropanol was 3:2 (V:V), phase ratio of co-solvents to microalgal biomass was 35:1 (mL:g), reactor stirring speed was 900 rpm, extraction time was 60 min. Additional pretreatment with acid, ultrasonic and microwave as well as enhanced subcritical pressure/heating treatments were also applied to further study their effects on lipid extraction. The results showed that the lipid recovery rate with acid pretreatment was 8.6 and 6.2% higher than ultrasonic and microwave pretreatment; the optimum enhanced subcritical condition was 55 °C with atmospheric pressure. Under optimal operating conditions, the lipid and FAME yield were 13.5 and 7.2%, which was 82.6 and 135.1% higher than the traditional method. The results indicated that the subcritical n-hexane/isopropanol extraction process had promising application potential.

  9. Automated process for solvent separation of organic/inorganic substance

    DOEpatents

    Schweighardt, F.K.

    1986-07-29

    There is described an automated process for the solvent separation of organic/inorganic substances that operates continuously and unattended and eliminates potential errors resulting from subjectivity and the aging of the sample during analysis. In the process, metered amounts of one or more solvents are passed sequentially through a filter containing the sample under the direction of a microprocessor control apparatus. The mixture in the filter is agitated by ultrasonic cavitation for a timed period and the filtrate is collected. The filtrate of each solvent extraction is collected individually and the residue on the filter element is collected to complete the extraction process. 4 figs.

  10. Automated process for solvent separation of organic/inorganic substance

    DOEpatents

    Schweighardt, Frank K.

    1986-01-01

    There is described an automated process for the solvent separation of organic/inorganic substances that operates continuously and unattended and eliminates potential errors resulting from subjectivity and the aging of the sample during analysis. In the process, metered amounts of one or more solvents are passed sequentially through a filter containing the sample under the direction of a microprocessor control apparatus. The mixture in the filter is agitated by ultrasonic cavitation for a timed period and the filtrate is collected. The filtrate of each solvent extraction is collected individually and the residue on the filter element is collected to complete the extraction process.

  11. Automated apparatus for solvent separation of a coal liquefaction product stream

    DOEpatents

    Schweighardt, Frank K.

    1985-01-01

    An automated apparatus for the solvent separation of a coal liquefaction product stream that operates continuously and unattended and eliminates potential errors resulting from subjectivity and the aging of the sample during analysis. In use of the apparatus, metered amounts of one or more solvents are passed sequentially through a filter containing the sample under the direction of a microprocessor control means. The mixture in the filter is agitated by means of ultrasonic cavitation for a timed period and the filtrate is collected. The filtrate of each solvent extraction is collected individually and the residue on the filter element is collected to complete the extraction process.

  12. Chemical treatment of low-grade uranium ores. Extraction of uranium from tricalcium phosphate; TRAITEMENT CHIMIQUE DES MINERAIS PAUVRES D'URANIUM. EXTRACTION DE L'URANIUM DU PHOSPHATE TRICALCIQUE (in French)

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Mechelynck, Ph.

    1958-07-15

    After an examination of the different processes for the treatment of uranium minerals, it is concluded that the extraction of uranium by ion exchange is not applicable to hydrochloric acid solutions of phosphates. A sulfuric or phosphoric solution can be used. For solvent extraction of uranium, sulfuric or phosphoric solutions are the best, but hydrochloric solutions can be used. The cost of the solvents used would determine the cost of the operation. It is necessary, in the case of liquid-liquid extraction, to filter or decant the solution before extraction. (tr-auth)

  13. Sugaring-out extraction of acetoin from fermentation broth by coupling with fermentation.

    PubMed

    Dai, Jian-Ying; Ma, Lin-Hui; Wang, Zhuang-Fei; Guan, Wen-Tian; Xiu, Zhi-Long

    2017-03-01

    Acetoin is a natural flavor and an important bio-based chemical which could be separated from fermentation broth by solvent extraction, salting-out extraction or recovered in the form of derivatives. In this work, a novel method named as sugaring-out extraction coupled with fermentation was tried in the acetoin production by Bacillus subtilis DL01. The effects of six solvents on bacterial growth and the distribution of acetoin and glucose in different solvent-glucose systems were explored. The operation parameters such as standing time, glucose concentration, and volume ratio of ethyl acetate to fermentation broth were determined. In a system composed of fermentation broth, glucose (100%, m/v) and two-fold volume of ethyl acetate, nearly 100% glucose was distributed into bottom phase, and 61.2% acetoin into top phase without coloring matters and organic acids. The top phase was treated by vacuum distillation to remove solvent and purify acetoin, while the bottom phase was used as carbon source to produce acetoin in the next batch of fermentation.

  14. Chemical composition and antibacterial activity of Cordia verbenacea extracts obtained by different methods.

    PubMed

    Michielin, Eliane M Z; Salvador, Ana A; Riehl, Carlos A S; Smânia, Artur; Smânia, Elza F A; Ferreira, Sandra R S

    2009-12-01

    The present study describes the chemical composition and the antibacterial activity of extracts from Cordia verbenacea DC (Borraginaceae), a traditional medicinal plant that grows widely along the southeastern coast of Brazil. The extracts were obtained using different extraction techniques: high-pressure operations and low-pressure methods. The high-pressure technique was applied to obtain C. verbenacea extracts using pure CO(2) and CO(2) with co-solvent at pressures up to 30MPa and temperatures of 30, 40 and 50 degrees C. Organic solvents such as n-hexane, ethyl acetate, ethanol, acetone and dichloromethane were used to obtain extracts by low-pressure processes. The antibacterial activity of the extracts was also subjected to screening against four strains of bacteria using the agar dilution method. The extraction yields were up to 5.0% w/w and up to 8.6% w/w for supercritical fluid extraction with pure CO(2) and with ethyl acetate as co-solvent, respectively, while the low-pressure extraction indicates yields up to 24.0% w/w in the soxhlet extraction using water and aqueous mixture with 50% ethanol as solvents. The inhibitory activity of the extracts in gram-positive bacteria was significantly higher than in gram-negative. The quantification and the identification of the extracts recovered were accomplished using GC/MS analysis. The most important components identified in the extract were artemetin, beta-sitosterol, alpha-humulene and beta-caryophyllene, among others.

  15. Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

    USGS Publications Warehouse

    Ferrer, I.; Furlong, E.T.

    2002-01-01

    Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

  16. Regeneration strategies of polymers employed in ex-situ remediation of contaminated soil: Bioregeneration versus solvent extraction.

    PubMed

    Mosca Angelucci, Domenica; Tomei, M Concetta

    2015-08-15

    In this study we evaluated the feasibility of two regeneration strategies of contaminated polymers employed for ex-situ soil remediation in a two-step process. Soil decontamination is achieved by sorption of the pollutants on the polymer beads, which are regenerated in a subsequent step. Tested soil was contaminated with a mixture of 4-chlorophenol and pentachlorophenol, and a commercial polymer, Hytrel, has been employed for extraction. Removal efficiencies of the polymer-soil extraction are in the range of 51-97% for a contact time ≤ 24 h. Two polymer regeneration strategies, solvent extraction and biological regeneration (realized in a two-phase partitioning bioreactor), were tested and compared. Performance was assessed in terms of removal rates and efficiencies and an economic analysis based on the operating costs has been performed. Results demonstrated the feasibility of both regeneration strategies, but the bioregeneration was advantageous in that provided the biodegradation of the contaminants desorbed from the polymer. Practically complete removal for 4-chlorophenol and up to 85% biodegradation efficiency for pentachlorophenol were achieved. Instead, in the solvent extraction, a relevant production (184-831 L kg(pol)(-1)) of a highly polluted stream to be treated or disposed of is observed. The cost analysis of the two strategies showed that the bioregeneration is much more convenient with operating costs of ∼12 €/kg(pol) i.e. more than one order of magnitude lower in comparison to ∼233 €/kg(pol) of the solvent extraction. Copyright © 2015 Elsevier Ltd. All rights reserved.

  17. 40 CFR 265.1032 - Standards: Process vents.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... owner or operator of a fa-cil-ity with process vents associated with distillation, fractionation, thin-film evaporation, solvent extraction or -air or steam stripping operations man-aging haz-ard-ous wastes...

  18. 40 CFR 265.1032 - Standards: Process vents.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... owner or operator of a fa-cil-ity with process vents associated with distillation, fractionation, thin-film evaporation, solvent extraction or -air or steam stripping operations man-aging haz-ard-ous wastes...

  19. Identification and determination of the saikosaponins in Radix bupleuri by accelerated solvent extraction combined with rapid-resolution LC-MS.

    PubMed

    Yang, Yun-Yun; Tang, You-Zhi; Fan, Chun-Lin; Luo, Hui-Tai; Guo, Peng-Ran; Chen, Jian-Xin

    2010-07-01

    A method based on accelerated solvent extraction combined with rapid-resolution LC-MS for efficient extraction, rapid separation, online identification and accurate determination of the saikosaponins (SSs) in Radix bupleuri (RB) was developed. The RB samples were extracted by accelerated solvent extraction using 70% aqueous ethanol v/v as solvent, at a temperature of 120 degrees C and pressure of 100 bar, with 10 min of static extraction time and three extraction cycles. Rapid-resolution LC separation was performed by using a C(18) column at gradient elution of water (containing 0.5% formic acid) and acetonitrile, and the major constituents were well separated within 20 min. A TOF-MS and an IT-MS were used for online identification of the major constituents, and 27 SSs were identified or tentatively identified. Five major bioactive SSs (SSa, SSc, SSd, 6''-O-acetyl-SSa and 6''-O-acetyl-SSd) with obvious peak areas and good resolution were chosen as benchmark substances, and a triple quadrupole MS operating in multiple-reaction monitoring mode was used for their quantitative analysis. A total of 16 RB samples from different regions of China were analyzed. The results indicated that the method was rapid, efficient, accurate and suitable for use in the quality control of RB.

  20. Design of experiment approach for the process optimisation of microwave assisted extraction of lupeol from Ficus racemosa leaves using response surface methodology.

    PubMed

    Das, Anup Kumar; Mandal, Vivekananda; Mandal, Subhash C

    2013-01-01

    Triterpenoids are a group of important phytocomponents from Ficus racemosa (syn. Ficus glomerata Roxb.) that are known to possess diverse pharmacological activities and which have prompted the development of various extraction techniques and strategies for its better utilisation. To develop an effective, rapid and ecofriendly microwave-assisted extraction (MAE) strategy to optimise the extraction of a potent bioactive triterpenoid compound, lupeol, from young leaves of Ficus racemosa using response surface methodology (RSM) for industrial scale-up. Initially a Plackett-Burman design matrix was applied to identify the most significant extraction variables amongst microwave power, irradiation time, particle size, solvent:sample ratio loading, varying solvent strength and pre-leaching time on lupeol extraction. Among the six variables tested, microwave power, irradiation time and solvent-sample/loading ratio were found to have a significant effect (P < 0.05) on lupeol extraction and were fitted to a Box-Behnken-design-generated quadratic polynomial equation to predict optimal extraction conditions as well as to locate operability regions with maximum yield. The optimal conditions were microwave power of 65.67% of 700 W, extraction time of 4.27 min and solvent-sample ratio loading of 21.33 mL/g. Confirmation trials under the optimal conditions gave an experimental yield (18.52 µg/g of dry leaves) close to the RSM predicted value of 18.71 µg/g. Under the optimal conditions the mathematical model was found to be well fitted with the experimental data. The MAE was found to be a more rapid, convenient and appropriate extraction method, with a higher yield and lower solvent consumption when compared with conventional extraction techniques. Copyright © 2012 John Wiley & Sons, Ltd.

  1. Surface area generation and droplet size control in solvent extraction systems utilizing high intensity electric fields

    DOEpatents

    Scott, Timothy C.; Wham, Robert M.

    1988-01-01

    A method and system for solvent extraction where droplets are shattered by a high intensity electric field. These shattered droplets form a plurality of smaller droplets which have a greater combined surface area than the original droplet. Dispersion, coalescence and phase separation are accomplished in one vessel through the use of the single pulsing high intensity electric field. Electric field conditions are chosen so that simultaneous dispersion and coalescence are taking place in the emulsion formed in the electric field. The electric field creates a large amount of interfacial surface area for solvent extraction when the droplet is disintegrated and is capable of controlling droplet size and thus droplet stability. These operations take place in the presence of a counter current flow of the continuous phase.

  2. Microfluidic process monitor for industrial solvent extraction system

    DOEpatents

    Gelis, Artem; Pereira, Candido; Nichols, Kevin Paul Flood

    2016-01-12

    The present invention provides a system for solvent extraction utilizing a first electrode with a raised area formed on its surface, which defines a portion of a microfluidic channel; a second electrode with a flat surface, defining another portion of the microfluidic channel that opposes the raised area of the first electrode; a reversibly deformable substrate disposed between the first electrode and second electrode, adapted to accommodate the raised area of the first electrode and having a portion that extends beyond the raised area of the first electrode, that portion defining the remaining portions of the microfluidic channel; and an electrolyte of at least two immiscible liquids that flows through the microfluidic channel. Also provided is a system for performing multiple solvent extractions utilizing several microfluidic chips or unit operations connected in series.

  3. Membrane-mediated extractive fermentation for lactic acid production from cellulosic biomass.

    PubMed

    Chen, R; Lee, Y Y

    1997-01-01

    Lactic acid production from cellulosic biomass by cellulase and Lactobacillus delbrueckii was studied in a fermenter-extractor employing a microporous hollow fiber membrane (MHF). This bioreactor system was operated under a fed-batch mode with continuous removal of lactic acid by anin situ extraction. A tertiary amine (Alamine 336) was used as an extractant for lactic acid. The extraction capacity of Alamine 336 is greatly enhanced by addition of alcohol. Long-chain alcohols serve well for this purpose since they are less toxic to micro-organism. Addition of kerosene, a diluent, was necessary to reduce the solvent viscosity. A solvent mixture of 20% Alamine 336, 40% oleyl alcohol, and 40% kerosene was found to be most effective in the extraction of lactic acid. Progressive change of pH from an initial value of 5.0 down to 4.3 has significantly improved the overall performance of the simultaneous saccharification and extractive fermentation over that of constant pH operation. The change of pH was applied to promote cell growth in the early phase, and extraction in the latter phase.

  4. Microporous plastic member such as a battery separator and process for making same

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Sundberg, E.G.; Campbell, G.A.; Doucette, E.I.

    A process for producing a microporous plastic member useful as a battery separator comprises the following operations: forming a coherent dough by mixing a vinyl chloride resin with a plasticizing amount of a first solvent and with finely divided particles of a filler which contains volatilizable releasable constituent by heating and which shrinks substantially and irreversibly upon release of the volatilizable constituent, an example of which is hydrated silica; forming the solvent-containing dough into a shaped member; extracting the first solvent from the member before any substantial evaporation of solvent occurs by contacting it with a second solvent in amore » liquid bath at a temperature substantially below the boiling point of any liquid present, the second solvent being one which is capable of dissolving the first solvent without dissolving the resin and the filler, thereby deplasticizing the member by extractively removing the first solvent from the member; and thereafter heating the member at an elevated temperature but below the softening point of the resin until the filler is shrunk within the member by release of its volatilizable content. 10 claims.« less

  5. Compositional similarities of non-solvent extractable fatty acids from recent marine sediments deposited in differing environments

    NASA Astrophysics Data System (ADS)

    Nishimura, Mitsugu; Baker, Earl W.

    1987-06-01

    Five recent sediment samples from a variety of North American continental shelves were analyzed for fatty acids (FAs) in the solvent-extractable (SOLEX) lipids as well as four types of non-solvent extractable (NONEX) lipids. The NONEX lipids were operationally defined by the succession of extraction procedure required to recover them. The complete procedure included (i) very mild acid treatment, (ii) HF digestion and (iii) saponification of the sediment residue following exhaustive solvent extraction. The distribution pattern and various compositional parameters of SOLEX FAs in the five sediments were divided into three different groups, indicating the difference of biological sources and also diagenetic factors and processes among the three groups of samples. Nevertheless, the compositions of the corresponding NONEX FAs after acid treatment were surprisingly very similar. This was also true for the remaining NONEX FA groups in the five sediment samples. The findings implied that most of the NONEX FAs reported here are derived directly from living organisms. It is also concluded that a large part of NONEX FAs are much more resistant to biodegradation than we have thought, so that they can form the large percentage of total lipids with increasing depth of water and sediments.

  6. Membrane-assisted extraction of monoterpenes: from in silico solvent screening towards biotechnological process application

    PubMed Central

    2018-01-01

    This work focuses on the process development of membrane-assisted solvent extraction of hydrophobic compounds such as monoterpenes. Beginning with the choice of suitable solvents, quantum chemical calculations with the simulation tool COSMO-RS were carried out to predict the partition coefficient (logP) of (S)-(+)-carvone and terpinen-4-ol in various solvent–water systems and validated afterwards with experimental data. COSMO-RS results show good prediction accuracy for non-polar solvents such as n-hexane, ethyl acetate and n-heptane even in the presence of salts and glycerol in an aqueous medium. Based on the high logP value, n-heptane was chosen for the extraction of (S)-(+)-carvone in a lab-scale hollow-fibre membrane contactor. Two operation modes are investigated where experimental and theoretical mass transfer values, based on their related partition coefficients, were compared. In addition, the process is evaluated in terms of extraction efficiency and overall product recovery, and its biotechnological application potential is discussed. Our work demonstrates that the combination of in silico prediction by COSMO-RS with membrane-assisted extraction is a promising approach for the recovery of hydrophobic compounds from aqueous solutions. PMID:29765654

  7. [Simultaneous determination of arsanilic, nitarsone and roxarsone residues in foods of animal origin by ASE-LC-AFS].

    PubMed

    Xiao, Ya-Bing; Zhang, Man; Wen, Hua-Wei

    2014-04-01

    A method for simultaneous determination of arsanilic, nitarsone and roxarsone (ROX) residues in foods of animal origin was developed by accelerated solvent extraction-liquid chromatography-atomic fluorescence spectrometry (ASE-LC-AFS). The ultrasound centrifugation extraction and accelerated solvent extraction were compared, and the accelerated solvent extraction conditions, namely the proportion of the extraction solvent, the extraction temperature, extraction time and extraction times, were optimized. The operating conditions of LC-AFS and the mobile phase were optimized. Under the optimal conditions, the calibration curves for ASA , NIT and ROX were linear over the concentration range of 0-2.0 mg x L(-1) and their correlation coefficients were 0.999 2-0.999 8. The detection limits of ASA, NIT and ROX were 2.4, 7.4 and 4.1 microg x L(-1) respectively. The average recoveries of ASA, NIT and ROX from two samples spiked at three levels of 0.5, 2, 5 mg x kg(-1) were in the ranges of 87.1%-93.2%, 85.2%-93.9%, and 84.2%-93.7% with RSDs of 1.4%-4.6%, 1.2%-4.2%, and 1.1%-4.5%, respectively. This method possesses the merits of convenience and good repeatability, and is a feasible method for analysis of ASA, NIT and ROX in foods of animal origin.

  8. Effects of high-pressure process on kinetics of leaching oil from soybean powder using hexane in batch systems.

    PubMed

    Uhm, Joo Tae; Yoon, Won Byong

    2011-08-01

    Mass transfer models of leaching oil from soybean (Glycine max) flour with hexane after high-pressure process (HPP) treatment were developed. High pressure (450 MPa) was applied to the soybean flour (mean diameter of flour particle: 365 μm) for 30 min before leaching the oil components in the solvent. The ratio of solvent (volume, mL) to soybean flour (mass, g), such as 1:10 and 1:20, was employed to characterize the effect of solvent ratio on the leaching rate in the batch type of extraction process. Ultraviolet absorbance at 300 nm was used to monitor the extraction rate. Saturation solubility (C(AS)) was determined to be 21.73 kg/m³. The mass transfer coefficients (k) were determined based on the 1st- and 2nd-order kinetic models. The 2nd kinetic model showed better fit. The HPP treatment showed a higher extraction rate and yield compared to the control, while the amount of solvent did not affect the extraction rate and yield. The scanning electron microscope showed that HPP-treated soybean particles included more pores than the untreated. The pores observed in the HPP-treated soybean flours might help increase the mass transfer rate of solvent and solute in the solid matrix. High-pressure processing can help increase the extraction rate of oil from the soybean flour operated in batch systems. The conventional solid to solvent ratio (1:20) used to extract oil composition from the plant seed did not help increase the amount of oil extracted from the soybean flour. © 2011 Institute of Food Technologists®

  9. STORAGE STABILITY OF PESTICIDES IN EXTRACT SOLVENTS AND SAMPLING MEDIA

    EPA Science Inventory

    Demonstrating that pesticides are stable in field media and their extracts over extended storage periods allows operational flexibility and cost efficiency. Stability of the 31 neutral pesticides and 2 acid herbicides of the Agricultural Health Study exposure pilot was evaluate...

  10. Extraction and identification of bioactive compounds from agarwood leaves

    NASA Astrophysics Data System (ADS)

    Lee, N. Y.; Yunus, M. A. C.; Idham, Z.; Ruslan, M. S. H.; Aziz, A. H. A.; Irwansyah, N.

    2016-11-01

    Agarwood commonly known as gaharu, aloeswood or eaglewood have been used as traditional medicine for centuries and its essential oil also being used as perfumery ingredients and aroma enhancers in food products. However, there is least study on the agarwood leaves though it contains large number of biomolecules component that show diverse pharmacological activity. Previous study showed that the extracted compounds from the leaves possess activities like anti-mutagenic, anti-tumor and anti-helminthic. The main objectives of this research were to determine bioactive compounds in agarwood leaves; leaves extract and oil yield obtained from maceration and soxhlet extraction methods respectively. The maceration process was performed at different operating temperature of 25°C, 50°C and 75°C and different retention time at 30, 60, 90 and 120 minutes. Meanwhile, various solvents were used to extract the oil from agarwood leaves using soxhlet method which are hexane, water, isopropanol and ethanol. The extracted oil from agarwood leaves by soxhlet extraction was analyzed using gas chromatography mass spectrometry. The results showed that the highest extract of 1.53% was obtained when increase the temperature to 75 °C and longest retention time of 120 minutes gave the highest oil yield of 2.10 % by using maceration. This is because at higher temperature enhances the solubility solute and diffusivity coefficient, thus increase the extract yield while longer retention time allow the reaction between solvent and solute occurred more rapidly giving higher extract. Furthermore, the soxhlet extraction using n-hexane as the solvent gave the highest oil yield as compared to other solvent due to the non-polar properties of n-hexane increase the efficiency of oil which is also non-polar to soluble in the solvent. In addition, the results also reported that the oil extracted from agarwood leaves contains bioactive compounds which are phytol, squalene, n-hexadecanoic acid and octadecatrienoic acid. Therefore, oil extracted from agarwood leaves has the potential to be applied in food, pharmaceutical, nutraceutical and cosmetics industries.

  11. Novel Approaches to Extraction Methods in Recovery of Capsaicin from Habanero Pepper (CNPH 15.192).

    PubMed

    Martins, Frederico S; Borges, Leonardo L; Ribeiro, Claudia S C; Reifschneider, Francisco J B; Conceição, Edemilson C

    2017-07-01

    The objective of this study was to compare three capsaicin extraction methods: Shoxlet, Ultrasound-assisted Extraction (UAE), and Shaker-assisted Extraction (SAE) from Habanero pepper, CNPH 15.192. The different parameters evaluated were alcohol degree, time extraction, and solid-solvent ratio using response surface methodology (RSM). The three parameters found significant ( p < 0.05) were for UAE and solvent concentration and extraction time for SAE. The optimum conditions for the capsaicin UAE and SAE were similar 95% alcohol degree, 30 minutes and solid-liquid ratio 2 mg/mL. The Soxhlet increased the extraction in 10-25%; however, long extraction times (45 minutes) degraded 2% capsaicin. The extraction of capsaicin was influenced by extraction method and by the operating conditions chosen. The optimized conditions provided savings of time, solvent, and herbal material. Prudent choice of the extraction method is essential to ensure optimal yield of extract, thereby making the study relevant and the knowledge gained useful for further exploitation and application of this resource. Habanero pepper , line CNPH 15.192, possess capsaicin in higher levels when compared with others speciesHigher levels of ethanolic strength are more suitable to obtain a higher levels of capsaicinBox-Behnken design indicates to be useful to explore the best conditions of ultrasound assisted extraction of capsaicin. Abbreviations used: Nomenclature UAE: Ultrasound-assisted Extraction; SAE: Shaker-assisted Extraction.

  12. Bio-Oil Separation and Stabilization by Near-Critical Propane Fractionation

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ginosar, Daniel M.; Petkovic, Lucia M.; Agblevor, Foster A.

    Bio-oils produced by thermal process are promising sources of sustainable, low greenhouse gas alternative fuels. These thermal processes are also well suited to decentralized energy production due to low capital and operating costs. Algae feedstocks for bio-oil production are of particular interest, due in part to their high-energy growth yields. Further, algae can be grown in non-arable areas in fresh, brackish, salt water, or even waste water. Unfortunately, bio-oils produced by thermal processes present significant stability challenges. These oils have complex chemical compositions, are viscous, reactive, and thermally unstable. Further, the components within the oils are difficult to separate bymore » fractional distillation. By far, the most effective separation and stabilization method has been solvent extraction. However, liquid phase extraction processes pose two main obstacles to commercialization; they require a significant amount of energy to remove and recover the solvent from the product, and they have a propensity for the solvent to become contaminated with minerals from the char and ash present in the original bio-oil. Separation and fractionation of thermally produced bio-oils using supercritical fluids (SCF) offers the advantages of liquid solvent extraction while drastically reducing energy demands and the predisposition to carry over solids into the extracted phase. SCFs are dense fluids with liquid-like solvent properties and gas-like transport properties. Further, SCF density and solvent strength can be tuned with minor adjustments in pressure, co-solvent addition, or gas anti-solvent addition. Catalytic pyrolysis oils were produced from Scenedesmus dimorphus algae using a fluid catalytic cracking catalyst. Bio-oil produced from catalytic fast pyrolysis (CFP) was separated using critical fluids. Propane extraction was performed at 65 °C at a fluid reduced pressure of 2.0 (85 bar) using an eight to one solvent to feed ratio by weight. Extraction of catalytic fast pyrolysis oil with near critical propane produced an oil extract that was physically and chemically different from and more stable than the original oil. The propane extract displayed lower viscosity and lower average molecular weight. The species present in the propane extract were likely the less polar that would be expected from using a non-polar solvent (propane). Carbonyl containing species in the extract were likely ketones and esters. The raffinate contained a higher amnount of OH bonded species along with the more polar more polar acids, amides, and alcohols. The higher concentration of nitrogen in the raffinate may confirm the presence of amides. Viscosity of the propane extract increased only half as much as that of the CFP bio-oil. Further, In situ NMR aging studies showed that the propane extract was more stable than the raw oil. In conclusion, propane extraction is a promising method to decrease the nitrogen content of bio-oils and to improve the stability of bio-oils obtained by the catalytic pyrolysis of algae based biomass.« less

  13. Membrane-mediated extractive fermentation for lactic acid production from cellulosic biomass

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chen, Rongfu; Lee, Y.Y.

    1997-12-31

    Lactic acid production from cellulosic biomass by cellulose and Lactobacillus delbrueckii was studied in a fermenter-extractor employing a microporous hollow fiber membrane (NIHF). This bioreactor system was operated under a fed-batch mode with continuous removal of lactic acid by an in situ extraction. A tertiary amine (Alamine 336) was used as an extractant for lactic acid. The extraction capacity of Alamine 336 is greatly enhanced by addition of alcohol. Long-chain alcohols serve well for this purpose since they are less toxic to micro-organism. Addition of kerosene, a diluent, was necessary to reduce the solvent viscosity. A solvent mixture of 20%more » Alamine 336,40% oleyl alcohol, and 40% kerosene was found to be most effective in the extraction of lactic acid. Progressive change of pH from an initial value of 5.0 down to 4.3 has significantly improved the overall performance of the simultaneous saccharification and extractive fermentation over that of constant pH operation. The change of pH was applied to promote cell growth in the early phase, and extraction in the latter phase. 20 refs., 10 figs., 1 tab.« less

  14. Room-temperature ionic liquids as replacements for organic solvents in multiphase bioprocess operations.

    PubMed

    Cull, S G; Holbrey, J D; Vargas-Mora, V; Seddon, K R; Lye, G J

    2000-07-20

    Organic solvents are widely used in a range of multiphase bioprocess operations including the liquid-liquid extraction of antibiotics and two-phase biotransformation reactions. There are, however, considerable problems associated with the safe handling of these solvents which relate to their toxic and flammable nature. In this work we have shown for the first time that room-temperature ionic liquids, such as 1-butyl-3-methylimi- dazolium hexafluorophosphate, [bmim][PF(6)], can be successfully used in place of conventional solvents for the liquid-liquid extraction of erythromycin-A and for the Rhodococcus R312 catalyzed biotransformation of 1, 3-dicyanobenzene (1,3-DCB) in a liquid-liquid, two-phase system. Extraction of erythromycin with either butyl acetate or [bmim][PF(6)] showed that values of the equilibrium partition coefficient, K, up to 20-25 could be obtained for both extractants. The variation of K with the extraction pH was also similar in the pH range 5-9 though differed significantly at higher pH values. Biotransformation of 1,3-DCB in both water-toluene and water-[bmim][PF(6)] systems showed similar profiles for the conversion of 1,3-DCB initially to 3-cyanobenzamide and then 3-cyanobenzoic acid. The initial rate of 3-cyanobenzamide production in the water-[bmim][PF(6)] system was somewhat lower, however, due to the reduced rate of 1,3-DCB mass transfer from the more viscous [bmim] [PF(6)] phase. It was also shown that the specific activity of the biocatalyst in the water-[bmim] [PF(6)] system was almost an order of magnitude greater than in the water-toluene system which suggests that the rate of 3-cyanobenzamide production was limited by substrate mass transfer rather than the activity of the biocatalyst. Copyright 2000 John Wiley & Sons, Inc.

  15. An approach of ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergistic extraction for two coumarins preparation from Cortex fraxini.

    PubMed

    Liu, Zaizhi; Gu, Huiyan; Yang, Lei

    2015-10-23

    Ionic liquids/lithium salts solvent system was successfully introduced into the separation technique for the preparation of two coumarins (aesculin and aesculetin) from Cortex fraxini. Ionic liquids/lithium salts based microwave irradiation pretreatment followed by ultrasound-microwave synergy extraction (ILSMP-UMSE) procedure was developed and optimized for the sufficient extraction of these two analytes. Several variables which can potentially influence the extraction yields, including pretreatment time and temperature, [C4mim]Br concentration, LiAc content, ultrasound-microwave synergy extraction (UMSE) time, liquid-solid ratio, and UMSE power were optimized by Plackett-Burman design. Among seven variables, UMSE time, liquid-solid ratio, and UMSE power were the statistically significant variables and these three factors were further optimized by Box-Behnken design to predict optimal extraction conditions and find out operability ranges with maximum extraction yields. Under optimum operating conditions, ILSMP-UMSE showed higher extraction yields of two target compounds than those obtained by reference extraction solvents. Method validation studies also evidenced that ILSMP-UMSE is credible for the preparation of two coumarins from Cortex fraxini. This study is indicative of the proposed procedure that has huge application prospects for the preparation of natural products from plant materials. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Comparison Pore Aggregate Levels After Extraction With Solvents Pertamax Plus And Gasoline

    NASA Astrophysics Data System (ADS)

    Anggraini, Muthia

    2017-12-01

    Loss of asphalt content extraction results become problems in Field Work For implementing parties. The use of solvents with high octane (pertamax plus) for the extraction, dissolving the asphalt more than gasoline. By comparing the levels of aggregate pores after using solvent extraction pertamax plus compared to gasoline could answer that pertamax plus more solvent dissolves the bitumen compared to gasoline. This study aims to obtain comparative levels of porous aggregate mix AC-WC after using solvent extraction pertamax plus compared to gasoline. This study uses the aggregate that has been extracted from the production of asphalt mixtures, when finisher and after compaction field. The method used is the assay of coarse and fine aggregate pores, extraction of bitumen content to separate the aggregate with bitumen. Results of testing the total absorption after extraction using a solvent preta max plus in the production of asphalt mixtures 0.80%, while gasoline solvent 0.67% deviation occurs 0.13%. In the finisher after the solvent extraction preta max plus 0.77%, while 0.67% gasoline solvent occurs deviation of 0.1%. At the core after extraction and solvent pertamax plus 0.71%, while gasoline solvent 0.60% 0.11% deviation occurs. The total water absorption after extraction using a solvent pertamax plus greater than gasoline. This proves that the solvent dissolves pertamax plus more asphalt than gasoline.

  17. Combination pulsed electric field with ethanol solvent for Nannochloropsis sp. extraction

    NASA Astrophysics Data System (ADS)

    Nafis, Ghazy Ammar; Mumpuni, Perwitasari Yekti; Indarto, Budiman, Arief

    2015-12-01

    Nowadays, energy is one of human basic needs. As the human population increased, energy consumption also increased. This condition causes energy depletion. In case of the situation, alternative energy is needed to replace existing energy. Microalgae is chosen to become one of renewable energy resource, especially biodiesel, because it contains high amount of lipid instead of other feedstock which usually used. Fortunately, Indonesia has large area of water and high intensity of sunlight so microalgae cultivation becomes easier. Nannochloropsis sp., one of microalgae species, becomes the main focus because of its high lipid content. Many ways to break the cell wall of microalgae so the lipid content inside the microalgae will be released, for example conventional extraction, ultrasonic wave extraction, pressing, and electrical method. The most effective way for extraction is electrical method such as pulsed electric field method (PEF). The principal work of this method is by draining the electrical current into parallel plate. Parallel plate will generate the electrical field to break microalgae cell wall and the lipid will be released. The aim of this work is to evaluate two-stage procedure for extraction of useful components from microalgae Nannochloropsis sp. The first stage of this procedure includes pre-treatment of microalgae by ethanol solvent extraction and the second stage applies the PEF extraction using a binary mixture of water and ethanol solvent. Ethanol is chosen as solvent because it's safer to be used and easier to be handled than other solvent. Some variables that used to study the most effective operation conditions are frequency and duty cycle for microalgae. The optimum condition based on this research are at frequency 1 Hz and duty cycle 13%.

  18. Novel Approaches to Extraction Methods in Recovery of Capsaicin from Habanero Pepper (CNPH 15.192)

    PubMed Central

    Martins, Frederico S.; Borges, Leonardo L.; Ribeiro, Claudia S. C.; Reifschneider, Francisco J. B.; Conceição, Edemilson C.

    2017-01-01

    Introduction: The objective of this study was to compare three capsaicin extraction methods: Shoxlet, Ultrasound-assisted Extraction (UAE), and Shaker-assisted Extraction (SAE) from Habanero pepper, CNPH 15.192. Materials and Methods: The different parameters evaluated were alcohol degree, time extraction, and solid–solvent ratio using response surface methodology (RSM). Results: The three parameters found significant (p < 0.05) were for UAE and solvent concentration and extraction time for SAE. The optimum conditions for the capsaicin UAE and SAE were similar 95% alcohol degree, 30 minutes and solid–liquid ratio 2 mg/mL. The Soxhlet increased the extraction in 10–25%; however, long extraction times (45 minutes) degraded 2% capsaicin. Conclusion: The extraction of capsaicin was influenced by extraction method and by the operating conditions chosen. The optimized conditions provided savings of time, solvent, and herbal material. Prudent choice of the extraction method is essential to ensure optimal yield of extract, thereby making the study relevant and the knowledge gained useful for further exploitation and application of this resource. SUMMARY Habanero pepper, line CNPH 15.192, possess capsaicin in higher levels when compared with others speciesHigher levels of ethanolic strength are more suitable to obtain a higher levels of capsaicinBox-Behnken design indicates to be useful to explore the best conditions of ultrasound assisted extraction of capsaicin. Abbreviations used: Nomenclature UAE: Ultrasound-assisted Extraction; SAE: Shaker-assisted Extraction. PMID:28808409

  19. Centrifugal contactor modified for end stage operation in a multistage system

    DOEpatents

    Jubin, Robert T.

    1990-01-01

    A cascade formed of a plurality of centrifugal contactors useful for countercurrent solvent extraction processes such as utilizable for the reprocessing of nuclear reactor fuels is modified to permit operation in the event one or both end stages of the cascade become inoperative. Weir assemblies are connected to each of the two end stages by suitable conduits for separating liquids discharged from an inoperative end stage based upon the weight of the liquid phases uses in the solvent extraction process. The weir assembly at one end stage is constructed to separate and discharge the heaviest liquid phase while the weir assembly at the other end stage is constructed to separate and discharge the lightest liquid phase. These weir assemblies function to keep the liquid discharge from an inoperative end stages on the same weight phase a would occur from an operating end stage.

  20. Mathematical modelling for extraction of oil from Dracocephalum kotschyi seeds in supercritical carbon dioxide.

    PubMed

    Sodeifian, Gholamhossein; Sajadian, Seyed Ali; Honarvar, Bizhan

    2018-04-01

    Extraction of oil from Dracocephalum kotschyi Boiss seeds using supercritical carbon dioxide was designed using central composite design to evaluate the effect of various operating parameters including pressure, temperature, particle size and extraction time on the oil yield. Maximum extraction yield predicted from response surface method was 71.53% under the process conditions with pressure of 220 bar, temperature of 35 °C, particle diameter of 0.61 mm and extraction time of 130 min. Furthermore, broken and intact cells model was utilised to consider mass transfer kinetics of extracted natural materials. The results revealed that the model had a good agreement with the experimental data. The oil samples obtained via supercritical and solvent extraction methods were analysed by gas chromatography. The most abundant acid was linolenic acid. The results analysis showed that there was no significant difference between the fatty acid contents of the oils obtained by the supercritical and solvent extraction techniques.

  1. Impact of solvent extraction organics on adsorption and bioleaching of A. ferrooxidans and L. ferriphilum

    NASA Astrophysics Data System (ADS)

    Hualong, Yu; Xiaorong, Liu

    2017-04-01

    Copper solvent extraction entrained and dissoluted organics (SX organics) in the raffinate during SX operation can contaminated chalcopyrite ores and influence bioleaching efficiency by raffinate recycling. The adsorption and bioleaching of A. ferrooxidans and L. ferriphilum with contaminated ores were investigated. The results showed that, A. ferrooxidans and L. ferriphilum cells could adsorb quickly on minerals, the adsorption rate on contaminated ores were 83% and 60%, respectively, larger than on uncontaminated ores. However, in the bioleaching by the two kinds of acid bacterias, contaminated ores presented a lower bioleaching efficiency.

  2. Impact of solvent extraction organics on bioleaching by Acidithiobacillus ferrooxidans

    NASA Astrophysics Data System (ADS)

    Yu, Hualong; Liu, Xiaorong; Shen, Junhui; Chi, Daojie

    2017-03-01

    Solvent extraction organics (SX organics) entrained and dissoluted in the raffinate during copper SX operation, can impact bioleaching in case of raffinate recycling. The influence of SX organics on bioleaching process by Acidithiobacillus ferrooxidans (At. ferrooxidans) has been investigated. The results showed that, cells of At. ferrooxidans grew slower with contaminated low-grade chalcopyrite ores in shaken flasks bioleaching, the copper bioleaching efficiency reached 15%, lower than that of 24% for uncontaminated minerals. Obviously, the SX organics could adsorb on mineral surface and hinder its contact with bacterials, finanlly lead to the low bioleaching efficiency.

  3. Aqueous Chloride Operations Overview: Plutonium and Americium Purification/Recovery

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Gardner, Kyle Shelton; Kimball, David Bryan; Skidmore, Bradley Evan

    These are a set of slides intended for an information session as part of recruiting activities at Brigham Young University. It gives an overview of aqueous chloride operations, specifically on plutonium and americium purification/recovery. This presentation details the steps taken perform these processes, from plutonium size reduction, dissolution, solvent extraction, oxalate precipitation, to calcination. For americium recovery, it details the CLEAR (chloride extraction and actinide recovery) Line, oxalate precipitation and calcination.

  4. A microfluidic study of liquid-liquid extraction mediated by carbon dioxide.

    PubMed

    Lestari, Gabriella; Salari, Alinaghi; Abolhasani, Milad; Kumacheva, Eugenia

    2016-07-05

    Liquid-liquid extraction is an important separation and purification method; however, it faces a challenge in reducing the energy consumption and the environmental impact of solvent (extractant) recovery. The reversible chemical reactions of switchable solvents (nitrogenous bases) with carbon dioxide (CO2) can be implemented in reactive liquid-liquid extraction to significantly reduce the cost and energy requirements of solvent recovery. The development of new effective switchable solvents reacting with CO2 and the optimization of extraction conditions rely on the ability to evaluate and screen the performance of switchable solvents in extraction processes. We report a microfluidic strategy for time- and labour-efficient studies of CO2-mediated solvent extraction. The platform utilizes a liquid segment containing an aqueous extractant droplet and a droplet of a solution of a switchable solvent in a non-polar liquid, with gaseous CO2 supplied to the segment from both sides. Following the reaction of the switchable solvent with CO2, the solvent becomes hydrophilic and transfers from the non-polar solvent to the aqueous droplet. By monitoring the time-dependent variation in droplet volumes, we determined the efficiency and extraction time for the CO2-mediated extraction of different nitrogenous bases in a broad experimental parameter space. The platform enables a significant reduction in the amount of switchable solvents used in these studies, provides accurate temporal characterization of the liquid-liquid extraction process, and offers the capability of high-throughput screening of switchable solvents.

  5. Solventless and solvent-minimized sample preparation techniques for determining currently used pesticides in water samples: a review.

    PubMed

    Tankiewicz, Maciej; Fenik, Jolanta; Biziuk, Marek

    2011-10-30

    The intensification of agriculture means that increasing amounts of toxic organic and inorganic compounds are entering the environment. The pesticides generally applied nowadays are regarded as some of the most dangerous contaminants of the environment. Their presence in the environment, especially in water, is hazardous because they cause human beings to become more susceptible to disease. For these reasons, it is essential to monitor pesticide residues in the environment with the aid of all accessible analytical methods. The analysis of samples for the presence of pesticides is problematic, because of the laborious and time-consuming operations involved in preparing samples for analysis, which themselves may be a source of additional contaminations and errors. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solventless and solvent-minimized techniques are coming into use. This paper discusses the most commonly used over the last 15 years sample preparation techniques for monitoring organophosphorus and organonitrogen pesticides residue in water samples. Furthermore, a significant trend in sample preparation, in accordance with the principles of 'Green Chemistry' is the simplification, miniaturization and automation of analytical techniques. In view of this aspect, several novel techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. The paper describes extraction techniques requiring the use of solvents - liquid-liquid extraction (LLE) and its modifications, membrane extraction techniques, hollow fibre-protected two-phase solvent microextraction, liquid phase microextraction based on the solidification of a floating organic drop (LPME-SFO), solid-phase extraction (SPE) and single-drop microextraction (SDME) - as well as solvent-free techniques - solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The advantages and drawbacks of these techniques are also discussed, and some solutions to their limitations are proposed. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. Ligandless dispersive liquid--liquid microextraction of iron in biological and foodstuff samples and its determination by Electrothermal atomic absorption spectrometry.

    PubMed

    Madadizadeh, Mohadeseh; Taher, Mohammad Ali; Ashkenani, Hamid

    2013-01-01

    A new, simple, and efficient method comprising ligandless dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry is reported for the preconcentration and determination of ultratrace amounts of Fe(III). Carbon tetrachloride and acetone were used as the extraction and disperser solvents, respectively. Some effective parameters of the microextraction such as choice of extraction and disperser solvents, their volume, extraction time and temperature, salt and surfactant effect, and pH were optimized. Under the optimum conditions, the calibration curve was linear in the range of 0.02 to 0.46 microg/L of Fe(III), with LOD and LOQ of 5.2 and 17.4 ng/L, respectively. The RSD for seven replicated determinations of Fe(IIl) ion at 0.1 microg/L concentration level was 5.2%. Operational simplicity, rapidity, low cost, good repeatability, and low consumption of extraction solvent are the main advantages of the proposed method. The method was successfully applied to the determination of iron in biological, food, and certified reference samples.

  7. Solvent wash solution

    DOEpatents

    Neace, J.C.

    1984-03-13

    A process is claimed for removing diluent degradation products from a solvent extraction solution, which has been used to recover uranium and plutonium from spent nuclear fuel. A wash solution and the solvent extraction solution are combined. The wash solution contains (a) water and (b) up to about, and including, 50 vol % of at least one-polar water-miscible organic solvent based on the total volume of the water and the highly-polar organic solvent. The wash solution also preferably contains at least one inorganic salt. The diluent degradation products dissolve in the highly-polar organic solvent and the organic solvent extraction solvent do not dissolve in the highly-polar organic solvent. The highly-polar organic solvent and the extraction solvent are separated.

  8. Solvent wash solution

    DOEpatents

    Neace, James C.

    1986-01-01

    Process for removing diluent degradation products from a solvent extraction solution, which has been used to recover uranium and plutonium from spent nuclear fuel. A wash solution and the solvent extraction solution are combined. The wash solution contains (a) water and (b) up to about, and including, 50 volume percent of at least one-polar water-miscible organic solvent based on the total volume of the water and the highly-polar organic solvent. The wash solution also preferably contains at least one inorganic salt. The diluent degradation products dissolve in the highly-polar organic solvent and the organic solvent extraction solvent do not dissolve in the highly-polar organic solvent. The highly-polar organic solvent and the extraction solvent are separated.

  9. NEPTUNIUM SOLVENT EXTRACTION PROCESS

    DOEpatents

    Dawson, L.R.; Fields, P.R.

    1959-10-01

    The separation of neptunium from an aqueous solution by solvent extraction and the extraction of neptunium from the solvent solution are described. Neptunium is separated from an aqueous solution containing tetravalent or hexavalent neptunium nitrate, nitric acid, and a nitrate salting out agent, such as sodium nitrate, by contacting the solution with an organic solvent such as diethyl ether. Subsequently, the neptunium nitrate is extracted from the organic solvent extract phase with water.

  10. Determination of fatty acid composition and quality characteristics of oils from palm fruits using solvent extraction

    NASA Astrophysics Data System (ADS)

    Kasmin, Hasimah; Lazim, Azwan Mat; Awang, Roila

    2015-09-01

    Palm oil contains about 45% of saturated palmitic acid and 39% of mono-unsaturated oleic acid. Investigations made in the past to trace the fatty acid composition in palm revealed that ripeness of fresh fruit bunch (FFB) affect oil composition. However, there is no evidence that processing operations affect oil composition, although different stage of processing does affect the quality of oil extracted. An improved method for sterilizing the oil palm fruits by dry heating, followed by oil extraction has been studied. This method eliminates the use of water, thus, increasing the extraction of lipid soluble. The objective of this study is to determine the possibility production of palm oil with different fatty acid composition (FAC) as well as the changes in quality from conventional milling. The unripe and ripe FFB were collected, sterilized and extracted using different method of solvent extraction. Preliminary data have shown that variation in FAC will also alter the physical and chemical properties of the oil extracted.

  11. Measurement of dielectric constant of organic solvents by indigenously developed dielectric probe

    NASA Astrophysics Data System (ADS)

    Keshari, Ajay Kumar; Rao, J. Prabhakar; Rao, C. V. S. Brahmmananda; Ramakrishnan, R.; Ramanarayanan, R. R.

    2018-04-01

    The extraction, separation and purification of actinides (uranium and plutonium) from various matrices are an important step in nuclear fuel cycle. One of the separation process adopted in an industrial scale is the liquid-liquid extraction or solvent extraction. Liquid-liquid extraction uses a specific ligand/extractant in conjunction with suitable diluent. Solvent extraction or liquid-liquid extraction, involves the partitioning of the solute between two immiscible phases. In most cases, one of the phases is aqueous, and the other one is an organic solvent. The solvent used in solvent extraction should be selective for the metal of interest, it should have optimum distribution ratio, and the loaded metal from the organic phase should be easily stripped under suitable experimental conditions. Some of the important physical properties which are important for the solvent are density, viscosity, phase separation time, interfacial surface tension and the polarity of the extractant.

  12. Downstream Processing of Synechocystis for Biofuel Production

    NASA Astrophysics Data System (ADS)

    Sheng, Jie

    Lipids and free fatty acids (FFA) from cyanobacterium Synechocystis can be used for biofuel (e.g. biodiesel or renewable diesel) production. In order to utilize and scale up this technique, downstream processes including culturing and harvest, cell disruption, and extraction were studied. Several solvents/solvent systems were screened for lipid extraction from Synechocystis. Chloroform + methanol-based Folch and Bligh & Dyer methods were proved to be "gold standard" for small-scale analysis due to their highest lipid recoveries that were confirmed by their penetration of the cell membranes, higher polarity, and stronger interaction with hydrogen bonds. Less toxic solvents, such as methanol and MTBE, or direct transesterification of biomass (without preextraction step) gave only slightly lower lipid-extraction yields and can be considered for large-scale application. Sustained exposure to high and low temperature extremes severely lowered the biomass and lipid productivity. Temperature stress also triggered changes of lipid quality such as the degree of unsaturation; thus, it affected the productivities and quality of Synechocystis-derived biofuel. Pulsed electric field (PEF) was evaluated for cell disruption prior to lipid extraction. A treatment intensity > 35 kWh/m3 caused significant damage to the plasma membrane, cell wall, and thylakoid membrane, and it even led to complete disruption of some cells into fragments. Treatment by PEF enhanced the potential for the low-toxicity solvent isopropanol to access lipid molecules during subsequent solvent extraction, leading to lower usage of isopropanol for the same extraction efficiency. Other cell-disruption methods also were tested. Distinct disruption effects to the cell envelope, plasma membrane, and thylakoid membranes were observed that were related to extraction efficiency. Microwave and ultrasound had significant enhancement of lipid extraction. Autoclaving, ultrasound, and French press caused significant release of lipid into the medium, which may increase solvent usage and make medium recycling difficult. Production of excreted FFA by mutant Synechocystis has the potential of reducing the complexity of downstream processing. Major problems, such as FFA precipitation and biodegradation by scavengers, account for FFA loss in operation. Even a low concentration of FFA scavengers could consume FFA at a high rate that outpaced FFA production rate. Potential strategies to overcome FFA loss include high pH, adsorptive resin, and sterilization techniques.

  13. Compressed air-assisted solvent extraction (CASX) for metal removal.

    PubMed

    Li, Chi-Wang; Chen, Yi-Ming; Hsiao, Shin-Tien

    2008-03-01

    A novel process, compressed air-assisted solvent extraction (CASX), was developed to generate micro-sized solvent-coated air bubbles (MSAB) for metal extraction. Through pressurization of solvent with compressed air followed by releasing air-oversaturated solvent into metal-containing wastewater, MSAB were generated instantaneously. The enormous surface area of MSAB makes extraction process extremely fast and achieves very high aqueous/solvent weight ratio (A/S ratio). CASX process completely removed Cr(VI) from acidic electroplating wastewater under A/S ratio of 115 and extraction time of less than 10s. When synthetic wastewater containing Cd(II) of 50mgl(-1) was treated, A/S ratios of higher than 714 and 1190 could be achieved using solvent with extractant/diluent weight ratio of 1:1 and 5:1, respectively. Also, MSAB have very different physical properties, such as size and density, compared to the emulsified solvent droplets, making separation and recovery of solvent from treated effluent very easy.

  14. 40 CFR 63.2855 - How do I determine the quantity of oilseed processed?

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR SOURCE CATEGORIES National Emission Standards for Hazardous Air Pollutants: Solvent Extraction for Vegetable Oil... operating month, you must determine the tons as received of each listed oilseed processed for the operating...

  15. 40 CFR 63.2861 - What reports must I submit and when?

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Standards for Hazardous Air Pollutants: Solvent Extraction for Vegetable Oil Production Notifications... certification: (1) The name and address of the owner or operator. (2) The physical address of the vegetable oil... or operator. (2) The physical address of the vegetable oil production process. (3) Each listed...

  16. 40 CFR 63.2861 - What reports must I submit and when?

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Standards for Hazardous Air Pollutants: Solvent Extraction for Vegetable Oil Production Notifications... certification: (1) The name and address of the owner or operator. (2) The physical address of the vegetable oil... or operator. (2) The physical address of the vegetable oil production process. (3) Each listed...

  17. SOLVENT EXTRACTION PROCESS

    DOEpatents

    Jonke, A.A.

    1957-10-01

    In improved solvent extraction process is described for the extraction of metal values from highly dilute aqueous solutions. The process comprises contacting an aqueous solution with an organic substantially water-immiscible solvent, whereby metal values are taken up by a solvent extract phase; scrubbing the solvent extract phase with an aqueous scrubbing solution; separating an aqueous solution from the scrubbed solvent extract phase; and contacting the scrubbed solvent phase with an aqueous medium whereby the extracted metal values are removed from the solvent phase and taken up by said medium to form a strip solution containing said metal values, the aqueous scrubbing solution being a mixture of strip solution and an aqueous solution which contains mineral acids anions and is free of the metal values. The process is particularly effective for purifying uranium, where one starts with impure aqueous uranyl nitrate, extracts with tributyl phosphate dissolved in carbon tetrachloride, scrubs with aqueous nitric acid and employs water to strip the uranium from the scrubbed organic phase.

  18. Integrated Stable Isotope - Reactive Transport Model Approach for Assessment of Chlorinated Solvent Degradation

    DTIC Science & Technology

    2016-05-01

    Certification Program ETH Ethene GC Gas Chromatography GC-IRMS Gas Chromatography Isotope Ratio Mass Spectroscopy H Hydrogen IRMS Isotope...tool for attenuation of chlorinated solvents. The Demonstration Site was Operable Unit 10 at Hill AFB, Utah , a site where groundwater is impacted...techniques. The method involves extraction of the target compounds from environmental sample matrix, followed by separation of the compounds using gas

  19. Determination of four major saponins in the seeds of Aesculus chinensis Bunge using accelerated solvent extraction followed by high-performance liquid chromatography and electrospray-time of flight mass spectrometry.

    PubMed

    Chen, Junhui; Li, Wenlong; Yang, Baijuan; Guo, Xiuchun; Lee, Frank Sen-Chun; Wang, Xiaoru

    2007-07-23

    A new method based on accelerated solvent extraction (ASE) followed by a reliable high-performance liquid chromatography-diode array detector (HPLC-DAD) and positive ion electrospray-time of flight mass spectrometry (ESI-TOF/MS) analysis has been developed for the characterization and quantification of four major saponins in extracts of the seeds of Aesculus chinensis Bunge (semen aesculi). The saponins escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted from seeds of A. chinesis Bunge via ASE, and the operational parameters of ASE were optimized, such as extraction solvent, extraction temperature, static extraction time and extraction cycles. The optimized procedure employed 70% MeOH as extraction solvent, 120 degrees C of extraction temperature, 7 min of static extraction time, 60% flush volume and the extraction recoveries of the four compounds were nearly to 100% for two cycles. The HPLC conditions are as follows: SinoChrom ODS BP C18 (4.6 mm x 200 mm, 5 microm) column, acetonitrile and 0.10% phosphoric acid solution as mobile phase, flow rate is 1.0 mL min(-1), detection length of UV is 203 nm, injection volume is 10 microL. The results indicated that the developed HPLC method is simple, sensitive and reliable for the determination of four major saponins in seeds of A. chinesis Bunge with a good linearity (r2 > 0.9994), precision (relative standard deviation (R.S.D.) < 1.5%) and the recovery ranges of 95.2-97.3%. The limits of detection (LOD) of the four compounds were in the range of 0.40-0.75 microg mL(-1). This assay can be readily utilized as a quality control method for semen aesculi and other related medicinal plants.

  20. Optimization of deep eutectic solvent-based ultrasound-assisted extraction of polysaccharides from Dioscorea opposita Thunb.

    PubMed

    Zhang, Lijin; Wang, Maoshan

    2017-02-01

    In this study, deep eutectic solvents were proposed for the ultrasound-assisted extraction of polysaccharides from Dioscorea opposita Thunb. Several deep eutectic solvents were prepared for the extraction of polysaccharides, among which the deep eutectic solvent composed of choline chloride and 1,4-butanediol was proved to be suitable for the extraction. Based on the screening of single-factor experiment design and orthogonal experiment design, three experimental factors were optimized for the Box-Behnken experimental design combined with response surface methodology, which gave the optimal extraction conditions: water content of 32.89%(v/v), extraction temperature of 94.00°C, and the extraction time of 44.74min. The optimal extraction conditions could supply higher extraction yield than those of hot water extraction and water-based ultrasound-assisted extraction. Therefore, deep eutectic solvents were an excellent extraction solvent alternative to the extraction of polysaccharides from sample matrices. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Novel micronisation β-carotene using rapid expansion supercritical solution with co-solvent

    NASA Astrophysics Data System (ADS)

    Kien, Le Anh

    2017-09-01

    Rapid expansion of supercritical solution (RESS) is the most common approach of pharmaceutical pacticle forming methods using supercritical fluids. The RESS method is a technology producing a small solid product with a very narrow particle size distribution, organic solvent-free particles. This process is also simple and easy to control the operating parameters in comparision with other ways based on supercritical techniques. In this study, β-carotene, a strongly colored red-orange pigment abundant in plants and fruits, has been forming by RESS. In addition, the size and morphology effect of four different RESS parameters including co-solvent, extraction temperature, and extraction pressure and expansion nozzle temperature has surveyed. The particle size distribution has been determined by using laser diffraction experiment. SEM has conducted to analyze the surface structure, DSC and FTIR for thermal and chemical structure analysis.

  2. 21 CFR 173.280 - Solvent extraction process for citric acid.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Solvent extraction process for citric acid. 173..., Lubricants, Release Agents and Related Substances § 173.280 Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation...

  3. Supercritical fluid extraction of plant flavors and fragrances.

    PubMed

    Capuzzo, Andrea; Maffei, Massimo E; Occhipinti, Andrea

    2013-06-19

    Supercritical fluid extraction (SFE) of plant material with solvents like CO₂, propane, butane, or ethylene is a topic of growing interest. SFE allows the processing of plant material at low temperatures, hence limiting thermal degradation, and avoids the use of toxic solvents. Although today SFE is mainly used for decaffeination of coffee and tea as well as production of hop extracts on a large scale, there is also a growing interest in this extraction method for other industrial applications operating at different scales. In this review we update the literature data on SFE technology, with particular reference to flavors and fragrance, by comparing traditional extraction techniques of some industrial medicinal and aromatic crops with SFE. Moreover, we describe the biological activity of SFE extracts by describing their insecticidal, acaricidal, antimycotic, antimicrobial, cytotoxic and antioxidant properties. Finally, we discuss the process modelling, mass-transfer mechanisms, kinetics parameters and thermodynamic by giving an overview of SFE potential in the flavors and fragrances arena.

  4. Effect of solvent addition sequence on lycopene extraction efficiency from membrane neutralized caustic peeled tomato waste.

    PubMed

    Phinney, David M; Frelka, John C; Cooperstone, Jessica L; Schwartz, Steven J; Heldman, Dennis R

    2017-01-15

    Lycopene is a high value nutraceutical and its isolation from waste streams is often desirable to maximize profits. This research investigated solvent addition order and composition on lycopene extraction efficiency from a commercial tomato waste stream (pH 12.5, solids ∼5%) that was neutralized using membrane filtration. Constant volume dilution (CVD) was used to desalinate the caustic salt to neutralize the waste. Acetone, ethanol and hexane were used as direct or blended additions. Extraction efficiency was defined as the amount of lycopene extracted divided by the total lycopene in the sample. The CVD operation reduced the active alkali of the waste from 0.66 to <0.01M and the moisture content of the pulp increased from 93% to 97% (wet basis), showing the removal of caustic salts from the waste. Extraction efficiency varied from 32.5% to 94.5%. This study demonstrates a lab scale feasibility to extract lycopene efficiently from tomato processing byproducts. Published by Elsevier Ltd.

  5. Process and apparatus for solvent extraction of oil from oil-containing diatomite ore

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Karnofsky, G. B.

    1980-12-16

    A process for solvent extraction of oil from oil bearing diatomite ore and an apparatus for use therewith, wherein the ore is extracted by countercurrent decantation with a hydrocarbon solvent, solvent is recovered from the extract by multiple effect evaporation followed by stripping, and the spent diatomite is contacted with water to displace a major portion of the solvent therefrom, and solvent is recovered from the aqueous slurry of the spent diatomite by stripping with steam at superatmospheric pressure.

  6. Microbial process for the preparation of acetic acid, as well as solvent for its extraction from the fermentation broth

    DOEpatents

    Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

    2007-03-27

    A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. Solvent mixtures formed of such a modified solvent with a desired co-solvent, preferably a low boiling hydrocarbon, are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

  7. Microbial process for the preparation of acetic acid, as well as solvent for its extraction from the fermentation broth

    DOEpatents

    Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

    2004-06-22

    A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. Solvent mixtures formed of such a modified solvent with a desired co-solvent, preferably a low boiling hydrocarbon, are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

  8. 21 CFR 173.280 - Solvent extraction process for citric acid.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 3 2013-04-01 2013-04-01 false Solvent extraction process for citric acid. 173... Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

  9. 21 CFR 173.280 - Solvent extraction process for citric acid.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 3 2011-04-01 2011-04-01 false Solvent extraction process for citric acid. 173... Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

  10. 21 CFR 173.280 - Solvent extraction process for citric acid.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 3 2012-04-01 2012-04-01 false Solvent extraction process for citric acid. 173... Solvent extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

  11. A three step supercritical process to improve the dissolution rate of eflucimibe.

    PubMed

    Rodier, Elisabeth; Lochard, Hubert; Sauceau, Martial; Letourneau, Jean-Jacques; Freiss, Bernard; Fages, Jacques

    2005-10-01

    The aim of this study is to improve the dissolution properties of a poorly-soluble active substance, Eflucimibe by associating it with gamma-cyclodextrin. To achieve this objective, a new three-step process based on supercritical fluid technology has been proposed. First, Eflucimibe and cyclodextrin are co-crystallized using an anti-solvent process, dimethylsulfoxide being the solvent and supercritical carbon dioxide being the anti-solvent. Second, the co-crystallized powder is held in a static mode under supercritical conditions for several hours. This is the maturing step. Third, in a final stripping step, supercritical CO(2) is flowed through the matured powder to extract the residual solvent. The coupling of the first two steps brings about a significant synergistic effect to improve the dissolution rate of the drug. The nature of the entity obtained at the end of each step is discussed and some suggestions are made as to what happens in these operations. It is shown the co-crystallization ensures a good dispersion of both compounds and is rather insensitive to the operating parameters tested. The maturing step allows some dissolution-recrystallization to occur thus intensifying the intimate contact between the two compounds. Addition of water is necessary to make maturing effective as this is governed by the transfer properties of the medium. The stripping step allows extraction of the residual solvent but also removes some of the Eflucimibe which is the main drawback of this final stage.

  12. Conventional and Accelerated-Solvent Extractions of Green Tea (Camellia sinensis) for Metabolomics-based Chemometrics

    PubMed Central

    Kellogg, Joshua J.; Wallace, Emily D.; Graf, Tyler N.; Oberlies, Nicholas H.; Cech, Nadja B.

    2018-01-01

    Metabolomics has emerged as an important analytical technique for multiple applications. The value of information obtained from metabolomics analysis depends on the degree to which the entire metabolome is present and the reliability of sample treatment to ensure reproducibility across the study. The purpose of this study was to compare methods of preparing complex botanical extract samples prior to metabolomics profiling. Two extraction methodologies, accelerated solvent extraction and a conventional solvent maceration, were compared using commercial green tea [Camellia sinensis (L.) Kuntze (Theaceae)] products as a test case. The accelerated solvent protocol was first evaluated to ascertain critical factors influencing extraction using a D-optimal experimental design study. The accelerated solvent and conventional extraction methods yielded similar metabolite profiles for the green tea samples studied. The accelerated solvent extraction yielded higher total amounts of extracted catechins, was more reproducible, and required less active bench time to prepare the samples. This study demonstrates the effectiveness of accelerated solvent as an efficient methodology for metabolomics studies. PMID:28787673

  13. Thermal degradation of the solvent employed in the next-generation caustic-side solvent extraction process and its effect on the extraction, scrubbing, and stripping of cesium

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Roach, Benjamin D.; Williams, Neil J.; Moyer, Bruce A.

    As part of the ongoing development of the Next-Generation Caustic-Side Solvent Extraction (NGS) process, the thermal stability of the process solvent was investigated and shown to be adequate for industrial application. The solvent was thermally treated at 35 C over a period of 13 months whilst in dynamic contact with each of the aqueous phases of the current NGS process, namely SRS 15 (a highly caustic waste simulant), sodium hydroxide scrub solution (0.025 M), and boric acid strip solution (0.01 M). The effect of thermal treatment was evaluated by assessing batch extract/scrub/strip performance as a function of time, by monitoringmore » the sodium extraction capacity of the solvent, and by analysis of the solvent using electrospray mass spectrometry. Current studies indicate that the NGS solvent should be thermally robust for a period of XXX months at the Modular Caustic-Side Solvent Extraction Unit (MCU) pilot plant located at Savannah River Site. Furthermore, the guanidine suppressor appears to be the solvent component most significantly impacted by thermal treatment of the solvent, showing significant degradation over time.« less

  14. Thermal degradation of the solvent employed in the next-generation caustic-side solvent extraction process and its effect on the extraction, scrubbing, and stripping of cesium

    DOE PAGES

    Roach, Benjamin D.; Williams, Neil J.; Moyer, Bruce A.

    2015-09-02

    As part of the ongoing development of the Next-Generation Caustic-Side Solvent Extraction (NGS) process, the thermal stability of the process solvent was investigated and shown to be adequate for industrial application. The solvent was thermally treated at 35 C over a period of 13 months whilst in dynamic contact with each of the aqueous phases of the current NGS process, namely SRS 15 (a highly caustic waste simulant), sodium hydroxide scrub solution (0.025 M), and boric acid strip solution (0.01 M). The effect of thermal treatment was evaluated by assessing batch extract/scrub/strip performance as a function of time, by monitoringmore » the sodium extraction capacity of the solvent, and by analysis of the solvent using electrospray mass spectrometry. Current studies indicate that the NGS solvent should be thermally robust for a period of XXX months at the Modular Caustic-Side Solvent Extraction Unit (MCU) pilot plant located at Savannah River Site. Furthermore, the guanidine suppressor appears to be the solvent component most significantly impacted by thermal treatment of the solvent, showing significant degradation over time.« less

  15. The extraction of essential oil from patchouli leaves (Pogostemon cablin Benth) using microwave hydrodistillation and solvent-free microwave extraction methods

    NASA Astrophysics Data System (ADS)

    Putri, D. K. Y.; Kusuma, H. S.; Syahputra, M. E.; Parasandi, D.; Mahfud, M.

    2017-12-01

    Patchouli plant (Pogostemon cablin Benth) is one of the important essential oil-producing plant, contributes more than 50% of total exports of Indonesia’s essential oil. However, the extraction of patchouli oil that has been done in Indonesia is generally still used conventional methods that require enormous amount of energy, high solvent usage, and long time of extraction. Therefore, in this study, patchouli oil extraction was carried out by using microwave hydrodistillation and solvent-free microwave extraction methods. Based on this research, it is known that the extraction of patchouli oil using microwave hydrodistillation method with longer extraction time (240 min) only produced patchouli oil’s yield 1.2 times greater than solvent-free microwave extraction method which require faster extraction time (120 min). Otherwise the analysis of electric consumption and the environmental impact, the solvent-free microwave extraction method showed a smaller amount when compared with microwave hydrodistillation method. It is conclude that the use of solvent-free microwave extraction method for patchouli oil extraction is suitably method as a new green technique.

  16. New method to enhance the extraction yield of rutin from Sophora japonica using a novel ultrasonic extraction system by determining optimum ultrasonic frequency.

    PubMed

    Liao, Jianqing; Qu, Baida; Liu, Da; Zheng, Naiqin

    2015-11-01

    A new method has been proposed for enhancing extraction yield of rutin from Sophora japonica, in which a novel ultrasonic extraction system has been developed to perform the determination of optimum ultrasonic frequency by a two-step procedure. This study has systematically investigated the influence of a continuous frequency range of 20-92 kHz on rutin yields. The effects of different operating conditions on rutin yields have also been studied in detail such as solvent concentration, solvent to solid ratio, ultrasound power, temperature and particle size. A higher extraction yield was obtained at the ultrasonic frequency of 60-62 kHz which was little affected under other extraction conditions. Comparative studies between existing methods and the present method were done to verify the effectiveness of this method. Results indicated that the new extraction method gave a higher extraction yield compared with existing ultrasound-assisted extraction (UAE) and soxhlet extraction (SE). Thus, the potential use of this method may be promising for extraction of natural materials on an industrial scale in the future. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Computational and experimental analysis of the flow in an annular centrifugal contactor

    NASA Astrophysics Data System (ADS)

    Wardle, Kent E.

    The annular centrifugal contactor has been developed for solvent extraction processes for recycling used nuclear fuel. The compact size and high efficiency of these contactors have made them the choice for advanced reprocessing schemes and a key equipment for a proposed future advanced fuel cycle facility. While a sufficient base of experience exists to facilitate successful operation of current contactor technology, a more complete understanding of the fluid flow within the contactor would enable further advancements in design and operation of future units and greater confidence for use of such contactors in a variety of other solvent extraction applications. This research effort has coupled computational fluid dynamics modeling with a variety of experimental measurements and observations to provide a valid detailed analysis of the flow within the centrifugal contactor. CFD modeling of the free surface flow in the annular mixing zone using the Volume of Fluid (VOF) volume tracking method combined with Large Eddy Simulation (LES) of turbulence was found to have very good agreement with the experimental measurements and observations. A detailed study of the flow and mixing for different housing vane geometries was performed and it was found that the four straight mixing vane geometry had greater mixing for the flow rate simulated and more predictable operation over a range of low to moderate flow rates. The separation zone was also modeled providing a useful description of the flow in this region and identifying critical design features. It is anticipated that this work will form a foundation for additional efforts at improving the design and operation of centrifugal contactors and provide a framework for progress towards simulation of solvent extraction processes.

  18. Process and apparatus for solvent extraction of oil from oil-containing diatomite ore

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Karnofsky, G.B.

    1979-09-11

    A process is described for solvent extraction of oil-bearing diatomite ore. An apparatus is provided for use therewith, wherein the ore is extracted by countercurrent decantation with a hydrocarbon solvent. The solvent is recovered from the extract by multiple effect evaporation followed by stripping, and the spent diatomite is contacted with water to displace a major portion of the solvent therefrom. The solvent is recovered from the aqueous slurry of the spent diatomite by stripping with steam at superatmospheric pressure. 17 claims.

  19. Optimization of soy isoflavone extraction with different solvents using the simplex-centroid mixture design.

    PubMed

    Yoshiara, Luciane Yuri; Madeira, Tiago Bervelieri; Delaroza, Fernanda; da Silva, Josemeyre Bonifácio; Ida, Elza Iouko

    2012-12-01

    The objective of this study was to optimize the extraction of different isoflavone forms (glycosidic, malonyl-glycosidic, aglycone and total) from defatted cotyledon soy flour using the simplex-centroid experimental design with four solvents of varying polarity (water, acetone, ethanol and acetonitrile). The obtained extracts were then analysed by high-performance liquid chromatography. The profile of the different soy isoflavones forms varied with different extractions solvents. Varying the solvent or mixture used, the extraction of different isoflavones was optimized using the centroid-simplex mixture design. The special cubic model best fitted to the four solvents and its combination for soy isoflavones extraction. For glycosidic isoflavones extraction, the polar ternary mixture (water, acetone and acetonitrile) achieved the best extraction; malonyl-glycosidic forms were better extracted with mixtures of water, acetone and ethanol. Aglycone isoflavones, water and acetone mixture were best extracted and total isoflavones, the best solvents were ternary mixture of water, acetone and ethanol.

  20. Development of deep eutectic solvents applied in extraction and separation.

    PubMed

    Li, Xiaoxia; Row, Kyung Ho

    2016-09-01

    Deep eutectic solvents, as an alternative to ionic liquids, have greener credentials than ionic liquids, and have attracted considerable attention in related chemical research. Deep eutectic solvents have attracted increasing attention in chemistry for the extraction and separation of various target compounds from natural products. This review highlights the preparation of deep eutectic solvents, unique properties of deep eutectic solvents, and synthesis of deep-eutectic-solvent-based materials. On the other hand, application in the extraction and separation of deep eutectic solvents is also included in this report. In this paper, the available data and references in this field are reviewed to summarize the applications and developments of deep eutectic solvents. Based on the development of deep eutectic solvents, an exploitation of new deep eutectic solvents and deep eutectic solvents-based materials is expected to diversify into extraction and separation. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Ultrasonic Removal of Mucilage for Pressurized Liquid Extraction of Omega-3 Rich Oil from Chia Seeds (Salvia hispanica L.).

    PubMed

    Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

    2017-03-29

    Chia (Salvia hispanica L.) seeds contain an important amount of edible oil rich in omega-3 fatty acids. Fast and alternative extraction techniques based on polar solvents, such as ethanol or water, have become relevant for oil extraction in recent years. However, chia seeds also contain a large amount of soluble fiber or mucilage, which makes difficult an oil extraction process with polar solvents. For that reason, the aim of this study was to develop a gentle extraction method for mucilage in order to extract chia oil with polar solvents using pressurized liquids and compare with organic solvent extraction. The proposed mucilage extraction method, using an ultrasonic probe and only water, was optimized at mild conditions (50 °C and sonication 3 min) to guarantee the omega-3 oil quality. Chia oil extraction was performed using pressurized liquid extraction (PLE) with different solvents and their mixtures at five different extraction temperatures (60, 90, 120, 150, and 200 °C). Optimal PLE conditions were achieved with ethyl acetate or hexane at 90 °C in only 10 min of static extraction time (chia oil yield up to 30.93%). In addition, chia oils extracted with nonpolar and polar solvents by PLE were analyzed by gas chromatography-mass spectrometry (GC-MS) to evaluate fatty acid composition at different extraction conditions. Chia oil contained ∼65% of α-linolenic acid regardless of mucilage extraction method, solvent, or temperature used. Furthermore, tocopherols and tocotrienols were also analyzed by HPLC in the extracted chia oils. The mucilage removal allowed the subsequent extraction of the chia oil with polar or nonpolar solvents by PLE producing chia oil with the same fatty acid and tocopherol composition as traditional extraction.

  2. Substitution of carcinogenic solvent dichloromethane for the extraction of volatile compounds in a fat-free model food system.

    PubMed

    Cayot, Nathalie; Lafarge, Céline; Bou-Maroun, Elias; Cayot, Philippe

    2016-07-22

    Dichloromethane is known as a very efficient solvent, but, as other halogenated solvents, is recognized as a hazardous product (CMR substance). The objective of the present work is to propose substitution solvent for the extraction of volatile compounds. The most important physico-chemical parameters in the choice of an appropriate extraction solvent of volatile compounds are reviewed. Various solvents are selected on this basis and on their hazard characteristics. The selected solvents, safer than dichloromethane, are compared using the extraction efficiency of volatile compounds from a model food product able to interact with volatile compounds. Volatile compounds with different hydrophobicity are used. High extraction yields were positively correlated with high boiling points and high Log Kow values of volatile compounds. Mixtures of solvents such as azeotrope propan-2-one/cyclopentane, azeotrope ethyl acetate/ethanol, and mixture ethyl acetate/ethanol (3:1, v/v) gave higher extraction yields than those obtained with dichloromethane. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. [Determination of benzo(alpha)pyrene in food with microwave-assisted extraction].

    PubMed

    Zhou, Na; Luo, He-Dong; Li, Na; Li, Yao-Qun

    2014-03-01

    Coupling derivative technique and constant-energy synchronous fluorescence scanning technique, a method of determining benzo[alpha] pyrene in foods by second derivative constant-energy synchronous spectrofluorimetry after microwave-assisted treatment of samples was established using domestic microwave oven. The main factors of influencing the efficiency of microwave extraction were discussed, including the extraction solvent types and amounts, the microwave extraction time, microwave radiation power and cooling time. And the comparison with ultrasonic extraction was made. Low-fat food samples, which were just microwave-extracted with mixed-solvents, could be analyzed immediately by the spectrofluorimetric technique. For high-fat food samples, microwave-assisted saponification and extraction were made at the same time, thus simplifying operation steps and reducing sample analysis time. So the whole sample analysis process could be completed within one hour. This method was simple, rapid and inexpensive. In consequence, it was applied to determine benzo(a)pyrene in food with good reproducibility and the recoveries of benzo(alpha) pyrene ranged from 90.0% to 105.0% for the low fat samples and 83.3% to 94.6% for high-fat samples.

  4. A fully automated liquid–liquid extraction system utilizing interface detection

    PubMed Central

    Maslana, Eugene; Schmitt, Robert; Pan, Jeffrey

    2000-01-01

    The development of the Abbott Liquid-Liquid Extraction Station was a result of the need for an automated system to perform aqueous extraction on large sets of newly synthesized organic compounds used for drug discovery. The system utilizes a cylindrical laboratory robot to shuttle sample vials between two loading racks, two identical extraction stations, and a centrifuge. Extraction is performed by detecting the phase interface (by difference in refractive index) of the moving column of fluid drawn from the bottom of each vial containing a biphasic mixture. The integration of interface detection with fluid extraction maximizes sample throughput. Abbott-developed electronics process the detector signals. Sample mixing is performed by high-speed solvent injection. Centrifuging of the samples reduces interface emulsions. Operating software permits the user to program wash protocols with any one of six solvents per wash cycle with as many cycle repeats as necessary. Station capacity is eighty, 15 ml vials. This system has proven successful with a broad spectrum of both ethyl acetate and methylene chloride based chemistries. The development and characterization of this automated extraction system will be presented. PMID:18924693

  5. Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

    DOEpatents

    Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

    2006-07-11

    A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

  6. Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

    DOEpatents

    Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

    2002-01-01

    A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

  7. Evaluation of solvent effect on the extraction of phenolic compounds and antioxidant capacities from the berries: application of principal component analysis.

    PubMed

    Boeing, Joana Schuelter; Barizão, Erica Oliveira; E Silva, Beatriz Costa; Montanher, Paula Fernandes; de Cinque Almeida, Vitor; Visentainer, Jesuí Vergilio

    2014-01-01

    This study evaluated the effect of the solvent on the extraction of antioxidant compounds from black mulberry (Morus nigra), blackberry (Rubus ulmifolius) and strawberry (Fragaria x ananassa). Different extracts of each berry were evaluated from the determination of total phenolic content, anthocyanin content and antioxidant capacity, and data were applied to the principal component analysis (PCA) to gain an overview of the effect of the solvent in extraction method. For all the berries analyzed, acetone/water (70/30, v/v) solvent mixture was more efficient solvent in the extracting of phenolic compounds, and methanol/water/acetic acid (70/29.5/0.5, v/v/v) showed the best values for anthocyanin content. Mixtures of ethanol/water (50/50, v/v), acetone water/acetic acid (70/29.5/0.5, v/v/v) and acetone/water (50/50, v/v) presented the highest antioxidant capacities for black mulberries, blackberries and strawberries, respectively. Antioxidants extractions are extremely affected by the solvent combination used. In addition, the obtained extracts with the organic solvent-water mixtures were distinguished from the extracts obtained with pure organic solvents, through the PCA analysis.

  8. Effect of extraction method on the yield of furanocoumarins from fruits of Archangelica officinalis Hoffm.

    PubMed

    Waksmundzka-Hajnos, M; Petruczynik, A; Dragan, A; Wianowska, D; Dawidowicz, A L

    2004-01-01

    Optimal conditions for the extraction and analysis of furanocoumarins from fruits of Archangelica officinalis Hoffm. have been determined. The following extraction methods were used: exhaustive extraction in a Soxhlet apparatus, ultrasonication at 25 and 60 degrees C, microwave-assisted solvent extraction in open and closed systems, and accelerated solvent extraction (ASE). In most cases the yields of furanocoumarins were highest using the ASE method. The effects of extracting solvent, temperature and time of extraction using this method were investigated. The highest yield of furanocoumarins by ASE was obtained with methanol at 100-130 degrees C for 10 min. The extraction yields of furanocoumarins from plant material by ultrasonication at 60 degrees C and microwave-assisted solvent extraction in an open system were comparable to the extraction yields obtained in the time- and solvent-consuming exhaustive process involving the Soxhlet apparatus.

  9. Effect of Different Solvents on the Measurement of Phenolics and the Antioxidant Activity of Mulberry (Morus atropurpurea Roxb.) with Accelerated Solvent Extraction.

    PubMed

    Yang, Jiufang; Ou, XiaoQun; Zhang, Xiaoxu; Zhou, ZiYing; Ma, LiYan

    2017-03-01

    The effects of 9 different solvents on the measurement of the total phenolics and antioxidant activities of mulberry fruits were studied using accelerated solvent extraction (ASE). Sixteen to 22 types of phenolics (flavonols, flavan-3-ols, flavanol, hydroxycinnamic acids, hydroxybenzoic acids, and stilbenes) from different mulberry extracts were characterized and quantified using HPLC-MS/MS. The principal component analysis (PCA) was used to determine the suitable solvents to distinguish between different classes of phenolics. Additionally, the phenolic extraction abilities of ASE and ultrasound-assisted extraction (UAE) were compared. The highest extraction efficiency could be achieved by using 50% acidified methanol (50MA) as ASE solvents with 15.14 mg/gallic acid equivalents g dry weight of mulberry fruit. The PCA results revealed that the 50MA followed by 50% acidified acetone (50AA) was the most efficient solvent for the extraction of phenolics, particularly flavonols (627.12 and 510.31 μg/g dry weight, respectively), while water (W) was not beneficial to the extraction of all categories of phenolics. Besides, the results of 3 antioxidant capability assays (DPPH, ABTS free radical-scavenging assay, and ferric-reducing antioxidant power assay) showed that water-based organic solvents increased the antioxidant capabilities of the extracts compared with water or pure organic solvents. ASE was more suitable for the extraction of phenolics than UAE. © 2017 Institute of Food Technologists®.

  10. Switchable hydrophilicity solvents for lipid extraction from microalgae for biofuel production.

    PubMed

    Boyd, Alaina R; Champagne, Pascale; McGinn, Patrick J; MacDougall, Karen M; Melanson, Jeremy E; Jessop, Philip G

    2012-08-01

    A switchable hydrophilicity solvent (SHS) was studied for its effectiveness at extracting lipids from freeze-dried samples of Botryococcus braunii microalgae. The SHS N,N-dimethylcyclohexylamine extracted up to 22 wt.% crude lipid relative to the freeze-dried cell weight. The solvent was removed from the extract with water saturated with carbon dioxide at atmospheric pressure and recovered from the water upon de-carbonation of the mixture. Liquid chromatography-mass spectrometry (LC-MS) showed that the extracted lipids contained high concentrations of long chain tri-, di- and mono-acylglycerols, no phospholipids, and only 4-8% of residual solvent. Unlike extractions with conventional organic solvents, this new method requires neither distillation nor the use of volatile, flammable or chlorinated organic solvents. Copyright © 2012 Elsevier Ltd. All rights reserved.

  11. Terra-Kleen Response Group, Inc. Solvent Extraction Technology Rapid Commercialization Initiative Report

    EPA Science Inventory

    Terra-Kleen Response Group Inc. (Terra-Kleen), has commercialized a solvent extraction technology that uses a proprietary extraction solvent to transfer organic constituents from soil to a liquid phase in a batch process at ambient temperatures. The proprietary solvent has a rel...

  12. Integration of ceramic membrane and compressed air-assisted solvent extraction (CASX) for metal recovery.

    PubMed

    Li, Chi-Wang; Chiu, Chun-Hao; Lee, Yu-Cheng; Chang, Chia-Hao; Lee, Yu-Hsun; Chen, Yi-Ming

    2010-01-01

    In our previous publications, compressed air-assisted solvent extraction process (CASX) was developed and proved to be kinetically efficient process for metal removal. In the current study, CASX with a ceramic MF membrane integrated for separation of spent solvent was employed to remove and recover metal from wastewater. MF was operated either in crossflow mode or dead-end with intermittent flushing mode. Under crossflow mode, three distinct stages of flux vs. TMP (trans-membrane pressure) relationship were observed. In the first stage, flux increases with increasing TMP which is followed by the stage of stable flux with increasing TMP. After reaching a threshold TMP which is dependent of crossflow velocity, flux increases again with increasing TMP. At the last stage, solvent was pushed through membrane pores as indicated by increasing permeate COD. In dead-end with intermittent flushing mode, an intermittent flushing flow (2 min after a 10-min or a 30-min dead-end filtration) was incorporated to reduce membrane fouling by flush out MSAB accumulated on membrane surface. Effects of solvent concentration and composition were also investigated. Solvent concentrations ranging from 0.1 to 1% (w/w) have no adverse effect in terms of membrane fouling. However, solvent composition, i.e. D(2)EHPA/kerosene ratio, shows impact on membrane fouling. The type of metal extractants employed in CASX has significant impact on both membrane fouling and the quality of filtrate due to the differences in their viscosity and water solubility. Separation of MSAB was the limiting process controlling metal removal efficiency, and the removal efficiency of Cd(II) and Cr(VI) followed the same trend as that for COD.

  13. Automation of static and dynamic non-dispersive liquid phase microextraction. Part 1: Approaches based on extractant drop-, plug-, film- and microflow-formation.

    PubMed

    Alexovič, Michal; Horstkotte, Burkhard; Solich, Petr; Sabo, Ján

    2016-02-04

    Simplicity, effectiveness, swiftness, and environmental friendliness - these are the typical requirements for the state of the art development of green analytical techniques. Liquid phase microextraction (LPME) stands for a family of elegant sample pretreatment and analyte preconcentration techniques preserving these principles in numerous applications. By using only fractions of solvent and sample compared to classical liquid-liquid extraction, the extraction kinetics, the preconcentration factor, and the cost efficiency can be increased. Moreover, significant improvements can be made by automation, which is still a hot topic in analytical chemistry. This review surveys comprehensively and in two parts the developments of automation of non-dispersive LPME methodologies performed in static and dynamic modes. Their advantages and limitations and the reported analytical performances are discussed and put into perspective with the corresponding manual procedures. The automation strategies, techniques, and their operation advantages as well as their potentials are further described and discussed. In this first part, an introduction to LPME and their static and dynamic operation modes as well as their automation methodologies is given. The LPME techniques are classified according to the different approaches of protection of the extraction solvent using either a tip-like (needle/tube/rod) support (drop-based approaches), a wall support (film-based approaches), or microfluidic devices. In the second part, the LPME techniques based on porous supports for the extraction solvent such as membranes and porous media are overviewed. An outlook on future demands and perspectives in this promising area of analytical chemistry is finally given. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Conventional and accelerated-solvent extractions of green tea (camellia sinensis) for metabolomics-based chemometrics.

    PubMed

    Kellogg, Joshua J; Wallace, Emily D; Graf, Tyler N; Oberlies, Nicholas H; Cech, Nadja B

    2017-10-25

    Metabolomics has emerged as an important analytical technique for multiple applications. The value of information obtained from metabolomics analysis depends on the degree to which the entire metabolome is present and the reliability of sample treatment to ensure reproducibility across the study. The purpose of this study was to compare methods of preparing complex botanical extract samples prior to metabolomics profiling. Two extraction methodologies, accelerated solvent extraction and a conventional solvent maceration, were compared using commercial green tea [Camellia sinensis (L.) Kuntze (Theaceae)] products as a test case. The accelerated solvent protocol was first evaluated to ascertain critical factors influencing extraction using a D-optimal experimental design study. The accelerated solvent and conventional extraction methods yielded similar metabolite profiles for the green tea samples studied. The accelerated solvent extraction yielded higher total amounts of extracted catechins, was more reproducible, and required less active bench time to prepare the samples. This study demonstrates the effectiveness of accelerated solvent as an efficient methodology for metabolomics studies. Copyright © 2017. Published by Elsevier B.V.

  15. Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples.

    PubMed

    Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

    2008-03-03

    The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 microL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 microgL(-1) with a detection limit of 0.5 microgL(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 microgL(-1) of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 microgL(-1) ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method.

  16. Attractive design: an elution solvent optimization platform for magnetic-bead-based fractionation using digital microfluidics and design of experiments.

    PubMed

    Lafrenière, Nelson M; Mudrik, Jared M; Ng, Alphonsus H C; Seale, Brendon; Spooner, Neil; Wheeler, Aaron R

    2015-04-07

    There is great interest in the development of integrated tools allowing for miniaturized sample processing, including solid phase extraction (SPE). We introduce a new format for microfluidic SPE relying on C18-functionalized magnetic beads that can be manipulated in droplets in a digital microfluidic platform. This format provides the opportunity to tune the amount (and potentially the type) of stationary phase on-the-fly, and allows the removal of beads after the extraction (to enable other operations in same device-space), maintaining device reconfigurability. Using the new method, we employed a design of experiments (DOE) operation to enable automated on-chip optimization of elution solvent composition for reversed phase SPE of a model system. Further, conditions were selected to enable on-chip fractionation of multiple analytes. Finally, the method was demonstrated to be useful for online cleanup of extracts from dried blood spot (DBS) samples. We anticipate this combination of features will prove useful for separating a wide range of analytes, from small molecules to peptides, from complex matrices.

  17. A comparison of accelerated solvent extraction, Soxhlet extraction, and ultrasonic-assisted extraction for analysis of terpenoids and sterols in tobacco.

    PubMed

    Shen, Jinchao; Shao, Xueguang

    2005-11-01

    The performance of accelerated solvent extraction in the analysis of terpenoids and sterols in tobacco samples was investigated and compared with those of Soxhlet extraction and ultrasonically assisted extraction with respect to yield, extraction time, reproducibility and solvent consumption. The results indicate that although the highest yield was achieved by Soxhlet extraction, ASE appears to be a promising alternative to classical methods since it is faster and uses less solvent, especially when applied to the investigation of large batch tobacco samples. However, Soxhlet extraction is still the preferred method for analyzing sterols since it gives a higher extraction efficiency than other methods.

  18. [Advances in studies on multi-stage countercurrent extraction technology in traditional Chinese medicine].

    PubMed

    Xie, Zhi-Peng; Liu, Xue-Song; Chen, Yong; Cai, Ming; Qu, Hai-Bin; Cheng, Yi-Yu

    2007-05-01

    Multi-stage countercurrent extraction technology, integrating solvent extraction, repercolation with dynamic and countercurrent extraction, is a novel extraction technology for the traditional Chinese medicine. This solvent-saving, energy-saving and high-extraction-efficiency technology can at the most drive active compounds to diffuse from the herbal materials into the solvent stage by stage by creating concentration differences between the herbal materials and the solvents. This paper reviewed the basic principle, the influence factors and the research progress and trends of the equipments and the application of the multi-stage countercurrent extraction.

  19. Phenolic Extracts from Wild Olive Leaves and Their Potential as Edible Oils Antioxidants

    PubMed Central

    Lafka, Theodora-Ioanna; Lazou, Andriana E.; Sinanoglou, Vassilia J.; Lazos, Evangelos S.

    2013-01-01

    The kinetics solid-liquid extraction of phenolics from wild olive leaves was elaborated using different mathematical models (Peleg, second order, Elovich, and power law model). As solvents, methanol, ethanol, ethanol:water 1:1, n-propanol, isopropanol and ethyl acetate were used. The second order model best described the solvent extraction process, followed by the Elovich model. The most effective solvent was ethanol with optimum phenol extraction conditions 180 min, solvent to sample ratio 5:1 v/w and pH 2. Ethanol extract exhibited the highest antiradical activity among solvent and supercritical fluid extraction (SFE) extracts, which in addition showed the highest antioxidant capacity compared to synthetic and natural food antioxidants such as BHT, ascorbyl palmitate and vitamin E. Antioxidant potential of SFE extract was quite high, although its phenolic potential was not. Leaf extracts were proven to be good protectors for olive and sunflower oils at levels of 150 ppm. PMID:28239093

  20. Determination of 129I in environmental samples by AMS and NAA using an anion exchange resin disk

    NASA Astrophysics Data System (ADS)

    Suzuki, Takashi; Banba, Shigeru; Kitamura, Toshikatsu; Kabuto, Shoji; Isogai, Keisuke; Amano, Hikaru

    2007-06-01

    We have developed a new extraction method for the measurement of 129I by accelerator mass spectrometry (AMS) utilizing an anion exchange resin disk. In comparison to traditional methods such as solvent extraction and ion exchange, this method provides for simple and quick sample handling. This extraction method was tested on soil, seaweed and milk samples, but because of disk clogging, the milk samples and some of the seaweed could not be applied successfully. Using this new extraction method to prepare samples for AMS analysis produced isotope ratios of iodine in good agreement with neutron activation analysis (NAA). The disk extraction method which take half an hour is faster than previous techniques, such as solvent extraction or ion exchange which take a few hours. The combination of the disk method and the AMS measurement is a powerful tool for the determination of 129I. Furthermore, these data will be available for the environmental monitoring before and during the operation of a new nuclear fuel reprocessing plant in Japan.

  1. Step-wise supercritical extraction of carbonaceous residua

    DOEpatents

    Warzinski, Robert P.

    1987-01-01

    A method of fractionating a mixture containing high boiling carbonaceous material and normally solid mineral matter includes processing with a plurality of different supercritical solvents. The mixture is treated with a first solvent of high critical temperature and solvent capacity to extract a large fraction as solute. The solute is released as liquid from solvent and successively treated with other supercritical solvents of different critical values to extract fractions of differing properties. Fractionation can be supplemented by solute reflux over a temperature gradient, pressure let down in steps and extractions at varying temperature and pressure values.

  2. Comparison of extraction methods for quantifying vitamin E from animal tissues.

    PubMed

    Xu, Zhimin

    2008-12-01

    Four extraction methods: (1) solvent (SOL), (2) ultrasound assisted solvent (UA), (3) saponification and solvent (SP), and (4) saponification and ultrasound assisted solvent (SP-UA), were used in sample preparation for quantifying vitamin E (tocopherols) in chicken liver and plasma samples. The extraction yields of SOL, UA, SP, and SP-UA methods obtained by adding delta-tocopherol as internal reference were 95%, 104%, 65%, and 62% for liver and 98%, 103%, 97%, and 94% for plasma, respectively. The methods with saponification significantly affected the stabilities of tocopherols in liver samples. The measured values of alpha- and gamma-tocopherols using the solvent only extraction (SOL) method were much lower than that using any of the other extraction methods. This indicated that less of the tocopherols in those samples were in a form that could be extracted directly by solvent. The measured value of alpha-tocopherol in the liver sample using the ultrasound assisted solvent (UA) method was 1.5-2.5 times of that obtained from the saponification and solvent (SP) method. The differences in measured values of tocopherols in the plasma samples by using the two methods were not significant. However, the measured value of the saponification and ultrasound assisted solvent (SP-UA) method was lower than either the saponification and solvent (SP) or the ultrasound assisted solvent (UA) method. Also, the reproducibility of the ultrasound assisted solvent (UA) method was greater than any of the saponification methods. Compared with the traditional saponification method, the ultrasound assisted solvent method could effectively extract tocopherols from sample matrix without any chemical degradation reactions, especially for complex animal tissue such as liver.

  3. Effect of Organic Solvents on Microalgae Growth, Metabolism and Industrial Bioproduct Extraction: A Review.

    PubMed

    Miazek, Krystian; Kratky, Lukas; Sulc, Radek; Jirout, Tomas; Aguedo, Mario; Richel, Aurore; Goffin, Dorothee

    2017-07-04

    In this review, the effect of organic solvents on microalgae cultures from molecular to industrial scale is presented. Traditional organic solvents and solvents of new generation-ionic liquids (ILs), are considered. Alterations in microalgal cell metabolism and synthesis of target products (pigments, proteins, lipids), as a result of exposure to organic solvents, are summarized. Applications of organic solvents as a carbon source for microalgal growth and production of target molecules are discussed. Possible implementation of various industrial effluents containing organic solvents into microalgal cultivation media, is evaluated. The effect of organic solvents on extraction of target compounds from microalgae is also considered. Techniques for lipid and carotenoid extraction from viable microalgal biomass (milking methods) and dead microalgal biomass (classical methods) are depicted. Moreover, the economic survey of lipid and carotenoid extraction from microalgae biomass, by means of different techniques and solvents, is conducted.

  4. Effect of Organic Solvents on Microalgae Growth, Metabolism and Industrial Bioproduct Extraction: A Review

    PubMed Central

    Miazek, Krystian; Sulc, Radek; Jirout, Tomas; Aguedo, Mario; Goffin, Dorothee

    2017-01-01

    In this review, the effect of organic solvents on microalgae cultures from molecular to industrial scale is presented. Traditional organic solvents and solvents of new generation-ionic liquids (ILs), are considered. Alterations in microalgal cell metabolism and synthesis of target products (pigments, proteins, lipids), as a result of exposure to organic solvents, are summarized. Applications of organic solvents as a carbon source for microalgal growth and production of target molecules are discussed. Possible implementation of various industrial effluents containing organic solvents into microalgal cultivation media, is evaluated. The effect of organic solvents on extraction of target compounds from microalgae is also considered. Techniques for lipid and carotenoid extraction from viable microalgal biomass (milking methods) and dead microalgal biomass (classical methods) are depicted. Moreover, the economic survey of lipid and carotenoid extraction from microalgae biomass, by means of different techniques and solvents, is conducted. PMID:28677659

  5. Optimization of antibacterial activity by Gold-Thread (Coptidis Rhizoma Franch) against Streptococcus mutans using evolutionary operation-factorial design technique.

    PubMed

    Choi, Ung-Kyu; Kim, Mi-Hyang; Lee, Nan-Hee

    2007-11-01

    This study was conducted to find the optimum extraction condition of Gold-Thread for antibacterial activity against Streptococcus mutans using The evolutionary operation-factorial design technique. Higher antibacterial activity was achieved in a higher extraction temperature (R2 = -0.79) and in a longer extraction time (R2 = -0.71). Antibacterial activity was not affected by differentiation of the ethanol concentration in the extraction solvent (R2 = -0.12). The maximum antibacterial activity of clove against S. mutans determined by the EVOP-factorial technique was obtained at 80 degrees C extraction temperature, 26 h extraction time, and 50% ethanol concentration. The population of S. mutans decreased from 6.110 logCFU/ml in the initial set to 4.125 logCFU/ml in the third set.

  6. Green extraction of grape skin phenolics by using deep eutectic solvents.

    PubMed

    Cvjetko Bubalo, Marina; Ćurko, Natka; Tomašević, Marina; Kovačević Ganić, Karin; Radojčić Redovniković, Ivana

    2016-06-01

    Conventional extraction techniques for plant phenolics are usually associated with high organic solvent consumption and long extraction times. In order to establish an environmentally friendly extraction method for grape skin phenolics, deep eutectic solvents (DES) as a green alternative to conventional solvents coupled with highly efficient microwave-assisted and ultrasound-assisted extraction methods (MAE and UAE, respectively) have been considered. Initially, screening of five different DES for proposed extraction was performed and choline chloride-based DES containing oxalic acid as a hydrogen bond donor with 25% of water was selected as the most promising one, resulting in more effective extraction of grape skin phenolic compounds compared to conventional solvents. Additionally, in our study, UAE proved to be the best extraction method with extraction efficiency superior to both MAE and conventional extraction method. The knowledge acquired in this study will contribute to further DES implementation in extraction of biologically active compounds from various plant sources. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. Optimization of the Ethanol Recycling Reflux Extraction Process for Saponins Using a Design Space Approach

    PubMed Central

    Gong, Xingchu; Zhang, Ying; Pan, Jianyang; Qu, Haibin

    2014-01-01

    A solvent recycling reflux extraction process for Panax notoginseng was optimized using a design space approach to improve the batch-to-batch consistency of the extract. Saponin yields, total saponin purity, and pigment yield were defined as the process critical quality attributes (CQAs). Ethanol content, extraction time, and the ratio of the recycling ethanol flow rate and initial solvent volume in the extraction tank (RES) were identified as the critical process parameters (CPPs) via quantitative risk assessment. Box-Behnken design experiments were performed. Quadratic models between CPPs and process CQAs were developed, with determination coefficients higher than 0.88. As the ethanol concentration decreases, saponin yields first increase and then decrease. A longer extraction time leads to higher yields of the ginsenosides Rb1 and Rd. The total saponin purity increases as the ethanol concentration increases. The pigment yield increases as the ethanol concentration decreases or extraction time increases. The design space was calculated using a Monte-Carlo simulation method with an acceptable probability of 0.90. Normal operation ranges to attain process CQA criteria with a probability of more than 0.914 are recommended as follows: ethanol content of 79–82%, extraction time of 6.1–7.1 h, and RES of 0.039–0.040 min−1. Most of the results of the verification experiments agreed well with the predictions. The verification experiment results showed that the selection of proper operating ethanol content, extraction time, and RES within the design space can ensure that the CQA criteria are met. PMID:25470598

  8. Evaluation of various solvent systems for lipid extraction from wet microalgal biomass and its effects on primary metabolites of lipid-extracted biomass.

    PubMed

    Ansari, Faiz Ahmad; Gupta, Sanjay Kumar; Shriwastav, Amritanshu; Guldhe, Abhishek; Rawat, Ismail; Bux, Faizal

    2017-06-01

    Microalgae have tremendous potential to grow rapidly, synthesize, and accumulate lipids, proteins, and carbohydrates. The effects of solvent extraction of lipids on other metabolites such as proteins and carbohydrates in lipid-extracted algal (LEA) biomass are crucial aspects of algal biorefinery approach. An effective and economically feasible algae-based oil industry will depend on the selection of suitable solvent/s for lipid extraction, which has minimal effect on metabolites in lipid-extracted algae. In current study, six solvent systems were employed to extract lipids from dry and wet biomass of Scenedesmus obliquus. To explore the biorefinery concept, dichloromethane/methanol (2:1 v/v) was a suitable solvent for dry biomass; it gave 18.75% lipids (dry cell weight) in whole algal biomass, 32.79% proteins, and 24.73% carbohydrates in LEA biomass. In the case of wet biomass, in order to exploit all three metabolites, isopropanol/hexane (2:1 v/v) is an appropriate solvent system which gave 7.8% lipids (dry cell weight) in whole algal biomass, 20.97% proteins, and 22.87% carbohydrates in LEA biomass. Graphical abstract: Lipid extraction from wet microalgal biomass and biorefianry approach.

  9. Highly efficient extraction of anthocyanins from grape skin using deep eutectic solvents as green and tunable media.

    PubMed

    Jeong, Kyung Min; Zhao, Jing; Jin, Yan; Heo, Seong Rok; Han, Se Young; Yoo, Da Eun; Lee, Jeongmi

    2015-12-01

    Deep eutectic solvents (DESs) were investigated as tunable, environmentally benign, yet superior extraction media to enhance the extraction of anthocyanins from grape skin, which is usually discarded as waste. Ten DESs containing choline chloride as hydrogen bond acceptor combined with different hydrogen bond donors were screened for high extraction efficiencies based on the anthocyanin extraction yields. As a result, citric acid, D-(+)-maltose, and fructose were selected as the effective DES components, and the newly designed DES, CM-6 that is composed of citric acid and D-(+)-maltose at 4:1 molar ratio, exhibited significantly higher levels of anthocyanin extraction yields than conventional extraction solvents such as 80% aqueous methanol. The final extraction method was established based on the ultrasound-assisted extraction under conditions optimized using response surface methodology. Its extraction yields were double or even higher than those of conventional methods that are time-consuming and use volatile organic solvents. Our method is truly a green method for anthocyanin extraction with great extraction efficiency using a minimal amount of time and solvent. Moreover, this study suggested that grape skin, the by-products of grape juice processing, could serve as a valuable source for safe, natural colorants or antioxidants by use of the eco-friendly extraction solvent, CM-6.

  10. EXTRACTION AND DETECTION OF ARSENICALS IN SEAWEED VIA ACCELERATED SOLVENT EXTRACTION WITH ION CHROMATOGRAPHIC SEPARATION AND ICP-MS DETECTION

    EPA Science Inventory

    An accelerated solvent extraction (ASE) device was evaluated as a semi-automated means of extracting arsenicals from ribbon kelp. Objective was to investigate effect of experimentally controllable ASE parameters (pressure, temperature, static time and solvent composition) on extr...

  11. Supercritical solvent extraction of oil sand bitumen

    NASA Astrophysics Data System (ADS)

    Imanbayev, Ye. I.; Ongarbayev, Ye. K.; Tileuberdi, Ye.; Mansurov, Z. A.; Golovko, A. K.; Rudyk, S.

    2017-08-01

    The supercritical solvent extraction of bitumen from oil sand studied with organic solvents. The experiments were performed in autoclave reactor at temperature above 255 °C and pressure 29 atm with stirring for 6 h. The reaction resulted in the formation of coke products with mineral part of oil sands. The remaining products separated into SARA fractions. The properties of the obtained products were studied. The supercritical solvent extraction significantly upgraded extracted natural bitumen.

  12. Solvent selection in ultrasonic-assisted emulsification microextraction: Comparison between high- and low-density solvents by means of novel type of extraction vessel.

    PubMed

    Nojavan, Saeed; Gorji, Tayebeh; Davarani, Saied Saeed Hosseiny; Morteza-Najarian, Amin

    2014-08-01

    There are numerous published reports about dispersive liquid phase microextraction of the wide range of substances, however, till now no broadly accepted systematic and purpose oriented selection of extraction solvent has been proposed. Most works deal with the optimization of available solvents without adequate pre-consideration of properness. In this study, it is tried to compare the performances of low- and high-density solvents at the same conditions by means of novel type of extraction vessel with head and bottom conical shape. Extraction efficiencies of seven basic pharmaceutical compounds using eighteen common organic solvents were studied in this work. It was much easier to work with high-density solvents and they mostly showed better performances. This work shows that although exact predicting the performance of the solvents is multifaceted case but the pre-consideration of initial selection of solvents with attention to the physiochemical properties of the desired analytes is feasible and promising. Finally, the practicality of the method for extraction from urine and plasma samples was investigated. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Separation of Gadolinium (Gd) using Synergic Solvent Mixed Topo-D2EHPA with Extraction Method.

    NASA Astrophysics Data System (ADS)

    Effendy, N.; Basuki, K. T.; Biyantoro, D.; Perwira, N. K.

    2018-04-01

    The main problem to obtain Gd with high purity is the similarity of chemical properties and physical properties with the other rare earth elements (REE) such as Y and Dy, it is necessary to do separation by the extraction process. The purpose of this research to determine the best solvent type, amount of solvent, feed and solvent ratio in the Gd extraction process, to determine the rate order and the value of the rate constant of Gd concentration based on experimental data of aqueous phase concentration as a function of time and to know the effect of temperature on the reaction speed constant. This research was conducted on variation of solvent, amount of solvent, feed and solvent ratio in the extraction process of Gd separation, extraction time to determine the order value and the rate constant of Gd concentration in extraction process based on the aqueous phase concentration data as a function of time, to the rate constant of decreasing concentration of Gd. Based on the calculation results, the solvent composition was obtained with the best feed to separate the rare earth elements Gd in the extraction process is 1 : 4 with 15% concentration of TOPO and 10% concentration of D2EHPA. The separation process of Gd using extraction method by solvent TOPO-D2EHPA 2 : 1 comparison is better than single solvent D2EHPA / TOPO because of the synergistic effect. The rate order of separation process of Gd follows order 1. The Arrhenius Gd equation becomes k = 1.46 x 10-7 exp (-6.96 kcal / mol / RT).

  14. Terpenes as green solvents for extraction of oil from microalgae.

    PubMed

    Dejoye Tanzi, Celine; Abert Vian, Maryline; Ginies, Christian; Elmaataoui, Mohamed; Chemat, Farid

    2012-07-09

    Herein is described a green and original alternative procedure for the extraction of oil from microalgae. Extractions were carried out using terpenes obtained from renewable feedstocks as alternative solvents instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using Soxhlet extraction followed by the elimination of the solvent from the medium using Clevenger distillation in the second step. Oils extracted from microalgae were compared in terms of qualitative and quantitative determination. No significant difference was obtained between each extract, allowing us to conclude that the proposed method is green, clean and efficient.

  15. Evaluation of the essential oil of Foeniculum vulgare Mill (fennel) fruits extracted by three different extraction methods by GC/MS.

    PubMed

    Hammouda, Faiza M; Saleh, Mahmoud A; Abdel-Azim, Nahla S; Shams, Khaled A; Ismail, Shams I; Shahat, Abdelaaty A; Saleh, Ibrahim A

    2014-01-01

    Hydrodistillation (HD) and steam-distillation, or solvent extraction methods of essential oils have some disadvantages like thermal decomposition of extracts, its contamination with solvent or solvent residues and the pollution of residual vegetal material with solvent which can be also an environmental problem. Thus, new green techniques, such as supercritical fluid extraction and microwave assisted techniques, are potential solutions to overcome these disadvantages. The aim of this study was to evaluate the essential oil of Foeniculum vulgare subsp. Piperitum fruits extracted by three different extraction methods viz. Supercritical fluid extraction (SFE) using CO2, microwave-assisted extraction (MAE) and hydro-distillation (HD) using gas chromatography-mass spectrometry (GC/MS). The results revealed that both MAE and SFE enhanced the extraction efficiency of the interested components. MAE gave the highest yield of oil as well as higher percentage of Fenchone (28%), whereas SFE gave the highest percentage of anethol (72%). Microwave-assisted extraction (MAE) and supercritical fluid extraction (SFE) not only enhanced the essential oil extraction but also saved time, reduced the solvents use and produced, ecologically, green technologies.

  16. Deep Eutectic Solvents as Efficient Media for the Extraction and Recovery of Cynaropicrin from Cynara cardunculus L. Leaves.

    PubMed

    de Faria, Emanuelle L P; do Carmo, Rafael S; Cláudio, Ana Filipa M; Freire, Carmen S R; Freire, Mara G; Silvestre, Armando J D

    2017-10-30

    In recent years a high demand for natural ingredients with nutraceutical properties has been witnessed, for which the development of more environmentally-friendly and cost-efficient extraction solvents and methods play a primary role. In this perspective, in this work, the application of deep eutectic solvents (DES), composed of quaternary ammonium salts and organic acids, as alternative solvents for the extraction of cynaropicrin from Cynara cardunculus L. leaves was studied. After selecting the most promising DES, their aqueous solutions were investigated, allowing to obtain a maximum cynaropicrin extraction yield of 6.20 wt %, using 70 wt % of water. The sustainability of the extraction process was further optimized by carrying out several extraction cycles, reusing either the biomass or the aqueous solutions of DES. A maximum cynaropicrin extraction yield of 7.76 wt % by reusing the solvent, and of 8.96 wt % by reusing the biomass, have been obtained. Taking advantage of the cynaropicrin solubility limit in aqueous solutions, water was added as an anti-solvent, allowing to recover 73.6 wt % of the extracted cynaropicrin. This work demonstrates the potential of aqueous solutions of DES for the extraction of value-added compounds from biomass and the possible recovery of both the target compounds and solvents.

  17. Comparison of extraction techniques and modeling of accelerated solvent extraction for the authentication of natural vanilla flavors.

    PubMed

    Cicchetti, Esmeralda; Chaintreau, Alain

    2009-06-01

    Accelerated solvent extraction (ASE) of vanilla beans has been optimized using ethanol as a solvent. A theoretical model is proposed to account for this multistep extraction. This allows the determination, for the first time, of the total amount of analytes initially present in the beans and thus the calculation of recoveries using ASE or any other extraction technique. As a result, ASE and Soxhlet extractions have been determined to be efficient methods, whereas recoveries are modest for maceration techniques and depend on the solvent used. Because industrial extracts are obtained by many different procedures, including maceration in various solvents, authenticating vanilla extracts using quantitative ratios between the amounts of vanilla flavor constituents appears to be unreliable. When authentication techniques based on isotopic ratios are used, ASE is a valid sample preparation technique because it does not induce isotopic fractionation.

  18. Ultrasonic-assisted extraction of essential oil from Botryophora geniculate using different extracting solvents

    NASA Astrophysics Data System (ADS)

    Habibullah, Wilfred, Cecilia Devi

    2016-11-01

    This study compares the performance of ionic liquids to substitute conventional solvents (hexane, dichloromethane and methanol) to extract essential oil from Botryophora geniculate plant. Two different Ionic liquids ([C3MIM][Ac], [C4MIM][Ac]) with co-solvent diethyl ether were used in the ultrasonic-assisted extraction. The effect of various experimental conditions such as time, temperature and solvent were studied. Gas chromatography-mass spectroscopy (GC-MS) was used to analyze essential oils. The results showed that in ultrasonic-assisted extraction using ionic liquids as a solvent gave highest yield (9.5%) in 30 min at temperature 70°C. When using ultrasonic bath with hexane, dichloromethane and methanol, yields was (3.34%), (3.6%) and (3.81%) at 90 min, respectively were obtained. The ultrasonic-assisted extraction under optimal extraction conditions (time 30 min, temperature of 70°C) gave the best yield for the essential oil extraction.

  19. A green deep eutectic solvent dispersive liquid-liquid micro-extraction (DES-DLLME) for the UHPLC-PDA determination of oxyprenylated phenylpropanoids in olive, soy, peanuts, corn, and sunflower oil.

    PubMed

    Ferrone, Vincenzo; Genovese, Salvatore; Carlucci, Maura; Tiecco, Matteo; Germani, Raimondo; Preziuso, Francesca; Epifano, Francesco; Carlucci, Giuseppe; Taddeo, Vito Alessandro

    2018-04-15

    A green dispersive liquid-liquid microextraction (DLLME) using deep eutectic solvent (DES) as the extracting solvent has been developed and applied for the simultaneous quantification of ferulic acid, umbelliferone, boropinic acid, 7-isopentenyloxycoumarin, 4'-geranyloxyferulic acid (GOFA), and auraptene in some vegetable oils using ultra high performance liquid chromatography (UHPLC) with photodiode array detection (PDA). All parameters in the extraction step, including selection and loading of both extracting and dispersing solvents, amount of both extractant and disperser solvent were investigated and optimized. PhAA/TMG DES achieved higher recovery and enrichment factor compared to other DESs. The validated method showed good linearity with correlation coefficients, r 2 >0.9990 for all the analytes. Furthermore, this is the first time that eco-friendly solvents are used for the extraction of oxyprenylated phenylpropanoids and the corresponding extract analyzed with ultra high performance liquid chromatography with photodiode array detection. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Process chemistry of americium-241

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Navratil, J.D.

    1983-01-01

    Americium-241, one of the most useful actinide isotopes, is produced as a by-product of plutonium scrap recovery operations. Rocky Flats has supplied high purity americium oxide to the US Department of Energy's Isotope Pool since 1962. Over the years, the evolving separation and purification processes have included such diverse operations as ion exchange, aqueous precipitation, and both molten-salt and organic-solvent extraction.

  1. Solvent and process for recovery of hydroxide from aqueous mixtures

    DOEpatents

    Moyer, Bruce A.; Chambliss, C. Kevin; Bonnesen, Peter V.; Keever, Tamara J.

    2001-01-01

    Hydroxide values and associated alkali metal may be recovered from alkaline aqueous solutions using classes of fluorinated alcohols in a water immiscible solvent. The alcohols are characterized by fluorine substituents which are proximal to the acidic alcohol protons and are located to adjust the acidity of the extractant and the solubility of the extractant in the solvent. A method for stripping the extractant and solvent to regenerate the extractant and purified aqueous hydroxide solution is described.

  2. Solvent extraction of diatomite

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Williams, W.

    1984-07-24

    There is provided a method of extracting hydrocarbons from a diatomite ore. The particle size of the ore is first reduced to form a processed ore. The processed ore is then mixed with a substantially irregular granular material to form an unstratified ore mixture having increased permeability to an extracting solvent. The unstratified ore mixture is then permeated with an extracting solvent to obtain a hydrocarbon-solvent stream from which hydrocarbons are subsequently separated. The irregular granular material may be sand.

  3. Improved Supercritical-Solvent Extraction of Coal

    NASA Technical Reports Server (NTRS)

    Compton, L.

    1982-01-01

    Raw coal upgraded by supercritical-solvent extraction system that uses two materials instead of one. System achieved extraction yields of 20 to 49 weight percent. Single-solvent yields are about 25 weight percent. Experimental results show extraction yields may be timedependent. Observed decreases in weight of coal agreed well with increases in ash content of residue.

  4. 21 CFR 173.280 - Solvent extraction process for citric acid.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 3 2010-04-01 2009-04-01 true Solvent extraction process for citric acid. 173.280... extraction process for citric acid. A solvent extraction process for recovery of citric acid from conventional Aspergillus niger fermentation liquor may be safely used to produce food-grade citric acid in...

  5. Physico-chemical separation process of nanoparticles in cosmetic formulations

    NASA Astrophysics Data System (ADS)

    Retamal Marín, R. R.; Babick, F.; Stintz, M.

    2017-06-01

    Understanding the world of nanoparticles, especially their interactions with the environment, begins with their correct detection and successive quantification. To achieve this purpose, one needs to perform correctly developed standard operating procedures (SOPs). Furthermore, the study of nanoparticles frequently requires their characterisation in complex media (e.g. in cosmetic formulations). In this study, a set of sample preparation procedures for the detection and extraction of NMs in emulsion-based formulations is proposed and their performance for model and real-life products is discussed. A separation or extraction of lipid phases is achieved by means of organic solvents. The polarity of the lipid phases is decisive for selecting an optimum solvent. The use of the Hansen Solubility Parameters (HSP) may clearly support this decision.

  6. Extraction of aucubin from seeds of Eucommia ulmoides Oliv. using supercritical carbon dioxide.

    PubMed

    Li, Hui; Hu, Jiangyu; Ouyang, Hui; Li, Yanan; Shi, Hui; Ma, Chengjin; Zhang, Yongkang

    2009-01-01

    Supercritical CO2 was used as solvent for the extraction of aucubin from the seeds of Eucommia ulmoides Oliv. The co-solvent composition was tested and extraction conditions were optimized. Results showed that the best co-solvent was a water-ethanol mixture (1 + 3, v/v), and the highest yield was obtained when the extraction was performed under 26 MPa at extraction and separation temperatures of 55 and 30 degrees C for 120 min, using 6 mL co-solvent/g material at a CO2 flow rate of 20 L/h. In a comparison of the supercritical CO2 and Soxhlet extraction methods, the Soxhlet method needed 3 h to extract 10 g material, whereas the supercritical CO2 extraction technique needed only 2 h to extract 100 g material, thus showing a high extraction capability. The supercritical CO2 extraction produced a higher yield, with a lower cost for the extraction. Owing to the advantages of low extraction temperature, high yield, and ease of separating the product from the solvent, supercritical CO2 extraction is likely to be developed into an ideal technique for the extraction of aucubin, a compound with thermal instability, from the seeds of this plant.

  7. Process for solvent refining of coal using a denitrogenated and dephenolated solvent

    DOEpatents

    Garg, Diwakar; Givens, Edwin N.; Schweighardt, Frank K.

    1984-01-01

    A process is disclosed for the solvent refining of non-anthracitic coal at elevated temperatures and pressure in a hydrogen atmosphere using a hydrocarbon solvent which before being recycled in the solvent refining process is subjected to chemical treatment to extract substantially all nitrogenous and phenolic constituents from the solvent so as to improve the conversion of coal and the production of oil in the solvent refining process. The solvent refining process can be either thermal or catalytic. The extraction of nitrogenous compounds can be performed by acid contact such as hydrogen chloride or fluoride treatment, while phenolic extraction can be performed by caustic contact or contact with a mixture of silica and alumina.

  8. Use of normal propyl bromide solvents for extraction and recovery of asphalt cements

    DOT National Transportation Integrated Search

    2000-11-01

    Four normal propyl bromide (nPB) solvents were evaluated for use as chlorinated solvent replacements in typical hot mix asphalt (HMA) extraction and recovery processes. The experimental design included one method of extraction (centrifuge), one metho...

  9. Semiautomated solid-phase extraction manifold with a solvent-level sensor.

    PubMed

    Orlando, R M; Rath, S; Rohwedder, J J R

    2013-11-15

    A semiautomated solid-phase extraction manifold for multiple extractions is presented. The manifold utilizes commercial solid-phase syringe cartridges and automatically introduces and elutes all the solvents during the extraction, reducing the typical workload and stress of the analyst. The manifold consists of a peristaltic pump with solenoid valves in a flow circuit that contains transmissive photomicrosensors. The photomicrosensors were used to control the solvent dispenser and the solvent level inside the cartridge. As solvent-level sensors, the photomicrosensors determined the exact time the solvent reached the top frit to avoid sorbent drying and accurately perform the solvent exchange. The repeatability of the manifold to introduce a particular volume of solvent into the cartridges was measured, and the precisions were between 0.05 and 2.89% (RSD). To evaluate the manifold, the amount of two fluoroquinolones in a fortified blank milk sample was determined. The results of the intra- and inter-day precision of multiple extractions from the fortified milk samples resulted in precisions better than 9.0% (RSD) and confirmed that the arrangement of the semiautomated manifold could adequately be used in solid-phase extraction with commercial cartridges. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Solvent Extraction of Chemical Attribution Signature Compounds from Painted Wall Board: Final Report

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Wahl, Jon H.; Colburn, Heather A.

    2009-10-29

    This report summarizes work that developed a robust solvent extraction procedure for recovery of chemical attribution signature (CAS) compound dimethyl methyl phosphonate (DMMP) (as well as diethyl methyl phosphonate (DEMP), diethyl methyl phosphonothioate (DEMPT), and diisopropyl methyl phosphonate (DIMP)) from painted wall board (PWB), which was selected previously as the exposed media by the chemical attribution scientific working group (CASWG). An accelerated solvent extraction approach was examined to determine the most effective method of extraction from PWB. Three different solvent systems were examined, which varied in solvent strength and polarity (i.e., 1:1 dichloromethane : acetone,100% methanol, and 1% isopropanol inmore » pentane) with a 1:1 methylene chloride : acetone mixture having the most robust and consistent extraction for four original target organophosphorus compounds. The optimum extraction solvent was determined based on the extraction efficiency of the target analytes from spiked painted wallboard as determined by gas chromatography x gas chromatography mass spectrometry (GCxGC-MS) analysis of the extract. An average extraction efficiency of approximately 60% was obtained for these four compounds. The extraction approach was further demonstrated by extracting and detecting the chemical impurities present in neat DMMP that was vapor-deposited onto painted wallboard tickets.« less

  11. Effect of solvent polarity on the extraction of components of pharmaceutical plastic containers.

    PubMed

    Ahmad, Iqbal; Sabah, Arif; Anwar, Zubair; Arif, Aysha; Arsalan, Adeel; Qadeer, Kiran

    2017-01-01

    A study of the extraction of polymeric material and dyes from the pharmaceutical plastic containers using various organic solvents was conducted to evaluate the effect of polarity on the extraction process. The plastic containers used included semi-opaque, opaque, transparent and amber colored and the solvent used were acetonitrile, methanol, ethanol, acetone, dichloroethane, chloroform and water. The determination of extractable material was carried out by gravimetric and spectrometric methods. The yield of extractable materials from containers in 60 h was 0.10-1.29% (w/w) and the first-order rate constant (kobs) for the extraction of polymeric material ranged from 0.52-1.50 × 10-3 min -1 and for the dyes 6.43- 6.74 x10-3min-1. The values of (k obs ) were found to be an inverse function of solvent dielectric constant and decreased linearly with the solvent acceptor number. The extractable polymeric materials exhibited absorption in the 200-400 nm region and the dyes in the 300-500nm region. The rates of extraction of polymeric material and dyes from plastic containers were dependent on the solvent dielectric constant. The solvents of low polarity were more effective in the extraction of material indicating that the extracted material were of low polarity or have non-polar character. The dyes were soluble in acetone and chloroform. No plastic material was found to be extracted from the containers in aqueous solution.

  12. Focused microwave-assisted solvent extraction and HPLC determination of effective constituents in Eucommia ulmodies Oliv. (E. ulmodies).

    PubMed

    Li, Hui; Chen, Bo; Zhang, Zhaohui; Yao, Shouzhuo

    2004-06-17

    A new focused microwave-assisted solvent extraction method using water as solvent has been developed for leaching geniposidic and chlorogenic acids from Eucommia ulmodies Oliv. The extraction procedures were optimized using a two indexes orthogonal experimental design and graphical analysis, by varying irradiation time, solvent volume, solvent composition and microwave power. The optimum extraction conditions were obtained: for geniposidic acid, 50% micorwave power, 40s irradiation, and 80% (v/v) aqueous methanol as extraction solvent (20mlg(-1) sample); and for chlorogenic acid, 50% micorwave power, 30s irradiation, and 20% aqueous methanol (20mlg(-1) sample). The composition of the extraction solvent was optimized and can be directly used as the mobile phase in the HPLC separation. Quantification of organic acids was done by HPLC at room temperature using Spherigel C(18) chromatographic column (250 mm x4.6 mm , i.d. 5mum), the methanol:water:acetic acid (20:80:1.0, v/v) mobile phase and UV detection at 240nm. The R.S.D. of the extraction process for geniposidic and chlorogenic acid were 3.8 and 4.1%, respectively.

  13. Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

    PubMed Central

    Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

    2017-01-01

    The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85%) and oleic acid (1.64%–18.97%). Thymoquinone (0.72%–21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. PMID:28814830

  14. Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

    PubMed

    Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

    2017-01-01

    The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P <0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

  15. Miscibility Evaluation Of The Next Generation Solvent With Polymers Currently Used At DWPF, MCU, And Saltstone

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F. F.

    The Office of Waste Processing, within the Office of Technology Innovation and Development, funded the development of an enhanced Caustic-Side Solvent Extraction (CSSX) solvent for deployment at the Savannah River Site for removal of cesium from High Level Waste. This effort lead to the development of the Next Generation Solvent (NGS) with Tris (3,7-dimethyl octyl) guanidine (TiDG). The first deployment target for the NGS solvent is within the Modular CSSX Unit (MCU). Deployment of a new chemical within an existing facility requires verification that the new chemical components are compatible with the installed equipment. In the instance of a newmore » organic solvent, the primary focus is on compatibility of the solvent with organic polymers used in the affected facility. This report provides the calculated data from exposing these polymers to the Next Generation Solvent. An assessment of the dimensional stability of polymers known to be used or present in the MCU, Defense Waste Processing Facility (DWPF), and Saltstone facilities that will be exposed to the NGS showed that TiDG could selectively affect the elastomers and some thermoplastics to varying extents, but the typical use of these polymers in a confined geometry will likely prevent the NGS from impacting component performance. The polymers identified as of primary concern include Grafoil® (flexible graphite), Tefzel®, Isolast®, ethylene-propylene-diene monomer (EPDM) rubber, nitrile-butadiene rubber (NBR), styrene-butadiene rubber (SBR), ultra high molecular weight polyethylene (UHMWPE), and fluorocarbon rubber (FKM). Certain polymers like NBR and EPDM were found to interact mildly with NGS but their calculated swelling and the confined geometry will impede interaction with NGS. In addition, it was found that Vellumoid (cellulose fibers-reinforced glycerin and protein) may leach protein and Polyvinyl Chloride (PVC) may leach plasticizer (such as Bis-Ethylhexyl-Phthalates) into the NGS solvent. Either case will not impact decontamination or immobilization operations at Savannah River Site (SRS). Some applications have zero tolerance for dimensional changes such as the operation of valves while other applications a finite dimensional change improves the function of the application such as seals and gaskets. Additional considerations are required before using the conclusions from this work to judge outcomes in field applications. Decane, a component of Isopar L that is most likely to interact with the polymers, mildly interacted with the elastomers and the propylene based polymers but their degree of swelling is at most 10% and the confined geometry that they are typically placed in indicate this is not significant. In addition, it was found that Vellumoid may leach protein into the NGS solvent. Since Vellumoid is used at the mixer in Saltstone where it sees minimum quantities of solvent, this leaching has no effect on the extraction process at MCU or the immobilization process at saltstone. No significant interaction is expected between MaxCalix and the polymers and elastomers used at MCU, DWPF, and Saltstone. Overall, minimal and insignificant interactions are expected on extraction and immobilization operations when MCU switches from CSSX to NGS solvent. It is expected that contacting NGS will not accelerate the aging rate of polymers and elastomers under radiation and heat. This is due to the minimal interaction between NGS and the polymers and the confined geometries for these polymers. SRNL recommends the use of the HSP method (for screening) and some testing to evaluate the impact of other organic such as alcohols, glycolate, and their byproducts on the polymers used throughout the site.« less

  16. Separation of nitrogen heterocyclic compounds from model coal tar fraction by solvent extraction

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kim, S.J.; Chun, Y.J.

    2005-07-01

    The separation of four kinds of nitrogen heterocyclic compounds (NHCs) from a model mixture comprising NHCs (indole (In), quinoline (Q), iso-quinoline (iQ), quinaldine (Qu)), three kinds of bicyclic aromatic compounds (BACs; 1-methyl-naphthalene (IMN), 2-methyl naphthalene (2MN), dimethylnaphthalene (DMN)), biphenyl (Bp) and phenyl ether (Pe) was examined by a solvent extraction. The model mixture used as a raw material of this work was prepared according to the components and compositions contained in coal tar fraction (the temperature ranges of fraction: 240-265{sup o}C). An aqueous solution of methanol, ethanol, iso-propyl alcohol, N,N-dimethyl acetamide, DMF, formamide, N-methylformamide/methanol, and formamide/methanol were used as solvents.more » An aqueous solution of formamide was found suitable for separating NHCs contained in coal tar fraction based on distribution coefficient and selectivity. The effect of operation factors on separating NHCs was investigated by the distribution equilibrium using an aqueous solution of formamide. Increasing the operation temperature and the volume ratio of solvent to feed at initial (S/F)(o) resulted in improving the distribution coefficients of each NHC, but increasing the volume fraction of water in the solvent at initial (y(w,O)) resulted in deteriorating the distribution coefficients of each NHC. With increasing y(w,O) and (S/F)(o), the selectivities of each NHC in reference to DMN increased. Increase in operation temperature resulted in decrease in selectivities of each NHC in reference to DMN. At an experimental condition fixed, the sequence of the distribution coefficient and selectivity in reference to DMN for each NHC was In {gt} iQ {gt} Q {gt} Qu, and also the sequence of the distribution coefficient for each BAC was IMN {gt} 2MN {gt} DMN. The sequence of the distribution coefficient for entire compounds analyzed by this work was In {gt} iQ {gt} Q {gt} Qu {gt} BP {gt} 1MN {gt} 2MN {gt} Pe {gt} DMN.« less

  17. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Moyer, Bruce A.

    The North American industry has employed major solvent-extraction processes to support a wide range of separations including but not limited to chemical, metallurgical, nuclear, biochemical, pharmaceutical, and petroleum applications. The knowledge enabling these separations has been obtained through fundamental studies in academe, government and industry. The International Solvent Extraction Conferences have been and continue to be a major gathering of scientists, engineers, operators, and vendors from around the world, who present new findings since the last meeting, exchange ideas, make business contacts, and conduct collegial discussions. The ISEC 2008 program emphasizes fundamentals to industrial applications of solvent extraction, particularly howmore » this broad spectrum of activities is interconnected and has led to the implementation of novel processes. The oral and poster sessions have been organized into seven topics: Fundamentals; Novel Reagents, Materials and Techniques; Nuclear Fuel Reprocessing; Hydrometallurgy and Metals Extraction; Analytical and Preparative Applications; Biotechnology, Pharmaceuticals, Life-Science Products, and Organic Products; and Process Chemistry and Engineering. Over 350 abstracts were received, resulting in more than 260 manuscripts published in these proceedings. Five outstanding plenary presentations have been identified, with five parallel sessions for oral presentations and posters. In recognition of the major role solvent extraction (SX) plays in the hydrometallurgical and nuclear industries, these proceedings begin with sections focusing on hydrometallurgy, process chemistry, and engineering. More fundamental topics follow, including sections on novel reagents, materials, and techniques, featuring novel applications in analytical and biotechnology areas. Despite the diversity of topics and ideas represented, however, the primary focus of the ISEC community continues to be metals extraction. Four papers from these proceedings have been entered already in INIS in the form of individual reports. Among the remaining papers, 60 have been selected from the following sessions: Plenary Lectures, Hydrometallurgy and Metals Extraction, Nuclear Fuel Reprocessing, Analytical and Preparative Applications, Fundamentals, and Novel Reagents, Materials, and Techniques.« less

  18. SOLVENT EXTRACTION OF URANIUM VALUES

    DOEpatents

    Feder, H.M.; Ader, M.; Ross, L.E.

    1959-02-01

    A process is presented for extracting uranium salt from aqueous acidic solutions by organic solvent extraction. It consists in contacting the uranium bearing solution with a water immiscible dialkylacetamide having at least 8 carbon atoms in the molecule. Mentioned as a preferred extractant is dibutylacetamide. The organic solvent is usually used with a diluent such as kerosene or CCl/sub 4/.

  19. Solidification of floating organic droplet in dispersive liquid-liquid microextraction as a green analytical tool.

    PubMed

    Mansour, Fotouh R; Danielson, Neil D

    2017-08-01

    Dispersive liquid-liquid microextraction (DLLME) is a special type of microextraction in which a mixture of two solvents (an extracting solvent and a disperser) is injected into the sample. The extraction solvent is then dispersed as fine droplets in the cloudy sample through manual or mechanical agitation. Hence, the sample is centrifuged to break the formed emulsion and the extracting solvent is manually separated. The organic solvents commonly used in DLLME are halogenated hydrocarbons that are highly toxic. These solvents are heavier than water, so they sink to the bottom of the centrifugation tube which makes the separation step difficult. By using solvents of low density, the organic extractant floats on the sample surface. If the selected solvent such as undecanol has a freezing point in the range 10-25°C, the floating droplet can be solidified using a simple ice-bath, and then transferred out of the sample matrix; this step is known as solidification of floating organic droplet (SFOD). Coupling DLLME to SFOD combines the advantages of both approaches together. The DLLME-SFOD process is controlled by the same variables of conventional liquid-liquid extraction. The organic solvents used as extractants in DLLME-SFOD must be immiscible with water, of lower density, low volatility, high partition coefficient and low melting and freezing points. The extraction efficiency of DLLME-SFOD is affected by types and volumes of organic extractant and disperser, salt addition, pH, temperature, stirring rate and extraction time. This review discusses the principle, optimization variables, advantages and disadvantages and some selected applications of DLLME-SFOD in water, food and biomedical analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Supercritical Fluid Extraction of Eucalyptus globulus Bark—A Promising Approach for Triterpenoid Production

    PubMed Central

    Domingues, Rui M. A.; Oliveira, Eduardo L. G.; Freire, Carmen S. R.; Couto, Ricardo M.; Simões, Pedro C.; Neto, Carlos P.; Silvestre, Armando J. D.; Silva, Carlos M.

    2012-01-01

    Eucalyptus bark contains significant amounts of triterpenoids with demonstrated bioactivity, namely triterpenic acids and their acetyl derivatives (ursolic, betulinic, oleanolic, betulonic, 3-acetylursolic, and 3-acetyloleanolic acids). In this work, the supercritical fluid extraction (SFE) of Eucalyptus globulus deciduous bark was carried out with pure and modified carbon dioxide to recover this fraction, and the results were compared with those obtained by Soxhlet extraction with dichloromethane. The effects of pressure (100–200 bar), co-solvent (ethanol) content (0, 5 and 8% wt), and multistep operation were studied in order to evaluate the applicability of SFE for their selective and efficient production. The individual extraction curves of the main families of compounds were measured, and the extracts analyzed by GC-MS. Results pointed out the influence of pressure and the important role played by the co-solvent. Ethanol can be used with advantage, since its effect is more important than increasing pressure by several tens of bar. At 160 bar and 40 °C, the introduction of 8% (wt) of ethanol greatly improves the yield of triterpenoids more than threefold. PMID:22837719

  1. Extraction of vitexin from binahong (Anredera cordifolia (Ten.) Steenis) leaves using betaine - 1,4 butanediol natural deep eutectic solvent (NADES)

    NASA Astrophysics Data System (ADS)

    Mulia, Kamarza; Muhammad, Fajri; Krisanti, Elsa

    2017-03-01

    The leaves of binahong (Anredera cordifolia (Ten) Steenis) contain flavonoids as bioactive substances that have efficacy to treat wounds and diseases caused by bacteria. One of the flavonoids contained in the leaves is 8-glucopyranosyl-4'5'7-trihydroxyflavone or vitexin. Conventional extraction of flavonoids from leaves of binahong has been developed and usually using non-friendly organic solvent. To overcome these problems, a Natural Deep Eutectic Solvent (NADES) is used to replace the conventional organic solvents, as it is an environmentally friendly, non-toxic and high boiling point solvent. In this study, a betaine-based NADES combined with 1,4-butanediol in 1:3 mole ratio was used as the extraction solvent. Vitexin in the extract was analyzed qualitatively and quantitatively using an HPLC. The extraction of vitexin from binahong leaves at room temperature (27 °C) for four hours give yield of 46 ppm, much lower than 200 ppm yield obtained after extraction at 55 °C for 90 minutes. This results showed that (a) NADES consisting of betaine and 1,4 butanediol is a promising green solvent for extraction of vitexin from binahong leaves, and, (b) the extraction can be performed above ambient temperature, as long as it does not exceed the degradation temperature of the bioactive compound extracted.

  2. PROCESS OF SEPARATING URANIUM FROM AQUEOUS SOLUTION BY SOLVENT EXTRACTION

    DOEpatents

    Warf, J.C.

    1958-08-19

    A process is described for separating uranium values from aqueous uranyl nitrate solutions. The process consists in contacting the uramium bearing solution with an organic solvent, tributyl phosphate, preferably diluted with a less viscous organic liquida whereby the uranyl nitrate is extracted into the organic solvent phase. The uranvl nitrate may be recovered from the solvent phase bv back extracting with an aqueous mediuin.

  3. Enzyme assisted extraction of biomolecules as an approach to novel extraction technology: A review.

    PubMed

    Nadar, Shamraja S; Rao, Priyanka; Rathod, Virendra K

    2018-06-01

    An interest in the development of extraction techniques of biomolecules from various natural sources has increased in recent years due to their potential applications particularly for food and nutraceutical purposes. The presence of polysaccharides such as hemicelluloses, starch, pectin inside the cell wall, reduces the extraction efficiency of conventional extraction techniques. Conventional techniques also suffer from low extraction yields, time inefficiency and inferior extract quality due to traces of organic solvents present in them. Hence, there is a need of the green and novel extraction methods to recover biomolecules. The present review provides a holistic insight to various aspects related to enzyme aided extraction. Applications of enzymes in the recovery of various biomolecules such as polyphenols, oils, polysaccharides, flavours and colorants have been highlighted. Additionally, the employment of hyphenated extraction technologies can overcome some of the major drawbacks of enzyme based extraction such as longer extraction time and immoderate use of solvents. This review also includes hyphenated intensification techniques by coupling conventional methods with ultrasound, microwave, high pressure and supercritical carbon dioxide. The last section gives an insight on application of enzyme immobilization as a strategy for large scale extraction. Immobilization of enzymes on magnetic nanoparticles can be employed to enhance the operational performance of the system by multiple use of expensive enzymes making them industrially and economically feasible. Copyright © 2018 Elsevier Ltd. All rights reserved.

  4. PREPARATION OF ALKYL PYROPHOSPHATE EXTRACTANTS

    DOEpatents

    Levine, C.A.; Skiens, W.E.; Moore, G.R.

    1960-08-01

    A process for providing superior solvent extractants for metal recovery processes is given wherein the extractant comprises an alkyl pyrophosphoric acid ester dissolved in an organic solvent diluent. Finely divided solid P/sub 2/O/ sub 5/ is slurried in an organic solvent-diluent selected from organic solvents such as kerosene, benzene, chlorobenzene, toluene, etc. An alcohol selected from the higher alcohols having 4 to 17 carbon atoms. e.g.. hexanol-1. heptanol-3, octanol-1. 2.6-dimethyl-heptanol-4, and decanol-1, is rapidly added to the P/sub 2/O/sub 5/ slurry in the amount of about 2 moles of alcohol to 1 mole of P/sub 2/ O/sub 5/. The temperature is maintained below about 110 deg C during the course of the P/sub 2/O/sub 5/-alcohol reaction. An alkyl pyrophosphate extractant compound is formed as a consequence of the reaction process. The alkyl pyrophosphate solvent-diluent extractant phase is useful in solvent extraction metal recovery processes.

  5. Process for the removal of impurities from combustion fullerenes

    DOEpatents

    Alford, J. Michael; Bolskar, Robert

    2005-08-02

    The invention generally relates to purification of carbon nanomaterials, particularly fullerenes, by removal of PAHs and other hydrocarbon impurities. The inventive process involves extracting a sample containing carbon nanomaterials with a solvent in which the PAHs are substantially soluble but in which the carbon nanomaterials are not substantially soluble. The sample can be repeatedly or continuously extracted with one or more solvents to remove a greater amount of impurities. Preferred solvents include ethanol, diethyl ether, and acetone. The invention also provides a process for efficiently separating solvent extractable fullerenes from samples containing fullerenes and PAHs wherein the sample is extracted with a solvent in which both fullerenes and PAHs are substantially soluble and the sample extract then undergoes selective extraction to remove PAHs. Suitable solvents in which both fullerenes and PAHs are soluble include o-xylene, toluene, and o-dichlorobenzene. The purification process is capable of treating quantities of combustion soot in excess of one kilogram and can produce fullerenes or fullerenic soot of suitable purity for many applications.

  6. Extraction of Illegal Dyes from Red Chili Peppers with Cholinium-Based Deep Eutectic Solvents

    PubMed Central

    Zhu, Shuqiang; Zhu, Xinyue; Su, Along

    2017-01-01

    Deep eutectic solvents (DESs) as a new kind of green solvents have been used to extract bioactive compounds but there are few applications in extracting chrysoidine dyes. In this study, we developed an ultrasonic-assisted extraction method with choline chloride/hydrogen bond donor (ChCl/HBD) DES for the extraction of chrysoidine G (COG), astrazon orange G (AOG), and astrazon orange R (AOR) in food samples. Some experimental parameters, such as extraction time, raw material/solvent ratio, and temperature, were evaluated and optimized as follows: the ratio of ChCl/HBD, 1 : 2 (v/v); the ratio of sample/DES, 1 : 10 (g/mL); extraction time, 20 min; extraction temperature, 50°C. Under the optimized conditions, the limits of detection (μg/mL) were 0.10 for COG and 0.06 for AOG and AOR. The relative standard deviations were in the range of 1.2–2.1%. The recoveries of the three dyes were in the range of 80.2–105.0%. By comparing with other commonly used solvents for extracting chrysoidine dyes, the advantages of DESs proved them to be potential extraction solvents for chrysoidine G, astrazon orange G, and astrazon orange R in foods. PMID:28831327

  7. Study to find the best extraction solvent for use with guava leaves (Psidium guajava L.) for high antioxidant efficacy.

    PubMed

    Seo, Jongkwon; Lee, Soojung; Elam, Marcus L; Johnson, Sarah A; Kang, Jonghoon; Arjmandi, Bahram H

    2014-03-01

    The effects of guava leaves extracted using solvents of water, ethanol, methanol, and different concentrations of hydroethanolic solvents on phenolic compounds and flavonoids, and antioxidant properties have been investigated. The antioxidant capability was assessed based on 2,2-diphenyl-1-picrylhydrazyl radical and 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) radical-scavenging abilities, reducing power, and nitric oxide-and nitrate-scavenging activities. The results demonstrated that the antioxidant ability of guava leaf extracts has a strong relationship with phenolic compound content rather than flavonoid content. Phenolic compound content of water extracted guava leaves was higher compared to pure ethanol and methanol extracts. However, phenolic compound content extracted using hydroethanolic solvent was higher than water, whereas 50% hydroethanolic was observed to be the most effective solvent showing high antioxidant ability.

  8. Deep eutectic solvents as efficient solvent system for the extraction of κ-carrageenan from Kappaphycus alvarezii.

    PubMed

    Das, Arun Kumar; Sharma, Mukesh; Mondal, Dibyendu; Prasad, Kamalesh

    2016-01-20

    Three different deep eutectic solvents (DESs) prepared by the complexation of choline chloride with urea, ethylene glycol and glycerol along with their hydrated counterparts were used for the selective extraction of κ-carrageenan from Kappaphycus alvarezii. Upon comparison of the quality of the polysaccharide with the one obtained using water as extraction media as well as the one extracted using widely practiced conventional method, it was found that, the physicochemical as well as rheological properties of κ-carrageenan obtained using DESs as solvents was at par to the one obtained using conventional method and was superior in quality when compared to κ-carrageenan obtained using water as solvent. Considering the tedious nature of the extraction method employed in conventional extraction process, the DESs can be considered as suitable alternative solvents for the facile extraction of the polysaccharide directly from the seaweed. However, among the hydrated and non-hydrated DESs, the hydrated ones were found to be more effective in comparison to their non-hydrated counterparts. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Development status of the life marker chip instrument for ExoMars

    NASA Astrophysics Data System (ADS)

    Sims, Mark R.; Cullen, David C.; Rix, Catherine S.; Buckley, Alan; Derveni, Mariliza; Evans, Daniel; Miguel García-Con, Luis; Rhodes, Andrew; Rato, Carla C.; Stefinovic, Marijan; Sephton, Mark A.; Court, Richard W.; Bulloch, Christopher; Kitchingman, Ian; Ali, Zeshan; Pullan, Derek; Holt, John; Blake, Oliver; Sykes, Jonathan; Samara-Ratna, Piyal; Canali, Massimiliano; Borst, Guus; Leeuwis, Henk; Prak, Albert; Norfini, Aleandro; Geraci, Ennio; Tavanti, Marco; Brucato, John; Holm, Nils

    2012-11-01

    The Life Marker Chip (LMC) is one of the instruments being developed for possible flight on the 2018 ExoMars mission. The instrument uses solvents to extract organic compounds from samples of martian regolith and to transfer the extracts to dedicated detectors based around the use of antibodies. The scientific aims of the instrument are to detect organics in the form of biomarkers that might be associated with extinct life, extant life or abiotic sources of organics. The instrument relies on a novel surfactant-based solvent system and bespoke, commercial and research-developed antibodies against a number of distinct biomarkers or molecular types. The LMC comprises of a number of subsystems designed to accept up to four discrete samples of martian regolith or crushed rock, implement the solvent extraction, perform microfluidic-based multiplexed antibody-assays for biomarkers and other targets, optically detect the fluorescent output of the assays, control the internal instrument pressure and temperature, in addition to the associated instrument control electronics and software. The principle of operation, the design and the instrument development status as of December 2011 are reported here. The instrument principle can be extended to other configurations and missions as needed.

  10. Solvent extraction of gold using ionic liquid based process

    NASA Astrophysics Data System (ADS)

    Makertihartha, I. G. B. N.; Zunita, Megawati; Rizki, Z.; Dharmawijaya, P. T.

    2017-01-01

    In decades, many research and mineral processing industries are using solvent extraction technology for metal ions separation. Solvent extraction technique has been used for the purification of precious metals such as Au and Pd, and base metals such as Cu, Zn and Cd. This process uses organic compounds as solvent. Organic solvents have some undesired properties i.e. toxic, volatile, excessive used, flammable, difficult to recycle, low reusability, low Au recovery, together with the problems related to the disposal of spent extractants and diluents, even the costs associated with these processes are relatively expensive. Therefore, a lot of research have boosted into the development of safe and environmentally friendly process for Au separation. Ionic liquids (ILs) are the potential alternative for gold extraction because they possess several desirable properties, such as a the ability to expanse temperature process up to 300°C, good solvent properties for a wide range of metal ions, high selectivity, low vapor pressures, stability up to 200°C, easy preparation, environmentally friendly (commonly called as "green solvent"), and relatively low cost. This review paper is focused in investigate of some ILs that have the potentials as solvent in extraction of Au from mineral/metal alloy at various conditions (pH, temperature, and pressure). Performances of ILs extraction of Au are studied in depth, i.e. structural relationship of ILs with capability to separate Au from metal ions aggregate. Optimal extraction conditon in order to gain high percent of Au in mineral processing is also investigated.

  11. Characteristics and antioxidant of Ulva intestinalis sulphated polysaccharides extracted with different solvents.

    PubMed

    Peasura, Napassorn; Laohakunjit, Natta; Kerdchoechuen, Orapin; Wanlapa, Sorada

    2015-11-01

    Ulva intestinalis, a tubular green seaweed, is a rich source of nutrient, especially sulphated polysaccharides. Sulphated polysaccharides from U. intestinalis were extracted with distilled water, 0.1N HCl, and 0.1N NaOH at 80°C for 1, 3, 6, 12, and 24h to study the effect of the extraction solvent and time on their chemical composition and antioxidant activity. Different types of solvents and extraction time had a significant influence on the chemical characteristics and antioxidant activity (p<0.05). Monosaccharide composition and FT-IR spectra analyses revealed that sulphated polysaccharides from all solvent extractions have a typical sugar backbone (glucose, rhamnose, and sulphate attached at C-2 or C-3 of rhamnose). Sulphated polysaccharides extracted with acid exhibited greater antioxidant activity than did those extracted with distilled water and alkali. The results indicated that solvent extraction could be an efficacious method for enhancing antioxidant activity by distinct molecular weight and chemical characteristic of sulphated polysaccharides. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. SOLVENT EXTRACTION PROCESS FOR THE SEPARATION OF URANIUM AND THORIUM FROM PROTACTINIUM AND FISSION PRODUCTS

    DOEpatents

    Rainey, R.H.; Moore, J.G.

    1962-08-14

    A liquid-liquid extraction process was developed for recovering thorium and uranium values from a neutron irradiated thorium composition. They are separated from a solvent extraction system comprising a first end extraction stage for introducing an aqueous feed containing thorium and uranium into the system consisting of a plurality of intermediate extractiorr stages and a second end extractron stage for introducing an aqueous immiscible selective organic solvent for thorium and uranium in countercurrent contact therein with the aqueous feed. A nitrate iondeficient aqueous feed solution containing thorium and uranium was introduced into the first end extraction stage in countercurrent contact with the organic solvent entering the system from the second end extraction stage while intro ducing an aqueous solution of salting nitric acid into any one of the intermediate extraction stages of the system. The resultant thorium and uranium-laden organic solvent was removed at a point preceding the first end extraction stage of the system. (AEC)

  13. Reductive stripping process for uranium recovery from organic extracts

    DOEpatents

    Hurst, F.J. Jr.

    1983-06-16

    In the reductive stripping of uranium from an organic extractant in a uranium recovery process, the use of phosphoric acid having a molarity in the range of 8 to 10 increases the efficiency of the reductive stripping and allows the strip step to operate with lower aqueous to organic recycle ratios and shorter retention time in the mixer stages. Under these operating conditions, less solvent is required in the process, and smaller, less expensive process equipment can be utilized. The high strength H/sub 3/PO/sub 4/ is available from the evaporator stage of the process.

  14. Reductive stripping process for uranium recovery from organic extracts

    DOEpatents

    Hurst, Jr., Fred J.

    1985-01-01

    In the reductive stripping of uranium from an organic extractant in a uranium recovery process, the use of phosphoric acid having a molarity in the range of 8 to 10 increases the efficiency of the reductive stripping and allows the strip step to operate with lower aqueous to organic recycle ratios and shorter retention time in the mixer stages. Under these operating conditions, less solvent is required in the process, and smaller, less expensive process equipment can be utilized. The high strength H.sub.3 PO.sub.4 is available from the evaporator stage of the process.

  15. REMEDIATING PESTICIDE CONTAMINATED SOILS USING SOLVENT EXTRACTION

    EPA Science Inventory

    Bench-scale solvent extraction studies were performed on soil samples obtained from a Superfund site contaminated with high levels of p,p'-DDT, p,p'-DDD,, p,p'-DDE and toxaphene. The effectiveness of the solvent extraction process was assessed using methanol and 2-propanol as sol...

  16. Solvent Extraction of Furfural From Biomass

    NASA Technical Reports Server (NTRS)

    Humphrey, M. F.

    1984-01-01

    Solvent-extraction method reduces energy required to remove furfural produced during acid hydrolysis of biomass. Acid hydrolysis performed in vessel containing both solvents and reacting ingredients. With intimate contact between solvents and aqueous hydrolyis liqour, furfural removed form liquor almost as fast as it forms.

  17. Extraction Techniques for Polycyclic Aromatic Hydrocarbons in Soils

    PubMed Central

    Lau, E. V.; Gan, S.; Ng, H. K.

    2010-01-01

    This paper aims to provide a review of the analytical extraction techniques for polycyclic aromatic hydrocarbons (PAHs) in soils. The extraction technologies described here include Soxhlet extraction, ultrasonic and mechanical agitation, accelerated solvent extraction, supercritical and subcritical fluid extraction, microwave-assisted extraction, solid phase extraction and microextraction, thermal desorption and flash pyrolysis, as well as fluidised-bed extraction. The influencing factors in the extraction of PAHs from soil such as temperature, type of solvent, soil moisture, and other soil characteristics are also discussed. The paper concludes with a review of the models used to describe the kinetics of PAH desorption from soils during solvent extraction. PMID:20396670

  18. Comparison of solvent extraction and solid-phase extraction for the determination of polychlorinated biphenyls in transformer oil.

    PubMed

    Mahindrakar, A N; Chandra, S; Shinde, L P

    2014-01-01

    Solid-phase extraction (SPE) of nine polychlorinated biphenyls (PCBs) from transformer oil samples was evaluated using octadecyl (CI8)-bonded porous silica. The efficiency of SPE of these PCBs was compared with those obtained by solvent extraction with DMSO and hexane. Average recoveries exceeding 95% for these PCBs were obtained via the SPE method using small cartridges containing 100mg of 40 pm CI8-bonded porous silica. The average recovery by solvent extraction with DMSO and hexane exceeded 83%. It was concluded that the recoveries and precision for the solvent extraction of PCBs were poorer than those for the SPE. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. Ionic liquid solutions as extractive solvents for value-added compounds from biomass

    PubMed Central

    Passos, Helena; Freire, Mara G.; Coutinho, João A. P.

    2014-01-01

    In the past few years, the number of studies regarding the application of ionic liquids (ILs) as alternative solvents to extract value-added compounds from biomass has been growing. Based on an extended compilation and analysis of the data hitherto reported, the main objective of this review is to provide an overview on the use of ILs and their mixtures with molecular solvents for the extraction of value-added compounds present in natural sources. The ILs (or IL solutions) investigated as solvents for the extraction of natural compounds, such as alkaloids, flavonoids, terpenoids, lipids, among others, are outlined. The extraction techniques employed, namely solid–liquid extraction, and microwave-assisted and ultrasound-assisted extractions, are emphasized and discussed in terms of extraction yields and purification factors. Furthermore, the evaluation of the IL chemical structure and the optimization of the process conditions (IL concentration, temperature, biomass–solvent ratio, etc.) are critically addressed. Major conclusions on the role of the ILs towards the extraction mechanisms and improved extraction yields are additionally provided. The isolation and recovery procedures of the value-added compounds are ascertained as well as some scattered strategies already reported for the IL solvent recovery and reusability. Finally, a critical analysis on the economic impact versus the extraction performance of IL-based methodologies was also carried out and is here presented and discussed. PMID:25516718

  20. Ionic liquid solutions as extractive solvents for value-added compounds from biomass.

    PubMed

    Passos, Helena; Freire, Mara G; Coutinho, João A P

    2014-12-01

    In the past few years, the number of studies regarding the application of ionic liquids (ILs) as alternative solvents to extract value-added compounds from biomass has been growing. Based on an extended compilation and analysis of the data hitherto reported, the main objective of this review is to provide an overview on the use of ILs and their mixtures with molecular solvents for the extraction of value-added compounds present in natural sources. The ILs (or IL solutions) investigated as solvents for the extraction of natural compounds, such as alkaloids, flavonoids, terpenoids, lipids, among others, are outlined. The extraction techniques employed, namely solid-liquid extraction, and microwave-assisted and ultrasound-assisted extractions, are emphasized and discussed in terms of extraction yields and purification factors. Furthermore, the evaluation of the IL chemical structure and the optimization of the process conditions (IL concentration, temperature, biomass-solvent ratio, etc.) are critically addressed. Major conclusions on the role of the ILs towards the extraction mechanisms and improved extraction yields are additionally provided. The isolation and recovery procedures of the value-added compounds are ascertained as well as some scattered strategies already reported for the IL solvent recovery and reusability. Finally, a critical analysis on the economic impact versus the extraction performance of IL-based methodologies was also carried out and is here presented and discussed.

  1. 40 CFR 63.2855 - How do I determine the quantity of oilseed processed?

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR SOURCE CATEGORIES (CONTINUED) National Emission Standards for Hazardous Air Pollutants: Solvent Extraction for... following an operating month, you must determine the tons as received of each listed oilseed processed for...

  2. 40 CFR 63.2855 - How do I determine the quantity of oilseed processed?

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR SOURCE CATEGORIES (CONTINUED) National Emission Standards for Hazardous Air Pollutants: Solvent Extraction for... following an operating month, you must determine the tons as received of each listed oilseed processed for...

  3. 40 CFR 63.2855 - How do I determine the quantity of oilseed processed?

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR SOURCE CATEGORIES (CONTINUED) National Emission Standards for Hazardous Air Pollutants: Solvent Extraction for... following an operating month, you must determine the tons as received of each listed oilseed processed for...

  4. 76 FR 37349 - Agency Information Collection Activities; Submission to OMB for Review and Approval; Comment...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-06-27

    ... Vegetable Oil Production (Renewal) AGENCY: Environmental Protection Agency (EPA). ACTION: Notice. SUMMARY... for Solvent Extraction for Vegetable Oil Production (Renewal). ICR Numbers: EPA ICR Number 1947.05... disclose the information. Respondents/Affected Entities: Owners or operators of vegetable oil production...

  5. Separation of heavy metals: Removal from industrial wastewaters and contaminated soil

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, R.W.; Shem, L.

    1993-01-01

    This paper reviews the applicable separation technologies relating to removal of heavy metals from solution and from soils in order to present the state-of-the-art in the field. Each technology is briefly described and typical operating conditions and technology performance are presented. Technologies described include chemical precipitation (including hydroxide, carbonate, or sulfide reagents), coagulation/flocculation, ion exchange, solvent extraction, extraction with chelating agents, complexation, electrochemical operation, cementation, membrane operations, evaporation, adsorption, solidification/stabilization, and vitrification. Several case histories are described, with a focus on waste reduction techniques and remediation of lead-contaminated soils. The paper concludes with a short discussion of important research needsmore » in the field.« less

  6. Separation of heavy metals: Removal from industrial wastewaters and contaminated soil

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, R.W.; Shem, L.

    1993-03-01

    This paper reviews the applicable separation technologies relating to removal of heavy metals from solution and from soils in order to present the state-of-the-art in the field. Each technology is briefly described and typical operating conditions and technology performance are presented. Technologies described include chemical precipitation (including hydroxide, carbonate, or sulfide reagents), coagulation/flocculation, ion exchange, solvent extraction, extraction with chelating agents, complexation, electrochemical operation, cementation, membrane operations, evaporation, adsorption, solidification/stabilization, and vitrification. Several case histories are described, with a focus on waste reduction techniques and remediation of lead-contaminated soils. The paper concludes with a short discussion of important research needsmore » in the field.« less

  7. Continuous extraction of organic materials from water

    USGS Publications Warehouse

    Goldberg, M.C.; DeLong, L.; Kahn, L.

    1971-01-01

    A continuous liquid solvent extractor, designed to utilize organic solvents that are heavier than water, is described. The extractor is capable of handling input rates up to 2 liters per hour and has a 500-ml. extractant capacity. Extraction efficiency is dependent upon the p-value, the two solvent ratios, rate of flow of the aqueous phase, and rate of reflux of the organic phase. Extractors can be serially coupled to increase extraction efficiency and, when coupled with a lighter-than-water extractor, the system will allow the use of any immiscible solvent.

  8. Process for producing fuel grade ethanol by continuous fermentation, solvent extraction and alcohol separation

    DOEpatents

    Tedder, Daniel W.

    1985-05-14

    Alcohol substantially free of water is prepared by continuously fermenting a fermentable biomass feedstock in a fermentation unit, thereby forming an aqueous fermentation liquor containing alcohol and microorganisms. Continuously extracting a portion of alcohol from said fermentation liquor with an organic solvent system containing an extractant for said alcohol, thereby forming an alcohol-organic solvent extract phase and an aqueous raffinate. Said alcohol is separated from said alcohol-organic solvent phase. A raffinate comprising microorganisms and unextracted alcohol is returned to the fermentation unit.

  9. Microwave-assisted extraction (MAE) of bioactive saponin from mahogany seed (Swietenia mahogany Jacq)

    NASA Astrophysics Data System (ADS)

    Waziiroh, E.; Harijono; Kamilia, K.

    2018-03-01

    Mahogany is frequently used for medicines for cancer, tumor, and diabetes, as it contains saponin and flavonoid. Saponin is a complex glycosydic compound consisted of triterpenoids or steroids. Saponin can be extracted from a plant by using a solvent extraction. Microwave Assisted Extraction (MAE) is a non-conventional extraction method that use micro waves in the process. This research was conducted by a Complete Random Design with two factors which were extraction time (120, 150, and 180 seconds) and solvent ratio (10:1, 15:1, and 20:1 v/w). The best treatment of MAE were the solvent ratio 15:1 (v/w) for 180 seconds. The best treatment resulting crude saponin extract yield of 41.46%, containing 11.53% total saponins, and 49.17% of antioxidant activity. Meanwhile, the treatment of maceration method were the solvent ratio 20:1 (v/w) for 48 hours resulting 39.86% yield of saponin crude extract, 9.26% total saponins and 56.23% of antioxidant activity. The results showed MAE was more efficient (less time of extraction and solvent amount) than maceration method.

  10. Study to find the best extraction solvent for use with guava leaves (Psidium guajava L.) for high antioxidant efficacy

    PubMed Central

    Seo, Jongkwon; Lee, Soojung; Elam, Marcus L; Johnson, Sarah A; Kang, Jonghoon; Arjmandi, Bahram H

    2014-01-01

    The effects of guava leaves extracted using solvents of water, ethanol, methanol, and different concentrations of hydroethanolic solvents on phenolic compounds and flavonoids, and antioxidant properties have been investigated. The antioxidant capability was assessed based on 2,2-diphenyl-1-picrylhydrazyl radical and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) radical-scavenging abilities, reducing power, and nitric oxide-and nitrate-scavenging activities. The results demonstrated that the antioxidant ability of guava leaf extracts has a strong relationship with phenolic compound content rather than flavonoid content. Phenolic compound content of water extracted guava leaves was higher compared to pure ethanol and methanol extracts. However, phenolic compound content extracted using hydroethanolic solvent was higher than water, whereas 50% hydroethanolic was observed to be the most effective solvent showing high antioxidant ability. PMID:24804076

  11. A combination of solvent extraction and freeze thaw for oil recovery from petroleum refinery wastewater treatment pond sludge.

    PubMed

    Hu, Guangji; Li, Jianbing; Hou, Haobo

    2015-01-01

    A combination of solvent extraction and freeze thaw was examined for recovering oil from the high-moisture petroleum refinery wastewater treatment pond sludge. Five solvents including cyclohexane (CHX), dichloromethane (DCM), methyl ethyl ketone (MEK), ethyl acetate (EA), and 2-propanol (2-Pro) were examined. It was found that these solvents except 2-Pro showed a promising oil recovery rate of about 40%, but the recycling of DCM solvent after oil extraction was quite low. Three solvents (CHX, MEK and EA) were then selected for examining the effect of freeze/thaw treatment on improving the quality of recovered oil. This treatment increased the total petroleum hydrocarbon (TPH) content in recovered oil from about 40% to 60% for both MEK and EA extractions, but little effect was observed for CHX extraction. Although the solid residue after oil recovery had a significantly decreased TPH content, a high concentration of heavy metals was observed, indicating that this residue may require proper management. In general, the combination of solvent extraction with freeze/thaw is effective for high-moisture oily hazardous waste treatment. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Optimisation of Microwave-Assisted Extraction of Pomegranate (Punica granatum L.) Seed Oil and Evaluation 
of Its Physicochemical and Bioactive Properties.

    PubMed

    Çavdar, Hasene Keskin; Yanık, Derya Koçak; Gök, Uğur; Göğüş, Fahrettin

    2017-03-01

    Pomegranate seed oil was extracted in a closed-vessel high-pressure microwave system. The characteristics of the obtained oil, such as fatty acid composition, free fatty acidity, total phenolic content, antioxidant activity and colour, were compared to those of the oil obtained by cold solvent extraction. Response surface methodology was applied to optimise extraction conditions: power (176-300 W), time (5-20 min), particle size ( d =0.125-0.800 mm) and solvent to sample ratio (2:1, 6:1 and 10:1, by mass). The predicted highest extraction yield (35.19%) was obtained using microwave power of 220 W, particle size in the range of d =0.125-0.450 mm and solvent-to-sample ratio of 10:1 (by mass) in 5 min extraction time. Microwave-assisted solvent extraction (MASE) resulted in higher extraction yield than that of Soxhlet (34.70% in 8 h) or cold (17.50% in 8 h) extraction. The dominant fatty acid of pomegranate seed oil was punicic acid (86%) irrespective of the extraction method. Oil obtained by MASE had better physicochemical properties, total phenolic content and antioxidant activity than the oil obtained by cold solvent extraction.

  13. Group extraction of organic compounds present in liquid samples

    NASA Technical Reports Server (NTRS)

    Jahnsen, Vilhelm J. (Inventor)

    1976-01-01

    An extraction device is disclosed comprising a tube containing a substantially inert, chemically non-reactive packing material with a large surface area to volume ratio. A sample which consists of organic compounds dissolved in a liquid, is introduced into the tube. As the sample passes through the packing material it spreads over the material's large surface area to form a thin liquid film which is held on the packing material in a stationary state. A particular group or family of compounds is extractable from the sample by passing a particular solvent system consisting of a solvent and selected reagents through the packing material. The reagents cause optimum conditions to exist for the compounds of the particular family to pass through the phase boundary between the sample liquid and the solvent of the solvent system. Thus, the compounds of the particular family are separated from the sample liquid and become dissolved in the solvent of the solvent system. The particular family of compounds dissolved in the solvent, representing an extract, exits the tube together with the solvent through the tube's nozzle, while the rest of the sample remains on the packing material in a stationary state. Subsequently, a different solvent system may be passed through the packing material to extract another family of compounds from the remaining sample on the packing material.

  14. EXTRACTION OF SEDIMENT-BOUND CHLORINATED ORGANIC COMPOUNDS: IMPLICATIONS ON FATE AND HAZARD ASSESSMENT. (R825513C007)

    EPA Science Inventory

    Five methods were used for the extraction of hexachlorobutadiene and chlorobenzenes from a contaminated estuarine sediment. The following extraction methods were used: Soxhlet extraction, sonication and solvent extraction, sequential solvent extraction, saponification and solv...

  15. Phenolic content and antioxidant activity of Hibiscus cannabinus L. seed extracts after sequential solvent extraction.

    PubMed

    Yusri, Noordin Mohd; Chan, Kim Wei; Iqbal, Shahid; Ismail, Maznah

    2012-10-25

    A sequential solvent extraction scheme was employed for the extraction of antioxidant compounds from kenaf (Hibiscus cannabinus L.) seeds. Yield of extracts varied widely among the solvents and was the highest for hexane extract (16.6% based on dry weight basis), while water extract exhibited the highest total phenolic content (18.78 mg GAE/g extract), total flavonoid content (2.49 mg RE/g extract), and antioxidant activities (p < 0.05). DPPH and hydroxyl radical scavenging, β-carotene bleaching, metal chelating activity, ferric thiocyanate and thiobarbituric acid reactive substances assays were employed to comprehensively assess the antioxidant potential of different solvent extracts prepared sequentially. Besides water, methanolic extract also exhibited high retardation towards the formation of hydroperoxides and thiobarbituric acid reactive substances in the total antioxidant activity tests (p < 0.05). As conclusion, water and methanol extracts of kenaf seed may potentially serve as new sources of antioxidants for food and nutraceutical applications.

  16. Effects of pH changes in water-based solvents to isolate antibacterial activated extracts of natural products

    NASA Astrophysics Data System (ADS)

    Buang, Yohanes; Suwari, Ola, Antonius R. B.

    2017-12-01

    Effects of pH changes in solvents on isolation of antibacterial activities of natural product extracts were conducted in the present study. Sarang semut (M. pendens) tubers as the model material for the study was considered to be the strategic resource of natural products based on its biochemical and therapeutical effects. The water with pH 5, 7, 9, and 13 was used as the solvents. The antibacterial activities of the resulted extracts indicated that higher the working pH, higher activities of the resulted extracts. The extent activities of the resulted extracts followed the increasing pH of the maceration system. The study also found that higher pH of the working solvent, higher the amounts of the antibacterial extracts isolated from the sample matrix of the natural product. The higher pH of the water solvents plays essential roles to promote the antibacterial activities of the natural product extracts from M. pendens tubers.

  17. Comparisons between conventional, ultrasound-assisted and microwave-assisted methods for extraction of anthraquinones from Heterophyllaea pustulata Hook f. (Rubiaceae).

    PubMed

    Barrera Vázquez, M F; Comini, L R; Martini, R E; Núñez Montoya, S C; Bottini, S; Cabrera, J L

    2014-03-01

    This work reports a comparative study about extraction methods used to obtain anthraquinones (AQs) from stems and leaves of Heterophyllae pustulata Hook (Rubiáceae). One of the conventional procedures used to extract these metabolites from a vegetable matrix is by successive Soxhlet extractions with solvents of increasing polarity: starting with hexane to eliminate chlorophylls and fatty components, following by benzene and finally ethyl acetate. However, this technique shows a low extraction yield of total AQs, and consumes large quantities of solvent and time. Ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) have been investigated as alternative methods to extract these compounds, using the same sequence of solvents. It was found that UAE increases the extraction yield of total AQs and reduces the time and amount of solvent used. Nevertheless, the combination UAE with benzene, plus MAE with ethyl acetate at a constant power of 900 W showed the best results. A higher yield of total AQs was obtained in less time and using the same amount of solvent that UAE. The optimal conditions for this latter procedure were UAE with benzene at 50 °C during 60 min, followed by MAE at 900 W during 15 min using ethyl acetate as extraction solvent. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Organosolv extraction of lignin from hydrolyzed almond shells and application of the delta-value theory.

    PubMed

    Quesada-Medina, Joaquín; López-Cremades, Francisco Javier; Olivares-Carrillo, Pilar

    2010-11-01

    The solubility of lignin from hydrolyzed almond (Prunus amygdalus) shells in different acetone, ethanol and dioxane-water mixtures and conditions (extraction time and temperature) was studied. The concept of the solubility parameter (delta-value) was applied to explain the effect of organic solvent concentration on lignin solubility. The organic solvent-water mixture that led to the highest lignin extraction was composed of a 75% vol. of organic solvent for all the solvent series investigated (acetone, ethanol and dioxane). Moreover, the best lignin extraction conditions were a temperature of 210 degrees C and an extraction time of 40 min for the acetone and ethanol series, and 25 min for the dioxane series. The delta-value of the hydrolyzed almond shell lignin [14.60 (cal/cm(3))(1/2)] and that of the organic solvent-water mixtures was calculated. The experimental delignification capacity of the aqueous organic solvents clearly reflected the proximity of their delta-value to that of lignin. The hydrogen-bonding capacity of the solvent-water mixtures was also taken into account. Copyright 2010 Elsevier Ltd. All rights reserved.

  19. Mass Transfer And Hydraulic Testing Of The V-05 And V-10 Contactors With The Next Generation Solvent

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Herman, D. T.; Duignan, M. R.; Williams, M. R.

    The Modular Caustic Side Solvent Extraction (CSSX) Unit (MCU) facility is actively pursuing the transition from the current BOBCalixC6 based solvent to the Next Generation Solvent (NGS)-MCU solvent. To support this integration of NGS into the MCU facilities, Savannah River Remediation (SRR) requested that Savannah River National Laboratory (SRNL) perform testing of a blend of the NGS (MaxCalix based solvent) with the current solvent (BOBCalixC6 based solvent) for the removal of cesium (Cs) from the liquid salt waste stream. This testing differs from prior testing by utilizing a blend of BOBCalixC6 based solvent and the NGS with the full (0.05more » M) concentration of the MaxCalix as well as a new suppressor, tris(3,7dimethyloctyl) guanidine. Single stage tests were conducted using the full size V-05 and V-10 centrifugal contactors installed at SRNL. These tests were designed to determine the mass transfer and hydraulic characteristics with the NGS solvent blended with the projected heel of the BOBCalixC6 based solvent that will exist in MCU at time of transition. The test program evaluated the amount of organic carryover and the droplet size of the organic carryover phases using several analytical methods. Stage efficiency and mass distribution ratios were determined by measuring Cs concentration in the aqueous and organic phases during single contactor testing. The nominal cesium distribution ratio, D(Cs) measured for extraction ranged from 37-60. The data showed greater than 96% stage efficiency for extraction. No significant differences were noted for operations at 4, 8 or 12 gpm aqueous salt simulant feed flow rates. The first scrub test (contact with weak caustic solution) yielded average scrub D(Cs) values of 3.3 to 5.2 and the second scrub test produced an average value of 1.8 to 2.3. For stripping behavior, the “first stage” D Cs) values ranged from 0.04 to 0.08. The efficiency of the low flow (0.27 gpm aqueous) was calculated to be 82.7%. The Spreadsheet Algorithm for Stagewise Solvent Extraction (SASSE) predicted equivalent DF for MCU from this testing is greater than 3,500 assuming 95% efficiency during extraction and 80% efficiency during scrub and strip. Hydraulically, the system performed very well in all tests. Target flows were easily obtained and stable throughout testing. Though some issues were encountered with plugging in the coalescer, they were not related to the solvent. No hydraulic upsets due to the solvent were experienced during any of the tests conducted. The first extraction coalescer element used in testing developed high pressure drop that made it difficult to maintain the target flow rates. Analysis showed an accumulation of sodium aluminosilicate solids. The coalescer was replaced with one from the same manufacturer’s lot and pressure drop was no longer an issue. Concentrations of Isopar™ L and Modifier were measured using semi-volatile organic analysis (SVOA) and high performance liquid chromatography (HPLC) to determine the amount of solvent carryover. For low-flow (0.27 gpm aqueous) conditions in stripping, SVOA measured the Isopar™ L post-contactor concentration to be 25 mg/L, HPLC measured 39 mg/L of Modifier. For moderate-flow (0.54 gpm aqueous) conditions, SVOA measured the Isopar™ L postcontactor to be ~69 mg/L, while the HPLC measured 56 mg/L for Modifier. For high-flow (0.8 gpm aqueous) conditions, SVOA measured the Isopar™ L post-contactor to be 39 mg/L. The post-coalescer (pre-decanter) measurements by SVOA for Isopar™ L were all less than the analysis detection limit of 10 mg/L. The HPLC measured 18, 22 and 20 mg/L Modifier for the low, medium, and high-low rates respectively. In extraction, the quantity of pre-coalescer Isopar™ L carryover measured by SVOA was ~280-410 mg/L at low flow (4 gpm aqueous), ~400-450 mg/L at moderate flow (8 gpm aqueous), and ~480 mg/L at high flow (12 gpm aqueous). The amount of post coalescer (pre-decanter) Isopar™ L carryover measured by SVOA was less than 45 mg/L for all flow rates. HPLC results for Modifier were 182, 217 and 222 mg/L for the post-contactor low, medium and high flow rates. The post-coalescer (pre-decanter) samples were measured to contain 12, 10 and 22 mg/L Modifier for the low, medium, and high flow rates. The carryover results and droplet size measurements were used to determine the decanter performance utilizing the decanter model developed by the ARES Corporation. Results show for the targeted salt flow rate of approximately 8 gpm, that over 93% of the solvent carryover from stripping is predicted to be recovered and over 96% solvent carryover from extraction is predicted to be recovered. This translates to a predicted solvent carryover of <3 ppm from stripping and <20 ppm solvent carryover from extraction. This projected performance at MCU is expected to be well within the operating limits and the historical performance for the baseline BOBCalixC6 based solvent. Droplet-size data obtained by MicroTrac™ S3400 analyzer consistently shows that the droplet size post-oalescer is significantly greater than the post-contactor or pre-coalescer samples. Increased flow rates did not show a consistent impact to the droplet size results. For the extraction testing, droplet size analysis showed that the post-contactor and pre-coalescer samples were essentially the same. The mean droplet sizes post-coalescer were less than the mean droplet sizes pre-coalescer with a very slight upward trend in the mean droplet size as the flow rate was increased. This result is probably due to the method of sampling. The larger post-coalescer drops immediately rise to the surface after leaving the coalescer element. The downstream sampling point was horizontally in-line with the element and therefore would only capture those organic droplets well mixed in the flowing aqueous stream.« less

  20. Supercritical multicomponent solvent coal extraction

    NASA Technical Reports Server (NTRS)

    Corcoran, W. H.; Fong, W. S.; Pichaichanarong, P.; Chan, P. C. F.; Lawson, D. D. (Inventor)

    1983-01-01

    The yield of organic extract from the supercritical extraction of coal with larger diameter organic solvents such as toluene is increased by use of a minor amount of from 0.1 to 10% by weight of a second solvent such as methanol having a molecular diameter significantly smaller than the average pore diameter of the coal.

  1. Oil recovery from petroleum sludge through ultrasonic assisted solvent extraction.

    PubMed

    Hu, Guangji; Li, Jianbing; Huang, Shuhui; Li, Yubao

    2016-09-18

    The effect of ultrasonic assisted extraction (UAE) process on oil recovery from refinery oily sludge was examined in this study. Two types of UAE treatment including UAE probe (UAEP) system and UAE bath (UAEB) system were investigated. Their oil recovery efficiencies were compared to that of mechanical shaking extraction (MSE). Three solvents including cyclohexane (CHX), ethyl acetate (EA), and methyl ethyl ketone (MEK) were examined as the extraction solvents. The influence of experimental factors on oil and solvent recovery was investigated using an orthogonal experimental design. Results indicated that solvent type, solvent-to-sludge (S/S) ratio, and treatment duration could have significant effects on oil recovery in UAE treatment. Under the optimum conditions, UAEP treatment can obtain an oil recovery of 68.8% within 20 s, which was higher than that (i.e., 62.0%) by MSE treatment after 60 min' extraction. UAEB treatment can also obtain a promising oil recovery within shorter extraction duration (i.e., 15 min) than MSE. UAE was thus illustrated as an effective and improved approach for oily sludge recycling.

  2. Alternatives for Benzene in the Extraction of Bitumen Fume from Exposure Sample Media.

    PubMed

    Sutter, Benjamin; Ravera, Christel; Hussard, Caroline; Langlois, Eddy

    2016-01-01

    Benzene is frequently used to extract collected bitumen fumes from personal sampler substrates. However, this solvent is particularly dangerous because of its carcinogenicity (group 1 of the International Agency for Research on Cancer classification). Therefore, to prevent the exposure of laboratory technicians to benzene during the fume extraction step from samplers, a compromise had to be found to identify a less toxic solvent with the same extraction capacity. To compare the extraction capacities of selected solvents, bitumen fumes were generated in the laboratory from three different batches of road surfacing bitumen collected on dedicated bitumen fume samplers. The samplers were then extracted by benzene and the solvents tested. Of 11 selected solvents less toxic than benzene and used in studies on bitumen and bitumen fume analyses, n-hexane and n-heptane were identified as alternatives to benzene. In particular, the results demonstrated that n-heptane was the best candidate solvent for benzene replacement, due to its extraction efficiency comparable to benzene for the three bitumen fumes tested and its low toxicity, which is highly compatible with benzene replacement. © The Author 2015. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.

  3. Operator care and eco-concerned development of a fast, facile and economical assay for basic nitrogenous drugs based on simplified ion-pair mini-scale extraction using safer solvent combined with drop-based spectrophotometry.

    PubMed

    Plianwong, Samarwadee; Sripattanaporn, Areerut; Waewsa-nga, Kwanrutai; Buacheen, Parin; Opanasopit, Praneet; Ngawhirunpat, Tanasait; Rojanarata, Theerasak

    2012-08-30

    A fast, facile, and economical assay for basic nitrogenous drugs has been developed based on the mini-scale extraction of the drug-dye ion pair complex combined with the use of safe-for-analyst and eco-friendlier organic extractant and drop-based micro-spectrophotometry. Instead of using large volume devices, the extraction was simply carried out in typical 1.5 mL microcentrifuge tubes along with the use of micropipettes for accurate transfer of liquids, vortex mixer for efficient partitioning of solutes and benchtop centrifuge for rapid phase separation. In the last step, back-extraction was performed by using the microvolume of acidic solution in order to concentrate the colored species into a confined aqueous microdrop and to keep the analyst away from unwanted contact and inhalation of organic solvents during the quantitation step which was achieved by using cuvetteless UV-vis micro-spectrophotometry without any prior dilutions. Using chlorpheniramine maleate as a representative analyte and n-butyl acetate as a less toxic and non-ozone depleting extractant, the miniaturized method was less laborious and much faster. It was accurate, precise and insensitive to the interferences from common excipients. Notably, it gave the assay results of drug in tablets and oral solution comparable to the large-scale pharmacopeial method while the consumption of organic solvents and the release of wastes were lowered by 200-400 folds. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. 40 CFR 63.2860 - What notifications must I submit and when?

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... National Emission Standards for Hazardous Air Pollutants: Solvent Extraction for Vegetable Oil Production... address of the owner or operator. (2) The physical address of the vegetable oil production process. (3) Identification of the relevant standard, such as the vegetable oil production NESHAP, and compliance date. (4) A...

  5. 40 CFR 63.2860 - What notifications must I submit and when?

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... National Emission Standards for Hazardous Air Pollutants: Solvent Extraction for Vegetable Oil Production... address of the owner or operator. (2) The physical address of the vegetable oil production process. (3) Identification of the relevant standard, such as the vegetable oil production NESHAP, and compliance date. (4) A...

  6. Optimisation and validation of the microwave-assisted extraction of phenolic compounds from rice grains.

    PubMed

    Setyaningsih, W; Saputro, I E; Palma, M; Barroso, C G

    2015-02-15

    A new microwave-assisted extraction (MAE) method has been investigated for the extraction of phenolic compounds from rice grains. The experimental conditions studied included temperature (125-175°C), microwave power (500-1000W), time (5-15min), solvent (10-90% EtOAc in MeOH) and solvent-to-sample ratio (10:1 to 20:1). The extraction variables were optimised by the response surface methodology. Extraction temperature and solvent were found to have a highly significant effect on the response value (p<0.0005) and the extraction time also had a significant effect (p<0.05). The optimised MAE conditions were as follows: extraction temperature 185°C, microwave power 1000W, extraction time 20min, solvent 100% MeOH, and solvent-to-sample ratio 10:1. The developed method had a high precision (in terms of CV: 5.3% for repeatability and 5.5% for intermediate precision). Finally, the new method was applied to real samples in order to investigate the presence of phenolic compounds in a wide variety of rice grains. Copyright © 2014 Elsevier Ltd. All rights reserved.

  7. Alternative Bio-Based Solvents for Extraction of Fat and Oils: Solubility Prediction, Global Yield, Extraction Kinetics, Chemical Composition and Cost of Manufacturing

    PubMed Central

    Sicaire, Anne-Gaëlle; Vian, Maryline; Fine, Frédéric; Joffre, Florent; Carré, Patrick; Tostain, Sylvain; Chemat, Farid

    2015-01-01

    The present study was designed to evaluate the performance of alternative bio-based solvents, more especially 2-methyltetrahydrofuran, obtained from crop’s byproducts for the substitution of petroleum solvents such as hexane in the extraction of fat and oils for food (edible oil) and non-food (bio fuel) applications. First a solvent selection as well as an evaluation of the performance was made with Hansen Solubility Parameters and the COnductor-like Screening MOdel for Realistic Solvation (COSMO-RS) simulations. Experiments were performed on rapeseed oil extraction at laboratory and pilot plant scale for the determination of lipid yields, extraction kinetics, diffusion modeling, and complete lipid composition in term of fatty acids and micronutrients (sterols, tocopherols and tocotrienols). Finally, economic and energetic evaluations of the process were conducted to estimate the cost of manufacturing using 2-methyltetrahydrofuran (MeTHF) as alternative solvent compared to hexane as petroleum solvent. PMID:25884332

  8. Supercritical solvent coal extraction

    NASA Technical Reports Server (NTRS)

    Compton, L. E. (Inventor)

    1984-01-01

    Yields of soluble organic extract are increased up to about 50% by the supercritical extraction of particulate coal at a temperature below the polymerization temperature for coal extract fragments (450 C.) and a pressure from 500 psig to 5,000 psig by the conjoint use of a solvent mixture containing a low volatility, high critical temperature coal dissolution catalyst such as phenanthrene and a high volatility, low critical temperature solvent such as toluene.

  9. Supercritical fluid extraction from spent coffee grounds and coffee husks: antioxidant activity and effect of operational variables on extract composition.

    PubMed

    Andrade, Kátia S; Gonçalvez, Ricardo T; Maraschin, Marcelo; Ribeiro-do-Valle, Rosa Maria; Martínez, Julian; Ferreira, Sandra R S

    2012-01-15

    The present study describes the chemical composition and the antioxidant activity of spent coffee grounds and coffee husks extracts, obtained by supercritical fluid extraction (SFE) with CO(2) and with CO(2) and co-solvent. In order to evaluate the high pressure method in terms of process yield, extract composition and antioxidant activity, low pressure methods, such as ultrasound (UE) and soxhlet (SOX) with different organic solvents, were also applied to obtain the extracts. The conditions for the SFE were: temperatures of 313.15K, 323.15K and 333.15K and pressures from 100 bar to 300 bar. The SFE kinetics and the mathematical modeling of the overall extraction curves (OEC) were also investigated. The extracts obtained by LPE (low pressure extraction) with ethanol showed the best results for the global extraction yield (X(0)) when compared to SFE results. The best extraction yield was 15±2% for spent coffee grounds with ethanol and 3.1±04% for coffee husks. The antioxidant potential was evaluated by DPPH method, ABTS method and Folin-Ciocalteau method. The best antioxidant activity was showed by coffee husk extracts obtained by LPE. The quantification and the identification of the extracts were accomplished using HPLC analysis. The main compounds identified were caffeine and chlorogenic acid for the supercritical extracts from coffee husks. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Ionic Liquids as Extraction Media for Metal Ions

    NASA Astrophysics Data System (ADS)

    Hirayama, Naoki

    In solvent extraction separation of metal ions, recently, many researchers have investigated possible use of hydrophobic ionic liquids as extraction media instead of organic solvents. Ionic liquids are salts of liquid state around room temperature and can act not only as solvents but also as ion-exchangers. Therefore, the extraction mechanism of metal ions into ionic liquids is complicated. This review presents current overview and perspective on evaluation of nature of hydrophobic ionic liquids as extraction media for metal ions.

  11. Effect of Piper betle L. and its extracts on the growth and aflatoxin production by Aspergillus parasiticus.

    PubMed

    Chou, C C; Yu, R C

    1984-01-01

    Ground powder of the leaf and fruit of Piper betle L., a tropical spice plant grown in Southeast Asia, was prepared and extracted by chloroform, ethanol and water with one solvent only or with 3 solvents in sequence. The betel powder and various extracts were added to YES broth to determine their effects on the growth and aflatoxin production by Aspergillus parasiticus. Results showed that betel leaf powder exhibited higher antimycotic activity than fruit. One half percent of ground leaf powder completely inhibited the growth and aflatoxin production by A. parasiticus. Among the solvent extracts, chloroform and ethanol extracts of betel leaf prepared from a single solvent extraction showed more antimycotic activity. The ethanol extract of betel leaf at the level of 450 micrograms/ml would eliminate A. parasiticus growth and aflatoxin production. The antimycotic activity of this ethanol extract was most pronounced at pH 4.

  12. FY10 Report on Multi-scale Simulation of Solvent Extraction Processes: Molecular-scale and Continuum-scale Studies

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Wardle, Kent E.; Frey, Kurt; Pereira, Candido

    2014-02-02

    This task is aimed at predictive modeling of solvent extraction processes in typical extraction equipment through multiple simulation methods at various scales of resolution. We have conducted detailed continuum fluid dynamics simulation on the process unit level as well as simulations of the molecular-level physical interactions which govern extraction chemistry. Through combination of information gained through simulations at each of these two tiers along with advanced techniques such as the Lattice Boltzmann Method (LBM) which can bridge these two scales, we can develop the tools to work towards predictive simulation for solvent extraction on the equipment scale (Figure 1). Themore » goal of such a tool-along with enabling optimized design and operation of extraction units-would be to allow prediction of stage extraction effrciency under specified conditions. Simulation efforts on each of the two scales will be described below. As the initial application of FELBM in the work performed during FYl0 has been on annular mixing it will be discussed in context of the continuum-scale. In the future, however, it is anticipated that the real value of FELBM will be in its use as a tool for sub-grid model development through highly refined DNS-like multiphase simulations facilitating exploration and development of droplet models including breakup and coalescence which will be needed for the large-scale simulations where droplet level physics cannot be resolved. In this area, it can have a significant advantage over traditional CFD methods as its high computational efficiency allows exploration of significantly greater physical detail especially as computational resources increase in the future.« less

  13. PROCESS FOR THE RECOVERY OF URANIUM FROM PHOSPHATIC ORE

    DOEpatents

    Long, R.L.

    1959-04-14

    A proccss is described for the recovery of uranium from phosphatic products derived from phosphatic ores. It has been discovered that certain alkyl phosphatic, derivatives can be employed in a direct solvent extraction operation to recover uranium from solid products, such as superphosphates, without first dissolving such solids. The organic extractants found suitable include alkyl derivatives of phosphoric, pyrophosphoric, phosof the derivative contains from 4 to 7 carbon atoms. A diluent such as kerosene is also used.

  14. Comparative Analysis of Chemical Composition, Antioxidant Activity and Quantitative Characterization of Some Phenolic Compounds in Selected Herbs and Spices in Different Solvent Extraction Systems.

    PubMed

    Sepahpour, Shabnam; Selamat, Jinap; Abdul Manap, Mohd Yazid; Khatib, Alfi; Abdull Razis, Ahmad Faizal

    2018-02-13

    This study evaluated the efficacy of various organic solvents (80% acetone, 80% ethanol, 80% methanol) and distilled water for extracting antioxidant phenolic compounds from turmeric, curry leaf, torch ginger and lemon grass extracts. They were analyzed regarding the total phenol and flavonoid contents, antioxidant activity and concentration of some phenolic compounds. Antioxidant activity was determined by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging assay and the ferric reducing antioxidant power (FRAP) assay. Quantification of phenolic compounds was carried out using high-performance liquid chromatography (HPLC). All the extracts possessed antioxidant activity, however, the different solvents showed different efficiencies in the extraction of phenolic compounds. Turmeric showed the highest DPPH values (67.83-13.78%) and FRAP (84.9-2.3 mg quercetin/g freeze-dried crude extract), followed by curry leaf, torch ginger and lemon grass. While 80% acetone was shown to be the most efficient solvent for the extraction of total phenolic compounds from turmeric, torch ginger and lemon grass (221.68, 98.10 and 28.19 mg GA/g freeze dried crude extract, respectively), for the recovery of phenolic compounds from curry leaf (92.23 mg GA/g freeze-dried crude extract), 80% ethanol was the most appropriate solvent. Results of HPLC revealed that the amount of phenolic compounds varied depending on the types of solvents used.

  15. Central composite design parameterization of microalgae/cyanobacteria co-culture pretreatment for enhanced lipid extraction using an external clamp-on ultrasonic transducer.

    PubMed

    Ellison, Candice R; Overa, Sean; Boldor, Dorin

    2018-05-19

    Lipids extracted from algal biomass could provide an abundant, rapidly growing, high yield feedstock for bio-diesel and other green fuels to supplement current fossil-based sources. Ultrasound pretreatment is a mechanical cell disruption method that has been shown to enhance lipid recovery from algae due to cavitation effects that disrupt algae cell walls. In this study, a locally grown mixture of Chlorella vulgaris/Cyanobacteria leptolyngbya was sonicated in an ultrasonic reactor with a clamp-on transducer prior to solvent lipid extraction. This configuration allows for a non-contact delivery method of ultrasonic energy with improved operational advantages (no fouling of transducer, continuous operation, and fully scalable design). A central composite design (CCD) was implemented to statistically analyze and evaluate the effect of ultrasonic power (350-750 W) and treatment time (5-30 min) on lipid yield. Lipid recovery was found to increase with both ultrasonic power and treatment time. Total lipid yields (on dry biomass basis) extracted via the Bligh and Dyer method from Chlorella vulgaris/cyanobacteria co-culture ranged from 8.3% for untreated algae to 16.9% for algae sonicated with 750 W power for 30 min, which corresponds to more than a doubling of lipid recovery due to ultrasound pretreatment. Increased power and treatment times were found to increase the degree of cell disruption as observed in the SEM and TEM images after ultrasonic pretreatment. Additionally, hexane (1:1 v/v) was evaluated as an alternative to the standard Bligh & Dyer (2:2:1.8 v/v/v chloroform/methanol/cell suspension) lipid extraction solvent system. On average, the Bligh and Dyer method extracted on average over twice the amount of lipids compared to hexane extraction. The lipid profile of the algae extracts indicates high concentrations of lauric acid (12:0), palmitic acid (16:0), stearic acid (18:0), oleic acid (18:1), and linoleic acid (18:2). This particular configuration of an ultrasonic system proved to be a viable method for the pretreatment of algae for enhanced lipid yields. Future research should focus on identifying alternative extraction solvents and expanding the range of treatment conditions to optimize the ultrasonic power and treatment times for maximum lipid recovery. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. ASE extraction method for simultaneous carbon and nitrogen stable isotope analysis in soft tissues of aquatic organisms.

    PubMed

    Bodin, Nathalie; Budzinski, Hélène; Le Ménach, Karyn; Tapie, Nathalie

    2009-06-08

    Since lipids are depleted in 13C relative to proteins and carbohydrates, variations in lipid composition among species and within individuals significantly influence delta13C and may result in misleading ecological interpretations. Whereas lipid extraction before IRMS analysis constitutes a way of stable isotope result lipid-normalisation, such a procedure was given up because of the un-controlled effects of the methods used (i.e., "Bligh & Dyer", Soxhlet, etc.) on delta15N. The aim of this work was to develop a simple, rapid and efficient lipid extraction method allowing for simultaneous C and N stable isotope analysis in the biological soft tissues of aquatic organisms. The goal was to be free from the lipid influence on delta13C values without interfering with delta15N values. For that purpose, the modern automated pressurized liquid extraction technique ASE (accelerated solvent extraction) was selected. Eel muscles representative of a broad range of fat contents were extracted via ASE by using different semi-polar solvents (100% dichloromethane and 80% n-hexane/20% acetone) and by operating at different temperature (ambient temperature and 100 degrees C) and pressure (750 and 1900 psi) conditions. The results were discussed in terms of lipid extraction efficiency as well as delta13C and delta15N variability.

  17. Free radical scavenging of grape pomace extracts from Cabernet sauvingnon (Vitis vinifera).

    PubMed

    de Campos, Luanda M A S; Leimann, Fernanda V; Pedrosa, Rozangela Curi; Ferreira, Sandra R S

    2008-11-01

    Pressed grape pomace obtained from the wine production of Cabernet sauvignon (Vitis vinifera) vintage was dried until 9.8% moisture content, ground and submitted to extraction of soluble components from different extraction techniques. Low pressure extractions were performed with ethanol maceration followed by fractionation with n-hexane, dichloromethane, butanol and ethyl acetate. These solvents were furthermore applied for soxhlet extraction. Supercritical fluid extraction (SFE) was also performed to obtain grape pomace extracts by using pure CO2 and CO2 with ethanol as co-solvent in concentrations of 10, 15 and 20%w/w. The operating condition used in high pressure extractions was 150bar and 40 degrees C. The antioxidant activity of the grape pomace extracts was determined considering the free radical scavenging assay using 1,1-Diphenyl-2-picrylhydrazyl (DPPH) and was correlated with the total phenol content determined according to the Folin-Ciocalteu method. The results obtained in DPPH tests indicate the highest antioxidant activity of 96.6+/-0.3%AA, with an IC50 value of 13+/-1, for the extracts obtained with ethyl acetate in solid-liquid extraction. The highest yield values were achieved in soxhlet extraction with ethanol (13.2%w/w) and with butanol (12.2%w/w), and also by SFE with 15% ethanol (9.2%w/w). The lipophilic composition of grape pomace extracts was evaluated by gas chromatography-mass spectrometry with the identification of components like linoleic acid and ethyl linoleate, with important therapeutic activities.

  18. Optimisation of Microwave-Assisted Extraction of Pomegranate (Punica granatum L.) Seed Oil and Evaluation 
of Its Physicochemical and Bioactive Properties

    PubMed Central

    Çavdar, Hasene Keskin; Gök, Uğur; Göğüş, Fahrettin

    2017-01-01

    Summary Pomegranate seed oil was extracted in a closed-vessel high-pressure microwave system. The characteristics of the obtained oil, such as fatty acid composition, free fatty acidity, total phenolic content, antioxidant activity and colour, were compared to those of the oil obtained by cold solvent extraction. Response surface methodology was applied to optimise extraction conditions: power (176–300 W), time (5–20 min), particle size (d=0.125–0.800 mm) and solvent to sample ratio (2:1, 6:1 and 10:1, by mass). The predicted highest extraction yield (35.19%) was obtained using microwave power of 220 W, particle size in the range of d=0.125–0.450 mm and solvent-to-sample ratio of 10:1 (by mass) in 5 min extraction time. Microwave-assisted solvent extraction (MASE) resulted in higher extraction yield than that of Soxhlet (34.70% in 8 h) or cold (17.50% in 8 h) extraction. The dominant fatty acid of pomegranate seed oil was punicic acid (86%) irrespective of the extraction method. Oil obtained by MASE had better physicochemical properties, total phenolic content and antioxidant activity than the oil obtained by cold solvent extraction. PMID:28559737

  19. Cesium and strontium extraction using a mixed extractant solvent including crown ether and calixarene extractants

    DOEpatents

    Meikrantz, David H.; Todd, Terry A.; Riddle, Catherine L.; Law, Jack D.; Peterman, Dean R.; Mincher, Bruce J.; McGrath, Christopher A.; Baker, John D.

    2007-11-06

    A mixed extractant solvent including calix[4]arene-bis-(tert-octylbenzo)-crown-6 ("BOBCalixC6"), 4',4',(5')-di-(t-butyldicyclo-hexano)-18-crown-6 ("DtBu18C6"), and at least one modifier dissolved in a diluent. The mixed extractant solvent may be used to remove cesium and strontium from an acidic solution. The DtBu18C6 may be present from approximately 0.01 M to approximately 0.4M, such as from approximately 0.086 M to approximately 0.108 M. The modifier may be 1-(2,2,3,3-tetrafluoropropoxy)-3-(4-sec-butylphenoxy)-2-propanol ("Cs-7SB") and may be present from approximately 0.01M to approximately 0.8M. In one embodiment, the mixed extractant solvent includes approximately 0.15M DtBu18C6, approximately 0.007M BOBCalixC6, and approximately 0.75M Cs-7SB modifier dissolved in an isoparaffinic hydrocarbon diluent. The mixed extractant solvent may form an organic phase in an extraction system that also includes an aqueous phase. Methods of extracting cesium and strontium as well as strontium alone are also disclosed.

  20. Effect of various solvent on the specific amino acids of black soybean (Glycine soja) sprout

    NASA Astrophysics Data System (ADS)

    Kanetro, B.; Slamet, A.; Wazyka, A.

    2018-01-01

    The objective of this research was to study the effect of various solvent extractions on the specific amino acids as small peptide or free amino acids that was contained in the extract after removal of the macromolecule protein of black soybean sprouts. The experimental design of this research was randomized complete design with one factor, which was the three various solvent, i.e. hexane, ethanol and water. The black soybean seed was germinated for 36 h. The small peptide and free amino acids of black soybean sprout were isolated at 3 various of solvents extraction, and then the macromolecule proteins in the extracts were precipitated at the pH 4. The extracts of black soybean sprout after removal of the macromolecule protein were analysed by HPLC to determine the profile of amino acids for stimulation of insulin secretion. The result of this research showed that the extracts contained the small peptide and free amino acid for stimulation of insulin secretion. The best solvent extraction was water that was due to the content of Leu, Arg, Ala, Phe, Ile, and Lys of water extract was higher than hexane and ethanol extracts.

  1. Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

    PubMed

    Sadeghi, Susan; Ashoori, Vahid

    2017-10-01

    The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  2. Alternative and Efficient Extraction Methods for Marine-Derived Compounds

    PubMed Central

    Grosso, Clara; Valentão, Patrícia; Ferreres, Federico; Andrade, Paula B.

    2015-01-01

    Marine ecosystems cover more than 70% of the globe’s surface. These habitats are occupied by a great diversity of marine organisms that produce highly structural diverse metabolites as a defense mechanism. In the last decades, these metabolites have been extracted and isolated in order to test them in different bioassays and assess their potential to fight human diseases. Since traditional extraction techniques are both solvent- and time-consuming, this review emphasizes alternative extraction techniques, such as supercritical fluid extraction, pressurized solvent extraction, microwave-assisted extraction, ultrasound-assisted extraction, pulsed electric field-assisted extraction, enzyme-assisted extraction, and extraction with switchable solvents and ionic liquids, applied in the search for marine compounds. Only studies published in the 21st century are considered. PMID:26006714

  3. Extraction of phenolic compounds from extra virgin olive oil by a natural deep eutectic solvent: Data on UV absorption of the extracts.

    PubMed

    Paradiso, Vito Michele; Clemente, Antonia; Summo, Carmine; Pasqualone, Antonella; Caponio, Francesco

    2016-09-01

    This data article refers to the paper "Towards green analysis of virgin olive oil phenolic compounds: extraction by a natural deep eutectic solvent and direct spectrophotometric detection" [1]. A deep eutectic solvent (DES) based on lactic acid and glucose was used as green solvent for phenolic compounds. Eight standard phenolic compounds were solubilized in the DES. Then, a set of extra virgin olive oil (EVOO) samples (n=65) were submitted to liquid-liquid extraction by the DES. The standard solutions and the extracts were analyzed by UV spectrophotometry. This article reports the spectral data of both the standard solutions and the 65 extracts, as well as the total phenolic content of the corresponding oils, assessed by the Folin-Ciocalteu assay.

  4. An interesting two-phase solvent system and its use in preparative isolation of aconitines from aconite roots by counter-current chromatography.

    PubMed

    Han, Quan-Bin; Tang, Wai-Lun; Dong, Cai-Xia; Xu, Hong-Xi; Jiang, Zhi-Hong

    2013-04-01

    Two-phase solvent system plays crucial role in successful separation of organic compounds using counter-current chromatography (CCC). An interesting two-phase solvent system, composed of chloroform/ethyl acetate/methanol/water, is reported here, in which both phases contain sufficient organic solvents to balance their dissolving capacities. Adjusting the solvent system to get satisfactory partition coefficients (K values) for target compounds becomes relatively simple. This solvent system succeeded in sample preparation of aconitine (8.07 mg, 93.69%), hypaconitine (7.74 mg, 93.17%), mesaconitine (1.95 mg, 94.52%) from raw aconite roots (102.24 mg, crude extract), benzoylmesaconine (34.79 mg, 98.67%) from processed aconite roots (400.01 mg, crude extract), and yunaconitine (253.59 mg, 98.65%) from a crude extract of Aconitum forrestii (326.69 mg, crude extract). © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Optimization of flavanones extraction by modulating differential solvent densities and centrifuge temperatures.

    PubMed

    Chebrolu, Kranthi K; Jayaprakasha, G K; Jifon, J; Patil, Bhimanagouda S

    2011-07-15

    Understanding the factors influencing flavonone extraction is critical for the knowledge in sample preparation. The present study was focused on the extraction parameters such as solvent, heat, centrifugal speed, centrifuge temperature, sample to solvent ratio, extraction cycles, sonication time, microwave time and their interactions on sample preparation. Flavanones were analyzed in a high performance liquid chromatography (HPLC) and later identified by liquid chromatography and mass spectrometry (LC-MS). The five flavanones were eluted by a binary mobile phase with 0.03% phosphoric acid and acetonitrile in 20 min and detected at 280 nm, and later identified by mass spectral analysis. Dimethylsulfoxide (DMSO) and dimethyl formamide (DMF) had optimum extraction levels of narirutin, naringin, neohesperidin, didymin and poncirin compared to methanol (MeOH), ethanol (EtOH) and acetonitrile (ACN). Centrifuge temperature had a significant effect on flavanone distribution in the extracts. The DMSO and DMF extracts had homogeneous distribution of flavanones compared to MeOH, EtOH and ACN after centrifugation. Furthermore, ACN showed clear phase separation due to differential densities in the extracts after centrifugation. The number of extraction cycles significantly increased the flavanone levels during extraction. Modulating the sample to solvent ratio increased naringin quantity in the extracts. Current research provides critical information on the role of centrifuge temperature, extraction solvent and their interactions on flavanone distribution in extracts. Published by Elsevier B.V.

  6. Extraction of organic compounds with room temperature ionic liquids.

    PubMed

    Poole, Colin F; Poole, Salwa K

    2010-04-16

    Room temperature ionic liquids are novel solvents with a rather specific blend of physical and solution properties that makes them of interest for applications in separation science. They are good solvents for a wide range of compounds in which they behave as polar solvents. Their physical properties of note that distinguish them from conventional organic solvents are a negligible vapor pressure, high thermal stability, and relatively high viscosity. They can form biphasic systems with water or low polarity organic solvents and gases suitable for use in liquid-liquid and gas-liquid partition systems. An analysis of partition coefficients for varied compounds in these systems allows characterization of solvent selectivity using the solvation parameter model, which together with spectroscopic studies of solvent effects on probe substances, results in a detailed picture of solvent behavior. These studies indicate that the solution properties of ionic liquids are similar to those of polar organic solvents. Practical applications of ionic liquids in sample preparation include extractive distillation, aqueous biphasic systems, liquid-liquid extraction, liquid-phase microextraction, supported liquid membrane extraction, matrix solvents for headspace analysis, and micellar extraction. The specific advantages and limitations of ionic liquids in these studies is discussed with a view to defining future uses and the need not to neglect the identification of new room temperature ionic liquids with physical and solution properties tailored to the needs of specific sample preparation techniques. The defining feature of the special nature of ionic liquids is not their solution or physical properties viewed separately but their unique combinations when taken together compared with traditional organic solvents. Copyright 2009 Elsevier B.V. All rights reserved.

  7. Headspace single drop microextraction coupled with microwave extraction of essential oil from plant materials.

    PubMed

    Zhai, Yujuan; Sun, Shuo; Wang, Ziming; Zhang, Yupu; Liu, He; Sun, Ye; Zhang, Hanqi; Yu, Aimin

    2011-05-01

    Headspace single drop microextraction (HS-SDME) coupled with microwave extraction (ME) was developed and applied to the extraction of the essential oil from dried Syzygium aromaticum (L.) Merr. et Perry and Cuminum cyminum L. The operational parameters, such as microdrop volume, microwave absorption medium (MAM), extraction time, and microwave power were optimized. Ten microliters of decane was used as the microextraction solvent. Ionic liquid and carbonyl iron powder were used as MAM. The extraction time was less than 7 min at the microwave power of 440 W. The proposed method was compared with hydrodistillation (HD). There were no obvious differences in the constituents of essential oils obtained by the two methods.

  8. Analysis of edible oil processing options for the BIO-Plex advanced life support system

    NASA Technical Reports Server (NTRS)

    Greenwalt, C. J.; Hunter, J.

    2000-01-01

    Edible oil is a critical component of the proposed plant-based Advanced Life Support (ALS) diet. Soybean, peanut, and single-cell oil are the oil source options to date. In terrestrial manufacture, oil is ordinarily extracted with hexane, an organic solvent. However, exposed solvents are not permitted in the spacecraft environment or in enclosed human tests by National Aeronautics and Space Administration due to their potential danger and handling difficulty. As a result, alternative oil-processing methods will need to be utilized. Preparation and recovery options include traditional dehulling, crushing, conditioning, and flaking, extrusion, pressing, water extraction, and supercritical extraction. These processing options were evaluated on criteria appropriate to the Advanced Life Support System and BIO-Plex application including: product quality, product stability, waste production, risk, energy needs, labor requirements, utilization of nonrenewable resources, usefulness of by-products, and versatility and mass of equipment to determine the most appropriate ALS edible oil-processing operation.

  9. Process for enhancing the value of hydrocabonaceous natural recources

    DOEpatents

    Bunger, James W.; Cogswell, Donald E.

    2005-04-05

    A process for upgrading hydrocarbonaceous oil containing heteroatom-containing compounds where the hydrocarbonaceous oil is contacted with a solvent system that is a mixture of a major portion of a polar solvent having a dipole moment greater than about 1 debye and a minor portion of water to selectively separate the constituents of the carbonaceous oil into a heteroatom-depleted raffinate fraction and heteroatom-enriched extract fraction. The polar solvent and the water-in-solvent system are formulated at a ratio where the water is an antisolvent in an amount to inhibit solubility of heteroatom-containing compounds and the polar solvent in the raffinate, and to inhibit solubility of non-heteroatom-containing compounds in the extract. The ratio of the hydrocarbonaceous oil to the solvent system is such that a coefficient of separation is at least 50%. The coefficient of separation is the mole percent of heteroatom-containing compounds from the carbonaceous oil that are recovered in the extract fraction minus the mole percent of non-heteroatom-containing compounds from the carbonaceous oil that are recovered in the extract fraction. The solvent-free extract and the raffinate concentrates may be used directly or processed to make valuable petroleum, chemical or industrial products.

  10. Optimisation of the recovery of carotenoids from tomato processing wastes: application on textile dyeing and assessment of its antioxidant activity.

    PubMed

    Baaka, Noureddine; El Ksibi, Imen; Mhenni, Mohamed Farouk

    2017-01-01

    The present study has been focused on the extraction of natural pigments from tomato industry waste. At first, different solvents and solvents mixture were compared to determine which one is the best for extracting carotenoids compounds from tomato by-products. A mixture of hexane and acetone gave the highest carotenoids extraction yield among the others examined. The extraction conditions were optimised using a five-level-five-factor central composite design. Under optimal conditions, solvent solid ratio 90, hexane percentage in the solvent mixture 60, extraction duration 50, number of extractions 4 and extraction temperature 35 °C, the yield of carotenoids was 80.7 μg/g. The coloured extract of tomato by-products was applied on textile fabrics to investigate the dyeing characteristics and antioxidant activities. The results indicate that extract can be applied on textile fabrics (wool, silk and polyamide) to produce coloured clothing with acceptable antioxidant properties.

  11. MICROWAVE-ASSISTED EXTRACTION OF PHENOLIC COMPOUNDS FROM POLYGONUM MULTIFLORUM THUNB. ROOTS.

    PubMed

    Quoc, Le Pham Tan; Muoi, Nguyen Van

    2016-01-01

    The aim of this study was to determine the best extraction conditions for total phenolic content (TPC) and antioxidant capacity (AC) of Polygonum multiflorum Thunb. root using microwave-assisted extraction (MAE). The raw material used was Polygonum multiflorum Thunb. root powder. Five factors such as solvent type, solvent concentrations, solvent/material ratio, extraction time and microwave power were studied; TPC and AC values were determined by the Folin-Ciocalteu method and DPPH free radical scavenging activity measurement, respectively. In addition, studies involved assaying the HPLC test of extracts and SEM of samples. Optimal results pointed to acetone as the solvent, acetone concentration of 60%, solvent/material ratio of 40/1 (v/w), extraction time of 5 mins and microwave power of 127 W. TPC and AC obtained were approximates 44.3 ±0.13 mg GAE/g DW and 341.26 ±1.54 μmol TE/g DW, respectively. The effect of microwaving on the cell destruction of Polygonum multiflorum Thunb. root was observed by scanning electron microscopy (SEM). Some phenolic compounds were determined by the HPLC method, for instance, gallic acid, catechin and resveratrol. These factors significantly affected TPC and AC. We can use acetone as a solvent with microwave-assisted extraction to achieve the best result.

  12. Ultrasonically assisted extraction of total phenols and flavonoids from Rhodiola rosea.

    PubMed

    Staneva, Jordanka; Todorova, Milka; Neykov, Neyko; Evstatieva, Ljuba

    2009-07-01

    This work deals with ultrasonically assisted extraction (UAE) of biologically active compounds from rhizomes of Rhodiola rosea, a popular medicinal plant. The influence of temperature, type of solvent and solid/solvent ratio on the yield of total extracts, total phenols and flavonoids was established. The best extraction of total phenols and flavonoids was achieved by using 50% aqueous EtOH and MeOH, respectively. Five times increase of solid/solvent ratio (from 1:20 to 1:100 (w/v)) leads to slow increase of the yield of total phenols and flavonoids. The extraction effectiveness of conventional maceration with 50% EtOH and UAE performed for 1 h at 25 degrees C using the same solvent with respect of total phenols was comparable.

  13. Green ultrasound-assisted extraction of carotenoids based on the bio-refinery concept using sunflower oil as an alternative solvent.

    PubMed

    Li, Ying; Fabiano-Tixier, Anne Sylvie; Tomao, Valérie; Cravotto, Giancarlo; Chemat, Farid

    2013-01-01

    A green, inexpensive and easy-to-use method for carotenoids extraction from fresh carrots assisted by ultrasound was designed in this work. Sunflower oil was applied as a substitute to organic solvents in this green ultrasound-assisted extraction (UAE): a process which is in line with green extraction and bio-refinery concepts. The processing procedure of this original UAE was first compared with conventional solvent extraction (CSE) using hexane as solvent. Moreover, the UAE optimal conditions for the subsequent comparison were optimized using response surface methodology (RSM) and ultra performance liquid chromatography--diode array detector--mass spectroscopy (UPLC-DAD-MS). The results showed that the UAE using sunflower as solvent has obtained its highest β-carotene yield (334.75 mg/l) in 20 min only, while CSE using hexane as solvent obtained a similar yield (321.35 mg/l) in 60 min. The green UAE performed under optimal extraction conditions (carrot to oil ratio of 2:10, ultrasonic intensity of 22.5 W cm(-2), temperature of 40 °C and sonication time of 20 min) gave the best yield of β-carotene. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Analysis of polycyclic aromatic hydrocarbons in water and beverages using membrane-assisted solvent extraction in combination with large volume injection-gas chromatography-mass spectrometric detection.

    PubMed

    Rodil, Rosario; Schellin, Manuela; Popp, Peter

    2007-09-07

    Membrane-assisted solvent extraction (MASE) in combination with large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) was applied for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. The MASE conditions were optimized for achieving high enrichment of the analytes from aqueous samples, in terms of extraction conditions (shaking speed, extraction temperature and time), extraction solvent and composition (ionic strength, sample pH and presence of organic solvent). Parameters like linearity and reproducibility of the procedure were determined. The extraction efficiency was above 65% for all the analytes and the relative standard deviation (RSD) for five consecutive extractions ranged from 6 to 18%. At optimized conditions detection limits at the ng/L level were achieved. The effectiveness of the method was tested by analyzing real samples, such as river water, apple juice, red wine and milk.

  15. Reactive extraction at liquid-liquid systems

    NASA Astrophysics Data System (ADS)

    Wieszczycka, Karolina

    2018-01-01

    The chapter summarizes the state of knowledge about a metal transport in two-phase system. The first part of this review focuses on the distribution law and main factors determination in classical solvent extraction (solubility and polarity of the solute, as well as inter- and intramolecules interaction. Next part of the chapter is devoted to the reactive solvent extraction and the molecular modeling requiring knowledge on type of extractants, complexation mechanisms, metals ions speciation and oxidation during complexes forming, and other parameters that enable to understand the extraction process. Also the kinetic data that is needed for proper modeling, simulation and design of processes needed for critical separations are discussed. Extraction at liquid-solid system using solvent impregnated resins is partially identical as in the case of the corresponding solvent extraction, therefore this subject was also presented in all aspects of separation process (equilibrium, mechanism, kinetics).

  16. Clean-in-Place and Reliability Testing of a Commercial 12.5-cm Annular Centrifugal Contactor at the INL

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    N. R. Mann; T. G. Garn; D. H. Meikrantz

    2007-09-01

    The renewed interest in advancing nuclear energy has spawned the research of advanced technologies for recycling nuclear fuel. A significant portion of the advanced fuel cycle includes the recovery of selected actinides by solvent extraction methods utilizing centrifugal contactors. Although the use of centrifugal contactors for solvent extraction is widely known, their operation is not without challenges. Solutions generated from spent fuel dissolution contain unknown quantities of undissolved solids. A majority of these solids will be removed via various methods of filtration. However, smaller particles are expected to carry through to downstream solvent extraction processes and equipment. In addition, solids/precipitatesmore » brought about by mechanical or chemical upsets are another potential area of concern. During processing, particulate captured in the rotor assembly by high centrifugal forces eventually forms a cake-like structure on the inner wall introducing balance problems and negatively affecting phase separations. One of the features recently developed for larger engineering scale Annular Centrifugal Contactors (ACCs) is the Clean-In-Place (CIP) capability. Engineered spray nozzles were installed into the hollow central rotor shaft in all four quadrants of the rotor assembly. This arrangement allows for a very convenient and effective method of solids removal from within the rotor assembly.« less

  17. Clean-in-Place and Reliability Testing of a Commercial 12.5 cm Annular Centrifugal Contactor at the INL

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    N. R. Mann; T. G. Garn; D. H. Meikrantz

    2007-09-01

    The renewed interest in advancing nuclear energy has spawned the research of advanced technologies for recycling nuclear fuel. A significant portion of the advanced fuel cycle includes the recovery of selected actinides by solvent extraction methods utilizing centrifugal contactors. Although the use of centrifugal contactors for solvent extraction is widely known, their operation is not without challenges. Solutions generated from spent fuel dissolution contain unknown quantities of undissolved solids. A majority of these solids will be removed via various methods of filtration. However, smaller particles are expected to carry through to downstream solvent extraction processes and equipment. In addition, solids/precipitatesmore » brought about by mechanical or chemical upsets are another potential area of concern. During processing, particulate captured in the rotor assembly by high centrifugal forces eventually forms a cake-like structure on the inner wall introducing balance problems and negatively affecting phase separations. One of the features recently developed for larger engineering scale Annular Centrifugal Contactors (ACCs) is the Clean-In-Place (CIP) capability. Engineered spray nozzles were installed into the hollow central rotor shaft in all four quadrants of the rotor assembly. This arrangement allows for a very convenient and effective method of solids removal from within the rotor assembly.« less

  18. A survey of extraction solvents in the forensic analysis of textile dyes.

    PubMed

    Groves, Ethan; Palenik, Christopher S; Palenik, Skip

    2016-11-01

    The characterization and identification of dyes in fibers can be used to provide investigative leads and strengthen associations between known and questioned items of evidence. The isolation of a dye from its matrix (e.g., a textile fiber) permits detailed characterization, comparison and, in some cases, identification using methods such as thin layer chromatography in conjunction with infrared and Raman spectroscopy. A survey of dye extraction publications reveals that pyridine:water (4:3) is among the most commonly cited extraction solvent across a range of fiber and dye chemistries. Here, the efficacy of this solvent system has been evaluated for the extraction of dyes from 172 commercially prevalent North American textile dyes. The evaluated population represents seven dye application classes, 18 chemical classes, and spans nine types of commercial textile fibers. The results of this survey indicate that ∼82% of the dyestuffs studied are extractable using this solvent system. The results presented here summarize the extraction efficacy by class and fiber type and illustrate that this solvent system is applicable to a wider variety of classes and fibers than previously indicated in the literature. While there is no universal solvent for fiber extraction, these results demonstrate that pyridine:water represents an excellent first step for extracting unknown dyes from questioned fibers in forensic casework. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  19. Method for recovering and using lignin in adhesive resins by extracting demethylated lignin

    DOEpatents

    Schroeder, Herbert A.

    1991-01-01

    Lignin, or a lignin derived material, which has been significantly demethylated (e.g., the demethylated lignin found in the raffinate produced as a by-product of dimethyl sulfide production which can be carried out using the spent liquor from wood pulping operations) can be isolated by a process wherein an organic solvent is added to a lignin-containing aqueous solution. The organic solvent is typically a polar, and at least a partially water-immiscible substance such as, for example, ethyl acetate. The resulting lignin-containing aqueous solution/organic solvent mixture is acidified to produce a water layer which is discarded and an organic solvent layer which contains the demethylated lignin. Upon its recovery, the demethylated lignin is preferably dried and stored until it is used (along with an alkali, an aldehyde and an adhesive filler) in compounding an adhesive of the type generally used in the manufacture of plywood.

  20. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F. F.; Jones, D. H.

    Savannah River National Laboratory (SRNL) received one set of three Solvent Hold Tank (SHT) samples (MCU-16-1363-1364-1365), pulled on 11/15/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1363-1364-1365 indicated the Isopar™L concentration is at its nominal level (100%). The extractant (MaxCalix) and the modifier (CS- 7SB) are 8% and 2 % below their nominal concentrations. The suppressor (TiDG) is 7% below its nominal concentration. This analysis confirms the trim and Isopar™ additions to the solvent in November. This analysis also indicates the solvent did not require further additions. Based on the current monthlymore » sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less

  1. Method for recovering and using lignin in adhesive resins by extracting demethylated lignin

    DOEpatents

    Schroeder, Herbert A.

    1991-01-01

    Lignin, or a lignin derived material, which has been significantly demethylated (e.g., the demethylated lignin found in the raffinate produced as a by-product of dimethyl sulfide production which can be carried out using the spent liquor from wood pulping operations) can be isolated by a process wherein an organic solvent is added to a lignin-containing aqueous solution. The organic solvent is typically a polar, and at least a partially water-immiscible substance such as, for example, ethyl acetate. The resulting lignin-containing aqueous solution/organic solvent mixture is acidified to produce a water layer which is discarded and an organic solvent layer which contains the demethylated lignin. Upon its recovery, the demethylated lignin is dissolved in an alkaline solution to which an aldehyde source is added to produce a resol-type resin. The aldehyde source may be formaldehyde in solution, paraformaldehyde, hexamethylenetetramine, or other aldehydes including acetaldehyde, furfural, and their derivatives.

  2. Optimization of an accelerated solvent extraction dispersive liquid-liquid microextraction method for the separation and determination of essential oil from Ligusticum chuanxiong Hort by gas chromatography with mass spectrometry.

    PubMed

    Yang, Guang; Sun, Qiushi; Hu, Zhiyan; Liu, Hua; Zhou, Tingting; Fan, Guorong

    2015-10-01

    In this study, an accelerated solvent extraction dispersive liquid-liquid microextraction coupled with gas chromatography and mass spectrometry was established and employed for the extraction, concentration and analysis of essential oil constituents from Ligusticum chuanxiong Hort. Response surface methodology was performed to optimize the key parameters in accelerated solvent extraction on the extraction efficiency, and key parameters in dispersive liquid-liquid microextraction were discussed as well. Two representative constituents in Ligusticum chuanxiong Hort, (Z)-ligustilide and n-butylphthalide, were quantitatively analyzed. It was shown that the qualitative result of the accelerated solvent extraction dispersive liquid-liquid microextraction approach was in good agreement with that of hydro-distillation, whereas the proposed approach took far less extraction time (30 min), consumed less plant material (usually <1 g, 0.01 g for this study) and solvent (<20 mL) than the conventional system. To sum up, the proposed method could be recommended as a new approach in the extraction and analysis of essential oil. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. 40 CFR 63.2832 - Am I subject to this subpart?

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Standards for Hazardous Air Pollutants: Solvent Extraction for Vegetable Oil Production What This Subpart... operate a vegetable oil production process that is a major source of HAP emissions or is collocated within... emissions. (i) A vegetable oil production process is defined in § 63.2872. In general, it is the collection...

  4. 40 CFR 63.2832 - Am I subject to this subpart?

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Standards for Hazardous Air Pollutants: Solvent Extraction for Vegetable Oil Production What This Subpart... operate a vegetable oil production process that is a major source of HAP emissions or is collocated within... emissions. (i) A vegetable oil production process is defined in § 63.2872. In general, it is the collection...

  5. Supercritical-Multiple-Solvent Extraction From Coal

    NASA Technical Reports Server (NTRS)

    Corcoran, W.; Fong, W.; Pichaichanarong, P.; Chan, P.; Lawson, D.

    1983-01-01

    Large and small molecules dissolve different constituents. Experimental apparatus used to test supercritical extraction of hydrogen rich compounds from coal in various organic solvents. In decreasing order of importance, relevant process parameters were found to be temperature, solvent type, pressure, and residence time.

  6. In-tube electro-membrane extraction with a sub-microliter organic solvent consumption as an efficient technique for synthetic food dyes determination in foodstuff samples.

    PubMed

    Bazregar, Mohammad; Rajabi, Maryam; Yamini, Yadollah; Asghari, Alireza; Abdossalami asl, Yousef

    2015-09-04

    A simple and efficient extraction technique with a sub-microliter organic solvent consumption termed as in-tube electro-membrane extraction (IEME) is introduced. This method is based upon the electro-kinetic migration of ionized compounds by the application of an electrical potential difference. For this purpose, a thin polypropylene (PP) sheet placed inside a tube acts as a support for the membrane solvent, and 30μL of an aqueous acceptor solution is separated by this solvent from 1.2mL of an aqueous donor solution. This method yielded high extraction recoveries (63-81%), and the consumption of the organic solvent used was only 0.5μL. By performing this method, the purification is high, and the utilization of the organic solvent, used as a mediator, is very simple and repeatable. The proposed method was evaluated by extraction of four synthetic food dyes (Amaranth, Ponceau 4R, Allura Red, and Carmoisine) as the model analytes. Optimization of variables affecting the method was carried out in order to achieve the best extraction efficiency. These variables were the type of membrane solvent, applied extraction voltage, extraction time, pH range, and concentration of salt added. Under the optimized conditions, IEME-HPLC-UV provided a good linearity in the range of 1.00-800ngmL(-1), low limits of detection (0.3-1ngmL(-1)), and good extraction repeatabilities (RSDs below 5.2%, n=5). It seems that this design is a proper one for the automation of the method. Also the consumption of the organic solvent in a sub-microliter scale, and its simplicity, high efficiency, and high purification can help one getting closer to the objectives of the green chemistry. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. [Study on ultrafine vibration extraction technology of Rhizoma Chuanxiong].

    PubMed

    Dai, Long

    2009-04-01

    To explore the best ultrafine vibration extraction technology of Rhizoma Chuanxiong. Using the content of ligustrazine hydrochloride and ferulic acid as determination indexes, quadrature test was used to choose extraction times, time, solvent amount and to compare with the result of conventional extraction technology. The best condition of the Rhizoma chuanxiong was with 90% ethanol of 4 times volume, extracting 2 times in 25 degrees C, 15 minutes each time. Comparing with conventional extraction technology, extraction time of UVET was 1/6, solvent amount was 4/7, the extraction rate of marker components was 1.19 and 1.09 times, respectivley. UVET can improve the extracting rate of effective constituents, reduce the time and solvent amount and be used in industrialization.

  8. High-efficient extraction of principal medicinal components from fresh Phellodendron bark (cortex phellodendri).

    PubMed

    Xu, Keqin; He, Gongxiu; Qin, Jieming; Cheng, Xuexiang; He, Hanjie; Zhang, Dangquan; Peng, Wanxi

    2018-05-01

    There are three key medicinal components (phellodendrine, berberine and palmatine) in the extracts of Phellodendron bark, as one of the fundamental herbs of traditional Chinese medicine. Different extraction methods and solvent combinations were investigated to obtain the optimal technologies for high-efficient extraction of these medicinal components. The results showed that combined solvents have higher extracting effect of phellodendrine, berberine and palmatine than single solvent, and the effect of ultrasonic extraction is distinctly better than those of distillation and soxhlet extraction. The hydrochloric acid/methanol-ultrasonic extraction has the best effect for three medicinal components of fresh Phellodendron bark, providing an extraction yield of 103.12 mg/g berberine, 24.41 mg/g phellodendrine, 1.25 mg/g palmatine.

  9. Nonflammable, Nonaqueous, Low Atmospheric Impact, High Performance Cleaning Solvents

    NASA Technical Reports Server (NTRS)

    Dhooge, P. M.; Glass, S. M.; Nimitz, J. S.

    2001-01-01

    For many years, chlorofluorocarbon (CFC) and chlorocarbon solvents have played an important part in aerospace operations. These solvents found extensive use as cleaning and analysis (EPA) solvents in precision and critical cleaning. However, CFCs and chlorocarbon solvents have deleterious effects on the ozone layer, are relatively strong greenhouse gases, and some are suspect or known carcinogens. Because of their ozone-depletion potential (ODP), the Montreal Protocol and its amendments, as well as other environmental regulations, have resulted in the phaseout of CFC-113 and 1,1,1-trichloroethane (TCA). Although alternatives have been recommended, they do not perform as well as the original solvents. In addition, some analyses, such as the infrared analysis of extracted hydrocarbons, cannot be performed with the substitute solvents that contain C-H bonds. CFC-113 solvent has been used for many critical aerospace applications. CFC-113, also known as Freon (registered) TF, has been used extensively in NASA's cleaning facilities for precision and critical cleaning, in particular the final rinsing in Class 100 areas, with gas chromatography analysis of rinse residue. While some cleaning can be accomplished by other processes, there are certain critical applications where CFC-113 or a similar solvent is highly cost-effective and ensures safety. Oxygen system components are one example where a solvent compatible with oxygen and capable of removing fluorocarbon grease is needed. Electronic components and precision mechanical components can also be damaged by aggressive cleaning solvents.

  10. Development of a novel ultrasound-assisted headspace liquid-phase microextraction and its application to the analysis of chlorophenols in real aqueous samples.

    PubMed

    Xu, Hui; Liao, Ying; Yao, Jinrong

    2007-10-05

    A new sample pretreatment technique, ultrasound-assisted headspace liquid-phase microextraction was developed as mentioned in this paper. In the technique, the volatile analytes were headspace extracted into a small drop of solvent, which suspended on the bottom of a cone-shaped PCR tube instead of the needle tip of a microsyringe. More solvent could be suspended in the PCR tube than microsyringe due to the larger interfacial tension, thus the analysis sensitivity was significantly improved with the increase of the extractant volume. Moreover, ultrasound-assisted extraction and independent controlling temperature of the extractant and the sample were performed to enhance the extraction efficiency. Following the extraction, the solvent-loaded sample was analyzed by high-performance liquid chromatography. Chlorophenols (2-chlorophenol, 2,4-dichlorophenol and 2,6-dichlorophenol) were chosen as model analytes to investigate the feasibility of the method. The experimental conditions related to the extraction efficiency were systematically studied. Under the optimum experimental conditions, the detection limit (S/N=3), intra- and inter-day RSD were 6 ng mL(-1), 4.6%, 3.9% for 2-chlorophenol, 12 ng mL(-1), 2.4%, 8.8% for 2,4-dichlorophenol and 23 ng mL(-1), 3.3%, 5.3% for 2,6-dichlorophenol, respectively. The proposed method was successfully applied to determine chlorophenols in real aqueous samples. Good recoveries ranging from 84.6% to 100.7% were obtained. In addition, the extraction efficiency of our method and the conventional headspace liquid-phase microextraction were compared; the extraction efficiency of the former was about 21 times higher than that of the latter. The results demonstrated that the proposed method is a promising sample pretreatment approach, its advantages over the conventional headspace liquid-phase microextraction include simple setup, ease of operation, rapidness, sensitivity, precision and no cross-contamination. The method is very suitable for the analysis of trace volatile and semivolatile pollutants in real aqueous sample.

  11. Inulin rich carbohydrates extraction from Jerusalem artichoke (Helianthus tuberosus L.) tubers and application of different drying methods.

    PubMed

    Rubel, Irene A; Iraporda, Carolina; Novosad, Rocio; Cabrera, Fernanda A; Genovese, Diego B; Manrique, Guillermo D

    2018-01-01

    In this study the operational extraction variables to obtain higher yields of inulin from Jerusalem artichoke tubers (JAT), as well as the optimal conditions to obtain a stable and dispersible powdered product by either spray or freeze drying, were studied. With this purpose, the powder yield, moisture content, water activity and flowability or products obtained by different experimental conditions were analyzed. Inulin rich carbohydrates (IRC) extraction was performed from lyophilized and ground tubers employing distilled hot water as solvent. It was proved that the solid:solvent ratio (S:S) was the critical variable in the extraction process, followed by temperature. Thus, the IRC extraction was optimal without ultrasound assistance, at 76°C, employing a S:S of 1:16, during 90min. In addition, the powder obtained by freeze-drying of the IRC extract showed advantages respect to powders obtained by spray-drying regarding the yield and considering that maltodextrin was not necessary as encapsulation agent. In another hand, spray drying process provided IRC powered materials with appropriate flow properties, and taking into account cost and time of production, this method should be considered as an alternative of freeze-drying. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Solvent-assisted dispersive micro-SPE by using aminopropyl-functionalized magnetite nanoparticle followed by GC-PID for quantification of parabens in aqueous matrices.

    PubMed

    Abbasghorbani, Maryam; Attaran, Abdolmohammad; Payehghadr, Mahmood

    2013-01-01

    In this research, solvent-assisted dispersive micro-SPE was introduced as a simple modified technique for the determination of parabens in water and cosmetic samples. Aminopropyl-functionalized magnetite nanoparticles (MNPs) were successfully synthesized and applied. GC with photoionization detector was used for the separation and detection of parabens. In this method, hexylacetate (15 μL) as a solvent and aminopropyl-functionalized MNPs (5 μg) as a sorbent were added to an aqueous sample (10 mL) and then the sample was sonicated. Dispersed magnetite was collected in the bottom of the conical tube by using a strong magnet and then ACN was added as a desorption solvent. Forty microliters of this solvent was transferred into a microvial and then acetic anhydride and pyridine were added, thus derivatization was performed by acetic anhydride. After evaporation, 1 μL of derivatized sample was injected into a gas chromatograph for analysis. Several important parameters, such as kind of organic solvent, desorption solvent and volume, amount of aminopropyl-functionalized MNPs and effect of salt addition were investigated. Under optimum conditions, the limits of detection achieved were between 50 and 300 ng/L, with RSDs (n = 5) lower than 8%. Under the optimum conditions, the enrichment factors ranged from 217 to 1253 and the extraction recoveries ranged from 10 to 62%. The recoveries were obtained for the analytes in river water and mouthwash solution and hand cream in the range of 87-103%. The advantages of proposed method are simplicity of operation, rapidity, high extraction yields, and environmental friendly character. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Further development of a robust workup process for solution-phase high-throughput library synthesis to address environmental and sample tracking issues.

    PubMed

    Kuroda, Noritaka; Hird, Nick; Cork, David G

    2006-01-01

    During further improvement of a high-throughput, solution-phase synthesis system, new workup tools and apparatus for parallel liquid-liquid extraction and evaporation have been developed. A combination of in-house design and collaboration with external manufacturers has been used to address (1) environmental issues concerning solvent emissions and (2) sample tracking errors arising from manual intervention. A parallel liquid-liquid extraction unit, containing miniature high-speed magnetic stirrers for efficient mixing of organic and aqueous phases, has been developed for use on a multichannel liquid handler. Separation of the phases is achieved by dispensing them into a newly patented filter tube containing a vertical hydrophobic porous membrane, which allows only the organic phase to pass into collection vials positioned below. The vertical positioning of the membrane overcomes the hitherto dependence on the use of heavier-than-water, bottom-phase, organic solvents such as dichloromethane, which are restricted due to environmental concerns. Both small (6-mL) and large (60-mL) filter tubes were developed for parallel phase separation in library and template synthesis, respectively. In addition, an apparatus for parallel solvent evaporation was developed to (1) remove solvent from the above samples with highly efficient recovery and (2) avoid the movement of individual samples between their collection on a liquid handler and registration to prevent sample identification errors. The apparatus uses a diaphragm pump to achieve a dynamic circulating closed system with a heating block for the rack of 96 sample vials and an efficient condenser to trap the solvents. Solvent recovery is typically >98%, and convenient operation and monitoring has made the apparatus the first choice for removal of volatile solvents.

  14. Evaluation of new natural deep eutectic solvents for the extraction of isoflavones from soy products.

    PubMed

    Bajkacz, Sylwia; Adamek, Jakub

    2017-06-01

    Natural deep eutectic solvents (NADESs) are considered to be new, safe solvents in green chemistry that can be widely used in many chemical processes such as extraction or synthesis. In this study, a simple extraction method based on NADES was used for the isolation of isoflavones (daidzin, genistin, genistein, daidzein) from soy products. Seventeen different NADES systems each including two or three components were tested. Multivariate data analysis revealed that NADES based on a 30% solution of choline chloride: citric acid (molar ratio of 1:1) are the most effective systems for the extraction of isoflavones from soy products. After extraction, the analytes were detected and quantified using ultra-high performance liquid chromatography with ultraviolet detection (UHPLC-UV). The proposed NADES extraction procedure achieved enrichment factors up to 598 for isoflavones and the recoveries of the analytes were in the range 64.7-99.2%. The developed NADES extraction procedure and UHPLC-UV determination method was successfully applied for the analysis of isoflavones in soy-containing food samples. The obtained results indicated that new natural deep eutectic solvents could be an alternative to traditional solvents for the extraction of isoflavones and can be used as sustainable and safe extraction media for another applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Thiolene and SIFEL-based Microfluidic Platforms for Liquid-Liquid Extraction

    PubMed Central

    Goyal, Sachit; Desai, Amit V.; Lewis, Robert W.; Ranganathan, David R.; Li, Hairong; Zeng, Dexing; Reichert, David E.; Kenis, Paul J.A.

    2014-01-01

    Microfluidic platforms provide several advantages for liquid-liquid extraction (LLE) processes over conventional methods, for example with respect to lower consumption of solvents and enhanced extraction efficiencies due to the inherent shorter diffusional distances. Here, we report the development of polymer-based parallel-flow microfluidic platforms for LLE. To date, parallel-flow microfluidic platforms have predominantly been made out of silicon or glass due to their compatibility with most organic solvents used for LLE. Fabrication of silicon and glass-based LLE platforms typically requires extensive use of photolithography, plasma or laser-based etching, high temperature (anodic) bonding, and/or wet etching with KOH or HF solutions. In contrast, polymeric microfluidic platforms can be fabricated using less involved processes, typically photolithography in combination with replica molding, hot embossing, and/or bonding at much lower temperatures. Here we report the fabrication and testing of microfluidic LLE platforms comprised of thiolene or a perfluoropolyether-based material, SIFEL, where the choice of materials was mainly guided by the need for solvent compatibility and fabrication amenability. Suitable designs for polymer-based LLE platforms that maximize extraction efficiencies within the constraints of the fabrication methods and feasible operational conditions were obtained using analytical modeling. To optimize the performance of the polymer-based LLE platforms, we systematically studied the effect of surface functionalization and of microstructures on the stability of the liquid-liquid interface and on the ability to separate the phases. As demonstrative examples, we report (i) a thiolene-based platform to determine the lipophilicity of caffeine, and (ii) a SIFEL-based platform to extract radioactive copper from an acidic aqueous solution. PMID:25246730

  16. Ultrasound-assisted extraction of three bufadienolides from Chinese medicine ChanSu.

    PubMed

    Sun, Yinshi; Bi, Jianjie; Zhang, Li; Ye, Baoxing

    2012-11-01

    In this study, the application of ultrasound-assisted extraction (UAE) method was shown to be more efficient in extracting anti-tumor bufadienolides (bufalin, cinobufagin and resibufogenin) from important animal medicine of ChanSu than the maceration extraction (ME) and soxhlet extraction (SE) method. The effects of ultrasonic variables including extraction solvent, solvent concentration, solvent to solid ratio, ultrasound power, temperature, extraction time and particle size on the yields of three bufadienolides were investigated. The optimum extraction conditions found were: 70% (v/v) methanol solution, solvent to solid ratio of 10ml/g, ultrasound power of 125W, temperature of 20°C, extraction time of 20min and particle size of 60-80 mesh. The extraction yields of bufalin, cinobufagin and resibufogenin were 43.17±0.85, 52.58±1.12, 137.70±2.65mg/g, respectively. In order to achieve a similar yield as UAE, soxhlet extraction required 6h and maceration extraction required much longer time of 18h. The results indicated that UAE is an alternative method for extracting bufadienolides from ChanSu. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. DEMONSTRATION BULLETIN: TERRA KLEEN SOLVENT EXTRACTION TECHNOLOGY - TERRA-KLEEN RESPONSE GROUP, INC.

    EPA Science Inventory

    The Terra-Kleen Solvent Extraction Technology was developed by Terra-Kleen Response Group, Inc., to remove polychlorinated biphenyls (PCB) and other organic constituents from contaminated soil. This batch process system uses a proprietary solvent at ambient temperatures to treat ...

  18. Research News: Emulsion Liquid Membrane Extraction in a Hollow-Fiber Contactor

    NASA Technical Reports Server (NTRS)

    Wiencek, John M.; Hu, Shih-Yao

    2000-01-01

    This article describes how ELMs (emulsion liquid membranes) can be used for extraction. The article addresses the disadvantages of ELM extraction in a stirred contactor, and the advantages of SELMs (supported emulsion liquid membranes). The introduction of the article provides background information on liquid-liquid solvent extraction and dispersion-free solvent extraction.

  19. AN EVALUATION OF SAMPLE DISPERSION MEDIAS USED WITH ACCELERATED SOLVENT EXTRACTION FOR THE EXTRACTION AND RECOVERY OF ARSENICALS FROM LFB AND DORM-2

    EPA Science Inventory

    An accelerated solvent extraction (ASE) device was evaluated as a semi-automated means for extracting arsenicals from quality control (QC) samples and DORM-2 [standard reference material (SRM)]. Unlike conventional extraction procedures, the ASE requires that the sample be dispe...

  20. A combination strategy for extraction and isolation of multi-component natural products by systematic two-phase solvent extraction-(13)C nuclear magnetic resonance pattern recognition and following conical counter-current chromatography separation: Podophyllotoxins and flavonoids from Dysosma versipellis (Hance) as examples.

    PubMed

    Yang, Zhi; Wu, Youqian; Wu, Shihua

    2016-01-29

    Despite of substantial developments of extraction and separation techniques, isolation of natural products from natural resources is still a challenging task. In this work, an efficient strategy for extraction and isolation of multi-component natural products has been successfully developed by combination of systematic two-phase liquid-liquid extraction-(13)C NMR pattern recognition and following conical counter-current chromatography separation. A small-scale crude sample was first distributed into 9 systematic hexane-ethyl acetate-methanol-water (HEMWat) two-phase solvent systems for determination of the optimum extraction solvents and partition coefficients of the prominent components. Then, the optimized solvent systems were used in succession to enrich the hydrophilic and lipophilic components from the large-scale crude sample. At last, the enriched components samples were further purified by a new conical counter-current chromatography (CCC). Due to the use of (13)C NMR pattern recognition, the kinds and structures of major components in the solvent extracts could be predicted. Therefore, the method could collect simultaneously the partition coefficients and the structural information of components in the selected two-phase solvents. As an example, a cytotoxic extract of podophyllotoxins and flavonoids from Dysosma versipellis (Hance) was selected. After the systematic HEMWat system solvent extraction and (13)C NMR pattern recognition analyses, the crude extract of D. versipellis was first degreased by the upper phase of HEMWat system (9:1:9:1, v/v), and then distributed in the two phases of the system of HEMWat (2:8:2:8, v/v) to obtain the hydrophilic lower phase extract and lipophilic upper phase extract, respectively. These extracts were further separated by conical CCC with the HEMWat systems (1:9:1:9 and 4:6:4:6, v/v). As results, total 17 cytotoxic compounds were isolated and identified. In general, whole results suggested that the strategy was very efficient for the systematic extraction and isolation of biological active components from the complex biomaterials. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. A comparison of certain extracting agents for extraction of adenosine triphosphate (ATP) from microorganisms for use in the firefly luciferase ATP assay

    NASA Technical Reports Server (NTRS)

    Knust, E. A.; Chappelle, E. W.; Picciolo, G. L.

    1975-01-01

    Firefly luciferase ATP assay is used in clinical and industrial applications, such as determination of urinary infection levels, microbial susceptibility testing, and monitoring of yeast levels in beverages. Three categories of extractants were investigated for their extracting efficiency. They were ionizing organic solvents, nonionizing organic solvents, and inorganic acids. Dimethylsulfoxide and formamide represented the ionizing organic solvents, while n-butanol, chloroform, ethanol, acetone, and methylene chloride were used for the nonionizing organic solvents. Nitric acid and perchloric acid were chosen for the inorganic acids category. Pathogens were tested with each solvent. They included: Saccharomyces carlsbergensis, E. coli, Staphylococcus aureus, Klebsiella pneumoniae, Enterobacter species, Proteus mirabilis, Proteus vulgaris, Staphylococcus epidermidis, Streptococcus faecalis, Pseudomonas aeruginosa, and Candida albicans. These results are shown in graphic representations.

  2. AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

    DOEpatents

    Van Berkel, Gary J.

    2015-06-23

    An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

  3. Optimisation of Croton gratissimus Oil Extraction by n-Hexane and Ethyl Acetate Using Response Surface Methodology.

    PubMed

    Jiyane, Phiwe Charles; Tumba, Kaniki; Musonge, Paul

    2018-04-01

    The extraction of oil from Croton gratissimus seeds was studied using the three-factor five-level full-factorial central composite rotatable design (CCRD) of the response surface methodology (RSM). The effect of the three factors selected, viz., extraction time, extraction temperature and solvent-to-feed ratio on the extraction oil yield was investigated when n-hexane and ethyl acetate were used as extraction solvents. The coefficients of determination (R 2 ) of the models developed were 0.98 for n-hexane extraction and 0.97 for ethyl acetate extraction. These results demonstrated that the models developed adequately represented the processes they described. From the optimized model, maximum extraction yield obtained from n-hexane and ethyl acetate extraction were 23.88% and 23.25%, respectively. In both cases the extraction temperature and solvent-to-feed ratio were 35°C and 5 mL/g, respectively. In n-hexane extraction the maximum conditions were reached only after 6 min whereas in ethyl acetate extraction it took 20 min to get the maximum extraction oil yield. Oil extraction of Croton gratissimus seeds, in this work, favoured the use of n-hexane as an extraction solvent as it offered higher oil yields at low temperatures and reduced residence times.

  4. MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

    EPA Science Inventory

    The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

  5. Extraction of basil leaves (ocimum canum) oleoresin with ethyl acetate solvent by using soxhletation method

    NASA Astrophysics Data System (ADS)

    Tambun, R.; Purba, R. R. H.; Ginting, H. K.

    2017-09-01

    The goal of this research is to produce oleoresin from basil leaves (Ocimum canum) by using soxhletation method and ethyl acetate as solvent. Basil commonly used in culinary as fresh vegetables. Basil contains essential oils and oleoresin that are used as flavouring agent in food, in cosmetic and ingredient in traditional medicine. The extraction method commonly used to obtain oleoresin is maceration. The problem of this method is many solvents necessary and need time to extract the raw material. To resolve the problem and to produce more oleoresin, we use soxhletation method with a combination of extraction time and ratio from the material with a solvent. The analysis consists of yield, density, refractive index, and essential oil content. The best treatment of basil leaves oleoresin extraction is at ratio of material and solvent 1:6 (w / v) for 6 hours extraction time. In this condition, the yield of basil oleoresin is 20.152%, 0.9688 g/cm3 of density, 1.502 of refractive index, 15.77% of essential oil content, and the colour of oleoresin product is dark-green.

  6. RECOVERY OF METAL VALUES FROM AQUEOUS SOLUTIONS BY SOLVENT EXTRACTION

    DOEpatents

    Moore, R.L.

    1959-09-01

    An organic solvent mixure is described for extracting actinides from aqueous solutions; the solvent mixture consists of from 10 to 25% by volume of tributyl phosphate and the remainder a chlorine-fluorine-substituted saturated hydrocarbon having two carbon atoms in the molecule.

  7. Thermal stability study of a new guanidine suppressor for the next-generation caustic-side solvent extraction process

    DOE PAGES

    Hill, Talon G.; Ensor, Dale D.; Delmau, Lætitia Helene; ...

    2016-02-06

    Cesium stripping performance of thermally stressed solvent degrades slowly over time in batch tests of the Next Generation Caustic-Side Solvent Extraction (NGS) process. NGS is currently used at pilot scale at the Savannah River Site for the selective removal of cesium from high-level salt waste. Recently a new guanidine, N,N',N" -tris(3,7-dimethyloctyl)guanidine (TiDG), was chosen for use as the suppressor, a lipophilic organic base needed for stripping, and the present study was undertaken to address the question of its stability. The NGS process solvent was evaluated for a period of three months under a variety of temperature and storage conditions. Themore » performance of the solvent was tested at 30-day increments using a standard extraction, scrub, strip, and extraction (ES 2S 3E) sequence. Lastly, the results provide insight on the effects of storage and process conditions, the stripping behavior of TiDG, and the stability of the new solvent composition.« less

  8. Thermal stability study of a new guanidine suppressor for the next-generation caustic-side solvent extraction process

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Hill, Talon G.; Ensor, Dale D.; Delmau, Lætitia Helene

    Cesium stripping performance of thermally stressed solvent degrades slowly over time in batch tests of the Next Generation Caustic-Side Solvent Extraction (NGS) process. NGS is currently used at pilot scale at the Savannah River Site for the selective removal of cesium from high-level salt waste. Recently a new guanidine, N,N',N" -tris(3,7-dimethyloctyl)guanidine (TiDG), was chosen for use as the suppressor, a lipophilic organic base needed for stripping, and the present study was undertaken to address the question of its stability. The NGS process solvent was evaluated for a period of three months under a variety of temperature and storage conditions. Themore » performance of the solvent was tested at 30-day increments using a standard extraction, scrub, strip, and extraction (ES 2S 3E) sequence. Lastly, the results provide insight on the effects of storage and process conditions, the stripping behavior of TiDG, and the stability of the new solvent composition.« less

  9. Extraction of three bioactive diterpenoids from Andrographis paniculata: effect of the extraction techniques on extract composition and quantification of three andrographolides using high-performance liquid chromatography.

    PubMed

    Kumar, Satyanshu; Dhanani, Tushar; Shah, Sonal

    2014-10-01

    Andrographis paniculata (Burm.f.) wall.ex Nees (Acanthaceae) or Kalmegh is an important medicinal plant finding uses in many Ayurvedic formulations. Diterpenoid compounds andrographolides (APs) are the main bioactive phytochemicals present in leaves and herbage of A. paniculata. The efficiency of supercritical fluid extraction (SFE) using carbon dioxide was compared with the solid-liquid extraction techniques such as solvent extraction, ultrasound-assisted solvent extraction and microwave-assisted solvent extraction with methanol, water and methanol-water as solvents. Also a rapid and validated reverse-phase high-performance liquid chromatography-diode array detection method was developed for the simultaneous determination of the three biologically active compounds, AP, neoandrographolide and andrograpanin, in the extracts of A. paniculata. Under the best SFE conditions tested for diterpenoids, which involved extraction at 60°C and 100 bar, the extractive efficiencies were 132 and 22 µg/g for AP and neoandrographolide, respectively. The modifier percentage significantly affected the extraction efficiency. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  10. An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides.

    PubMed

    Wang, Ziming; Zhao, Xin; Xu, Xu; Wu, Lijie; Su, Rui; Zhao, Yajing; Jiang, Chengfei; Zhang, Hanqi; Ma, Qiang; Lu, Chunmei; Dong, Deming

    2013-01-14

    A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Two-Stage Separation of V(IV) and Al(III) by Crystallization and Solvent Extraction from Aluminum-Rich Sulfuric Acid Leaching Solution of Stone Coal

    NASA Astrophysics Data System (ADS)

    Shi, Qihua; Zhang, Yimin; Liu, Tao; Huang, Jing; Liu, Hong

    2017-10-01

    To improve separation of V(IV) and Al(III) from aluminum-rich sulfuric acid leaching solution of stone coal, the two-stage separation by crystallization and solvent extraction methods have been developed. A co-extraction coefficient ( k) was put forward to evaluate comprehensively co-extraction extent in different solutions. In the crystallization stage, 68.2% of aluminum can be removed from the solution. In the solvent extraction stage, vanadium was selectively extracted using di-2-ethylhexyl phosphoric acid/tri-n-butyl phosphate from the crystalline mother solution, followed by H2SO4 stripped efficiently. A V2O5 product with purity of 98.39% and only 0.10% Al was obtained after oxidation, precipitation, and calcination. Compared with vanadium extraction from solution without crystallization, the counter-current extraction stage of vanadium can be decreased from 6 to 3 and co-extraction coefficient ( k) decreased from 2.51 to 0.58 with two-stage separation. It is suggested that the aluminum removal by crystallization can evidently weaken the influence of aluminum co-extraction on vanadium extraction and improve the selectivity of solvent extraction for vanadium.

  12. LC-MS determination of steroidal glycosides from Dioscorea deltoidea Wall cell suspension culture: Optimization of pre-LC-MS procedure parameters by Latin Square design.

    PubMed

    Sarvin, Boris; Fedorova, Elizaveta; Shpigun, Oleg; Titova, Maria; Nikitin, Mikhail; Kochkin, Dmitry; Rodin, Igor; Stavrianidi, Andrey

    2018-03-30

    In this paper, the ultrasound assisted extraction method for isolation of steroidal glycosides from D. deltoidea plant cell suspension culture with a subsequent HPLC-MS determination was developed. After the organic solvent was selected via a two-factor experiment the optimization via Latin Square 4 × 4 experimental design was carried out for the following parameters: extraction time, organic solvent concentration in extraction solution and the ratio of solvent to sample. It was also shown that the ultrasound assisted extraction method is not suitable for isolation of steroidal glycosides from the D. deltoidea plant material. The results were double-checked using the multiple successive extraction method and refluxing extraction. Optimal conditions for the extraction of steroidal glycosides by the ultrasound assisted extraction method were: extraction time, 60 min; acetonitrile (water) concentration in extraction solution, 50%; the ratio of solvent to sample, 400 mL/g. Also, the developed method was tested on D. deltoidea cell suspension cultures of different terms and conditions of cultivation. The completeness of the extraction was confirmed using the multiple successive extraction method. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Complex investigation of extraction techniques applied for cyclitols and sugars isolation from different species of Solidago genus.

    PubMed

    Ratiu, Ileana-Andreea; Al-Suod, Hossam; Ligor, Magdalena; Ligor, Tomasz; Railean-Plugaru, Viorica; Buszewski, Bogusław

    2018-03-15

    Cyclitols are phytochemicals naturally occurring in plant material, which attracted an increasing interest due to multiple medicinal attributes, among which the most important are the antidiabetic, antioxidant, and anticancer properties. Due to their valuable properties, sugars are used in the food industry as sweeteners, preservatives, texture modifiers, fermentation substrates, and flavoring and coloring agents. In this study, we report for the first time the quantitative analysis of sugars and cyclitols isolated from Solidago virgaurea L., which was used for the selection of the optimal solvent and extraction technique that can provide the best possible yield. Moreover, the quantities of sugars and cyclitols extracted from two other species, Solidago canadensis and Solidago gigantea, were investigated using the best extraction method and the most appropriate solvent. Comparative analysis of natural plant extracts obtained using five different techniques-maceration, Soxhlet extraction, pressurized liquid extraction, ultrasound-assisted extraction, and supercritical fluid extraction-was performed in order to decide the most suitable, efficient, and economically convenient extraction method. Three different solvents were used. Analysis of samples has been performed by solid-phase extraction for purification and pre-concentration, followed by derivation and GC-MS analysis. Highest efficiency for the total amount of obtained compounds has been reached by PLE, when water was used as a solvent. d-pinitol amount was almost similar for every solvent and for all the extraction techniques involved. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Enhanced and green extraction polyphenols and furanocoumarins from Fig (Ficus carica L.) leaves using deep eutectic solvents.

    PubMed

    Wang, Tong; Jiao, Jiao; Gai, Qing-Yan; Wang, Peng; Guo, Na; Niu, Li-Li; Fu, Yu-Jie

    2017-10-25

    Nowadays, green extraction of bioactive compounds from medicinal plants has gained increasing attention. As green solvent, deep eutectic solvent (DES) have been highly rated to replace toxic organic solvents in extraction process. In present study, to simultaneous extraction five main bioactive compounds from fig leaves, DES was tailor-made. The tailor-made DES composed of a 3:3:3 molar ratio of glycerol, xylitol and D-(-)-Fructose showed enhanced extraction yields for five target compounds simultaneously compared with traditional methanol and non-tailor DESs. Then, the tailor-made DES based extraction methods have compared and microwave-assisted extraction was selected and optimized due to its high extraction yields with lower time consumption. The influencing parameters including extraction temperature, liquid-solid ratio, and extraction time were optimized using response surface methodology (RSM). Under optimal conditions the extraction yield of caffeoylmalic acid, psoralic acid-glucoside, rutin, psoralen and bergapten was 6.482mg/g, 16.34mg/g, 5.207mg/g, 15.22mg/g and 2.475mg/g, respectively. Macroporous resin D101 has been used to recovery target compounds with recovery yields of 79.2%, 83.4%, 85.5%, 81.2% and 75.3% for caffeoylmalic acid, psoralic acid-glucoside, rutin, psoralen and bergapten, respectively. The present study suggests that DESs are truly designer and efficient solvents and the method we developed was efficient and sustainable for extraction main compounds from Fig leaves.mg/g. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Green procedure with a green solvent for fats and oils' determination. Microwave-integrated Soxhlet using limonene followed by microwave Clevenger distillation.

    PubMed

    Virot, Matthieu; Tomao, Valérie; Ginies, Christian; Visinoni, Franco; Chemat, Farid

    2008-07-04

    Here is described a green and original alternative procedure for fats and oils' determination in oleaginous seeds. Extractions were carried out using a by-product of the citrus industry as extraction solvent, namely d-limonene, instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using microwave energy: at first, extractions are attained using microwave-integrated Soxhlet, followed by the elimination of the solvent from the medium using a microwave Clevenger distillation in the second step. Oils extracted from olive seeds were compared with both conventional Soxhlet and microwave-integrated Soxhlet extraction procedures performed with n-hexane in terms of qualitative and quantitative determination. No significant difference was obtained between each extract allowing us to conclude that the proposed method is effective and valuable.

  16. Comparison of microwave hydrodistillation and solvent-free microwave extraction of essential oil from Melaleuca leucadendra Linn

    NASA Astrophysics Data System (ADS)

    Ismanto, A. W.; Kusuma, H. S.; Mahfud, M.

    2017-12-01

    The comparison of solvent-free microwave extraction (SFME) and microwave hydrodistillation (MHD) in the extraction of essential oil from Melaleuca leucadendra Linn. was examined. Dry cajuput leaves were used in this study. The purpose of this study is also to determine optimal condition (microwave power). The relative electric consumption of SFME and MHD methods are both showing 0,1627 kWh/g and 0,3279 kWh/g. The results showed that solvent-free microwave extraction methods able to reduce energy consumption and can be regarded as a green technique for extraction of cajuput oil.

  17. Process analysis and modeling of a single-step lutein extraction method for wet microalgae.

    PubMed

    Gong, Mengyue; Wang, Yuruihan; Bassi, Amarjeet

    2017-11-01

    Lutein is a commercial carotenoid with potential health benefits. Microalgae are alternative sources for the lutein production in comparison to conventional approaches using marigold flowers. In this study, a process analysis of a single-step simultaneous extraction, saponification, and primary purification process for free lutein production from wet microalgae biomass was carried out. The feasibility of binary solvent mixtures for wet biomass extraction was successfully demonstrated, and the extraction kinetics of lutein from chloroplast in microalgae were first evaluated. The effects of types of organic solvent, solvent polarity, cell disruption method, and alkali and solvent usage on lutein yields were examined. A mathematical model based on Fick's second law of diffusion was applied to model the experimental data. The mass transfer coefficients were used to estimate the extraction rates. The extraction rate was found more significantly related with alkali ratio to solvent than to biomass. The best conditions for extraction efficiency were found to be pre-treatment with ultrasonication at 0.5 s working cycle per second, react 0.5 h in 0.27 L/g solvent to biomass ratio, and 1:3 ether/ethanol (v/v) with 1.25 g KOH/L. The entire process can be controlled within 1 h and yield over 8 mg/g lutein, which is more economical for scale-up.

  18. Accelerated solvent extraction combined with dispersive liquid-liquid microextraction before gas chromatography with mass spectrometry for the sensitive determination of phenols in soil samples.

    PubMed

    Xing, Han-Zhu; Wang, Xia; Chen, Xiang-Feng; Wang, Ming-Lin; Zhao, Ru-Song

    2015-05-01

    A method combining accelerated solvent extraction with dispersive liquid-liquid microextraction was developed for the first time as a sample pretreatment for the rapid analysis of phenols (including phenol, m-cresol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) in soil samples. In the accelerated solvent extraction procedure, water was used as an extraction solvent, and phenols were extracted from soil samples into water. The dispersive liquid-liquid microextraction technique was then performed on the obtained aqueous solution. Important accelerated solvent extraction and dispersive liquid-liquid microextraction parameters were investigated and optimized. Under optimized conditions, the new method provided wide linearity (6.1-3080 ng/g), low limits of detection (0.06-1.83 ng/g), and excellent reproducibility (<10%) for phenols. Four real soil samples were analyzed by the proposed method to assess its applicability. Experimental results showed that the soil samples were free of our target compounds, and average recoveries were in the range of 87.9-110%. These findings indicate that accelerated solvent extraction with dispersive liquid-liquid microextraction as a sample pretreatment procedure coupled with gas chromatography and mass spectrometry is an excellent method for the rapid analysis of trace levels of phenols in environmental soil samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Application of natural deep eutectic solvents to the extraction of anthocyanins from Catharanthus roseus with high extractability and stability replacing conventional organic solvents.

    PubMed

    Dai, Yuntao; Rozema, Evelien; Verpoorte, Robert; Choi, Young Hae

    2016-02-19

    Natural deep eutectic solvents (NADES) have attracted a great deal of attention in recent times as promising green media. They are generally composed of neutral, acidic or basic compounds that form liquids of high viscosity when mixed in certain molar ratio. Despite their potential, viscosity and acid or basic nature of some ingredients may affect the extraction capacity and stabilizing ability of the target compounds. To investigate these effects, extraction with a series of NADES was employed for the analysis of anthocyanins in flower petals of Catharanthus roseus in combination with HPLC-DAD-based metabolic profiling. Along with the extraction yields of anthocyanins their stability in NADES was also studied. Multivariate data analysis indicates that the lactic acid-glucose (LGH), and 1,2-propanediol-choline chloride (PCH) NADES present a similar extraction power for anthocyanins as conventional organic solvents. Furthermore, among the NADES employed, LGH exhibits an at least three times higher stabilizing capacity for cyanidins than acidified ethanol, which facilitates their extraction and analysis process. Comparing NADES to the conventional organic solvents, in addition to their reduced environmental impact, they proved to provide higher stability for anthocyanins, and therefore have a great potential as possible alternatives to those organic solvents in health related areas such as food, pharmaceuticals and cosmetics. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Investigation of aggregation in solvent extraction of lanthanides by acidic extractants (organophosphorus and naphthenic acid)

    USGS Publications Warehouse

    Zhou, N.; Wu, J.; Yu, Z.; Neuman, R.D.; Wang, D.; Xu, G.

    1997-01-01

    Three acidic extractants (I) di(2-ethylhexyl) phosphoric acid (HDEHP), (II) 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (HEHPEHE) and (III) naphthenic acid were employed in preparing the samples for the characterization of the coordination structure of lanthanide-extractant complexes and the physicochemical nature of aggregates formed in the organic diluent of the solvent extraction systems. Photo correlation spectroscopy (PCS) results on the aggregates formed by the partially saponified HDEHP in n-heptane showed that the hydrodynamic radius of the aggregates was comparable to the molecular dimensions of HDEHP. The addition of 2-octanol into the diluent, by which the mixed solvent was formed, increased the dimensions of the corresponding aggregates. Aggregates formed from the lanthanide ions and HDEHP in the organic phase of the extraction systems were found very unstable. In the case of naphthenic acid, PCS data showed the formation of w/o microemulsion from the saponified naphthenic acid in the mixed solvent. The extraction of lanthanides by the saponified naphthenic acid in the mixed solvent under the given experimental conditions was a process of destruction of the w/o microemulsion. A possible mechanism of the breakdown of the w/o microemulsion droplets is discussed.

  1. Modified extraction procedure for gas-liquid chromatography applied to the identification of anaerobic bacteria.

    PubMed Central

    Thomann, W R; Hill, G B

    1986-01-01

    Chloroform and ether commonly are used as solvents to extract metabolic organic acids for analysis by gas-liquid chromatography in the identification of anaerobic bacteria. Because these solvents are potentially hazardous to personnel, modified extraction procedures involving the use of a safer solvent, methyl tert-butyl ether were developed which remained both simple to perform and effective for organism identification. PMID:3700623

  2. SOLVENT EXTRACTION OF RUTHENIUM

    DOEpatents

    Hyman, H.H.; Leader, G.R.

    1959-07-14

    The separation of rathenium from aqueous solutions by solvent extraction is described. According to the invention, a nitrite selected from the group consisting of alkali nitrite and alkaline earth nitrite in an equimolecular quantity with regard to the quantity of rathenium present is added to an aqueous solution containing ruthenium tetrantrate to form a ruthenium complex. Adding an organic solvent such as ethyl ether to the resulting mixture selectively extracts the rathenium complex.

  3. Comparison of microwave, ultrasound and accelerated-assisted solvent extraction for recovery of polyphenols from Citrus sinensis peels.

    PubMed

    Nayak, Balunkeswar; Dahmoune, Farid; Moussi, Kamal; Remini, Hocine; Dairi, Sofiane; Aoun, Omar; Khodir, Madani

    2015-11-15

    Peel of Citrus sinensis contains significant amounts of bioactive polyphenols that could be used as ingredients for a number of value-added products with health benefits. Extraction of polyphenols from the peels was performed using a microwave-assisted extraction (MAE) technique. The effects of aqueous acetone concentration, microwave power, extraction time and solvent-to-solid ratio on the total phenolic content (TPC), total antioxidant activity (TAA) (using DPPH and ORAC-values) and individual phenolic acids (IPA) were investigated using a response surface method. The TPC, TAA and IPA of peel extracts using MAE was compared with conventional, ultrasound-assisted and accelerated solvent extraction. The maximum predicted TPC under the optimal MAE conditions (51% acetone concentration in water (v/v), 500 W microwave power, 122 s extraction time and 25 mL g(-1) solvent to solid ratio), was 12.20 mg GAE g(-1) DW. The TPC and TAA in MAE extracts were higher than the other three extracts. Copyright © 2015 Elsevier Ltd. All rights reserved.

  4. The influence of purge times on the yields of essential oil components extracted from plants by pressurized liquid extraction.

    PubMed

    Wianowska, Dorota

    2014-01-01

    The influence of different purge times on the yield of the main essential oil constituents of rosemary (Rosmarinus officinalis L.), thyme (Thymus vulgaris L.), and chamomile (Chamomilla recutita L.) was investigated. The pressurized liquid extraction process was performed by applying different extraction temperatures and solvents. The results presented in the paper show that the estimated yield of essential oil components extracted from the plants in the pressurized liquid extraction process is purge time-dependent. The differences in the estimated yields are mainly connected with the evaporation of individual essential oil components and the applied solvent during the purge; the more volatile an essential oil constituent is, the greater is its loss during purge time, and the faster the evaporation of the solvent during the purge process is, the higher the concentration of less volatile essential oil components in the pressurized liquid extraction receptacle. The effect of purge time on the estimated yield of individual essential oil constituents is additionally differentiated by the extraction temperature and the extraction ability of the applied solvent.

  5. Interdisciplinary Chemistry Experiment: An Environmentally Friendly Extraction of Lycopene

    ERIC Educational Resources Information Center

    Zhu, Jie; Zhang, Mingjie; Liu, Qingwei

    2008-01-01

    A novel experiment for the extraction of lycopene from tomato paste without the use of an organic solvent is described. The experiment employs polymer, green, and analytical chemistry. This environmentally friendly extraction is more efficient and requires less time than the traditional approach using an organic solvent. The extraction is…

  6. Multiple Solvent Extraction System with Flow Injection Technology.

    DTIC Science & Technology

    1981-09-30

    encounters a back extraction step where the direction of the extraction is from organic to aqueous solvent. Thus it is advantageous to incorporate both...stainless steel ( Alltech Associates, Arlington Heights, IQ) and prepared from a single section of 180 cmn in length. The Section 2 mixing and extraction

  7. A green analytical chemistry approach for lipid extraction: computation methods in the selection of green solvents as alternative to hexane.

    PubMed

    Cascant, Mari Merce; Breil, Cassandra; Garrigues, Salvador; de la Guardia, Miguel; Fabiano-Tixier, Anne Silvie; Chemat, Farid

    2017-05-01

    There is a great interest in finding alternatives and green solvents in extraction processes to replace petroleum based solvents. In order to investigate these possibilities, computational methods, as Hansen solubility parameters (HSP) and conductor-like screening model for real solvent (COSMO-RS), were used in this work to predict the solvation power of a series of solvents in salmon fish lipids. Additionally, experimental studies were used to evaluate the performance in lipids extraction using 2-methyltetrahydrofurane, cyclopentyl methyl ether, dimethyl carbonate, isopropanol, ethanol, ethyl acetate, p-cymene and d-limonene compared with hexane. Lipid classes of extracts were obtained by using high performance thin-layer chromatography (HPTLC), whereas gas chromatography with a flame ionization detector (GC/FID) technique was employed to obtain fatty acid profiles. Some differences between theoretical and experimental results were observed, especially regarding the behavior of p-cymene and d-limonene, which separate from the predicted capability. Results obtained from HPTLC indicated that p-cymene and d-limonene extract triglycerides (TAGs) and diglycerides (DAGs) at levels of 73 and 19%, respectively, whereas the other studied extracts contain between 75 and 76% of TAGs and between 16 and 17% of DAGs. Fatty acid profiles, obtained by using GC-FID, indicated that saturated fatty acids (SFAs) between 19.5 and 19.9% of extracted oil, monounsaturated fatty acids (MUFAs) in the range between 43.5 and 44.9%, and PUFAs between 31.2 and 34.6% were extracted. p-Cymene and limonene extracts contained lower percentages than the other studied solvents of some PUFAs due probably to the fact that these unsaturated fatty acids are more susceptible to oxidative degradation than MUFAs. Ethyl acetate has been found to be the best alternative solvent to hexane for the extraction of salmon oil lipids. Graphical Abstract ᅟ.

  8. Systematic assessment of different solvents for the extraction of drugs of abuse and pharmaceuticals from an authentic hair pool.

    PubMed

    Madry, Milena M; Kraemer, Thomas; Baumgartner, Markus R

    2018-01-01

    Hair analysis has been established as a prevalent tool for retrospective drug monitoring. In this study, different extraction solvents for the determination of drugs of abuse and pharmaceuticals in hair were evaluated for their efficiency. A pool of authentic hair from drug users was used for extraction experiments. Hair was pulverized and extracted in triplicate with seven different solvents in a one- or two-step extraction. Three one- (methanol, acetonitrile, and acetonitrile/water) and four two-step extractions (methanol two-fold, methanol and methanol/acetonitrile/formate buffer, methanol and methanol/formate buffer, and methanol and methanol/hydrochloric acid) were tested under accurately equal experimental conditions. The extracts were directly analyzed by liquid chromatography-tandem mass spectrometry for opiates/opioids, stimulants, ketamine, selected benzodiazepines, antidepressants, antipsychotics, and antihistamines using deuterated internal standards. For most analytes, a two-step extraction with methanol did not significantly improve the yield compared to a one-step extraction with methanol. Extraction with acetonitrile alone was least efficient for most analytes. Extraction yields of acetonitrile/water, methanol and methanol/acetonitrile/formate buffer, and methanol and methanol/formate buffer were significantly higher compared to methanol. Highest efficiencies were obtained by a two-step extraction with methanol and methanol/hydrochloric acid, particularly for morphine, 6-monoacetylmorphine, codeine, 6-acetylcodeine, MDMA, zopiclone, zolpidem, amitriptyline, nortriptyline, citalopram, and doxylamine. For some analytes (e.g., tramadol, fluoxetine, sertraline), all extraction solvents, except for acetonitrile, were comparably efficient. There was no significant correlation between extraction efficiency with an acidic solvent and the pka or log P of the analyte. However, there was a significant trend for the extraction efficiency with acetonitrile to the log P of the analyte. The study demonstrates that the choice of extraction solvent has a strong impact on hair analysis outcomes. Therefore, validation protocols should include the evaluation of extraction efficiency of drugs by using authentic rather than spiked hair. Different extraction procedures may contribute to the scatter of quantitative results in inter-laboratory comparisons. Harmonization of extraction protocols is recommended, when interpretation is based on same cut-off levels. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. A high-throughput platform for low-volume high-temperature/pressure sealed vessel solvent extractions.

    PubMed

    Damm, Markus; Kappe, C Oliver

    2011-11-30

    A high-throughput platform for performing parallel solvent extractions in sealed HPLC/GC vials inside a microwave reactor is described. The system consist of a strongly microwave-absorbing silicon carbide plate with 20 cylindrical wells of appropriate dimensions to be fitted with standard HPLC/GC autosampler vials serving as extraction vessels. Due to the possibility of heating up to four heating platforms simultaneously (80 vials), efficient parallel analytical-scale solvent extractions can be performed using volumes of 0.5-1.5 mL at a maximum temperature/pressure limit of 200°C/20 bar. Since the extraction and subsequent analysis by either gas chromatography or liquid chromatography coupled with mass detection (GC-MS or LC-MS) is performed directly from the autosampler vial, errors caused by sample transfer can be minimized. The platform was evaluated for the extraction and quantification of caffeine from commercial coffee powders assessing different solvent types, extraction temperatures and times. For example, 141±11 μg caffeine (5 mg coffee powder) were extracted during a single extraction cycle using methanol as extraction solvent, whereas only 90±11 were obtained performing the extraction in methylene chloride, applying the same reaction conditions (90°C, 10 min). In multiple extraction experiments a total of ~150 μg caffeine was extracted from 5 mg commercial coffee powder. In addition to the quantitative caffeine determination, a comparative qualitative analysis of the liquid phase coffee extracts and the headspace volatiles was performed, placing special emphasis on headspace analysis using solid-phase microextraction (SPME) techniques. The miniaturized parallel extraction technique introduced herein allows solvent extractions to be performed at significantly expanded temperature/pressure limits and shortened extraction times, using standard HPLC autosampler vials as reaction vessels. Remarkable differences regarding peak pattern and main peaks were observed when low-temperature extraction (60°C) and high-temperature extraction (160°C) are compared prior to headspace-SPME-GC-MS performed in the same HPLC/GC vials. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Production and recovery of Americium-241

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Navratil, J.D.

    1984-01-01

    Americium-241, one of the most useful actinide isotopes, is produced as a by-product of plutonium scrap recovery operations. Rocky Flats (RF) has supplied high-purity americium oxide to the US Department of Energy's Isotope Pool since 1962. Over the years, the evolving separation and purification processes have included such diverse operations as aqueous precipitation, ion exchange, and both molten-salt and organic-solvent extraction. A review is presented of the production and recovery processes of americium-241. 5 references.

  11. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Lorenz, Matthias; Ovchinnikova, Olga S; Van Berkel, Gary J

    RATIONALE: Laser ablation provides for the possibility of sampling a large variety of surfaces with high spatial resolution. This type of sampling when employed in conjunction with liquid capture followed by nanoelectrospray ionization provides the opportunity for sensitive and prolonged interrogation of samples by mass spectrometry as well as the ability to analyze surfaces not amenable to direct liquid extraction. METHODS: A fully automated, reflection geometry, laser ablation liquid capture spot sampling system was achieved by incorporating appropriate laser fiber optics and a focusing lens into a commercially available, liquid extraction surface analysis (LESA ) ready Advion TriVersa NanoMate system.more » RESULTS: Under optimized conditions about 10% of laser ablated material could be captured in a droplet positioned vertically over the ablation region using the NanoMate robot controlled pipette. The sampling spot size area with this laser ablation liquid capture surface analysis (LA/LCSA) mode of operation (typically about 120 m x 160 m) was approximately 50 times smaller than that achievable by direct liquid extraction using LESA (ca. 1 mm diameter liquid extraction spot). The set-up was successfully applied for the analysis of ink on glass and paper as well as the endogenous components in Alstroemeria Yellow King flower petals. In a second mode of operation with a comparable sampling spot size, termed laser ablation/LESA , the laser system was used to drill through, penetrate, or otherwise expose material beneath a solvent resistant surface. Once drilled, LESA was effective in sampling soluble material exposed at that location on the surface. CONCLUSIONS: Incorporating the capability for different laser ablation liquid capture spot sampling modes of operation into a LESA ready Advion TriVersa NanoMate enhanced the spot sampling spatial resolution of this device and broadened the surface types amenable to analysis to include absorbent and solvent resistant materials.« less

  12. Microwave-assisted extraction of total bioactive saponin fraction from Gymnema sylvestre with reference to gymnemagenin: a potential biomarker.

    PubMed

    Mandal, Vivekananda; Dewanjee, Saikat; Mandal, Subhash C

    2009-01-01

    To develop a fast and ecofriendly microwave assisted extraction (MAE) technique for the effective and exhaustive extraction of gymnemagenin as an indicative biomarker for the quality control of Gymnema sylvestre. Several extraction parameters such as microwave power, extraction time, solvent composition, pre-leaching time, loading ratio and extraction cycle were studied for the determination of the optimum extraction condition. Scanning electron micrographs were obtained to elucidate the mechanism of extraction. The final optimum extraction conditions as obtained from the study were: 40% microwave power, 6 min irradiation time, 85% v/v methanol as the extraction solvent, 15 min pre-leaching time and 25 : 1 (mL/g) as the solvent-to-material loading ratio. The proposed extraction technique produced a maximum yield of 4.3% w/w gymnemagenin in 6 min which was 1.3, 2.5 and 1.95 times more efficient than 6 h of heat reflux, 24 h of maceration and stirring extraction, respectively. A synergistic heat and mass transfer theory was also proposed to support the extraction mechanism. Comparison with conventional extraction methods revealed that MAE could save considerable amounts of time and energy, whilst the reduction of volume of organic solvent consumed provides an ecofriendly feature.

  13. Extraction of Trivalent Actinides and Lanthanides from Californium Campaign Rework Solution Using TODGA-based Solvent Extraction System

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Benker, Dennis; Delmau, Laetitia Helene; Dryman, Joshua Cory

    This report presents the studies carried out to demonstrate the possibility of quantitatively extracting trivalent actinides and lanthanides from highly acidic solutions using a neutral ligand-based solvent extraction system. These studies stemmed from the perceived advantage of such systems over cationexchange- based solvent extraction systems that require an extensive feed adjustment to make a low-acid feed. The targeted feed solutions are highly acidic aqueous phases obtained after the dissolution of curium targets during a californium (Cf) campaign. Results obtained with actual Cf campaign solutions, but highly diluted to be manageable in a glove box, are presented, followed by results ofmore » tests run in the hot cells with Cf campaign rework solutions. It was demonstrated that a solvent extraction system based on the tetraoctyl diglycolamide molecule is capable of quantitatively extracting trivalent actinides from highly acidic solutions. This system was validated using actual feeds from a Cf campaign.« less

  14. Optimization by response surface methodology of lutein recovery from paprika leaves using accelerated solvent extraction.

    PubMed

    Kang, Jae-Hyun; Kim, Suna; Moon, BoKyung

    2016-08-15

    In this study, we used response surface methodology (RSM) to optimize the extraction conditions for recovering lutein from paprika leaves using accelerated solvent extraction (ASE). The lutein content was quantitatively analyzed using a UPLC equipped with a BEH C18 column. A central composite design (CCD) was employed for experimental design to obtain the optimized combination of extraction temperature (°C), static time (min), and solvent (EtOH, %). The experimental data obtained from a twenty sample set were fitted to a second-order polynomial equation using multiple regression analysis. The adjusted coefficient of determination (R(2)) for the lutein extraction model was 0.9518, and the probability value (p=0.0000) demonstrated a high significance for the regression model. The optimum extraction conditions for lutein were temperature: 93.26°C, static time: 5 min, and solvent: 79.63% EtOH. Under these conditions, the predicted extraction yield of lutein was 232.60 μg/g. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Ultrasound-Assisted Extraction of Stilbenes from Grape Canes.

    PubMed

    Piñeiro, Zulema; Marrufo-Curtido, Almudena; Serrano, Maria Jose; Palma, Miguel

    2016-06-16

    An analytical ultrasound-assisted extraction (UAE) method has been optimized and validated for the rapid extraction of stilbenes from grape canes. The influence of sample pre-treatment (oven or freeze-drying) and several extraction variables (solvent, sample-solvent ratio and extraction time between others) on the extraction process were analyzed. The new method allowed the main stilbenes in grape canes to be extracted in just 10 min, with an extraction temperature of 75 °C and 60% ethanol in water as the extraction solvent. Validation of the extraction method was based on analytical properties. The resulting RSDs (n = 5) for interday/intraday precision were less than 10%. Furthermore, the method was successfully applied in the analysis of 20 different grape cane samples. The result showed that grape cane byproducts are potentially sources of bioactive compounds of interest for pharmaceutical and food industries.

  16. Experiment on the treatment of waste extraction solvent from the molybdenum-99 process

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Hsien-Ming Hsiao; Chang-Liang Hu; Kuang-Li Chien

    2013-07-01

    In the Mo-99 (Molybdenum-99) isotope extraction test process for radiopharmaceutical applications, organic solvent is used to extract Mo-99 from an irradiated UO{sub 2} dissolution. The extraction solvent was stored when the test work was stopped. A total of about 120 liters of waste solvent was stored at INER (Institute of Nuclear Energy Research, Taiwan). The extraction solvent consisted of 5% di-(2-ethylhexyl)-phosphoric acid (D2EHPA) and kerosene. The radionuclides found in the waste solvent include Cs-137, Am-241, Tc-99, and Sr-90, which give off gross alpha and beta radioactivity of 1898 and 471 Bq/ml, respectively. This study aims to remove radionuclides from themore » waste solvent using sodium carbonate and sodium hydroxide solutions in different concentrations. After mixing the waste solvent with the alkaline solution followed by settling, a third phase other than organic and aqueous phase appeared which is expected due to the saponification reaction. The experimental results showed that increasing the number of washing and the alkaline solution concentration could enhance the radionuclides removal rate. An optimal removal method was proposed using 2 M Na{sub 2}CO{sub 3} solution twice followed by 1 M NaOH solution one time for the third phase generated early in the mixing stages. The remaining gross alpha and beta radioactivity of the treated organic solvent was 2 and 3 Bq/ml, respectively. The treated solvent could be stabilized by ashing at 500 deg. C and then immobilized. The alkaline solution would be neutralized by hydrochloric or nitric acid and then treated using a variety of adsorbents or bone char via adsorption to remove nuclides to meet the wastewater discharge limitation. (authors)« less

  17. Changes in total phenol, flavonoid contents and anti-Lactobacillus activity of Callisia fragrans due to extraction solvent

    NASA Astrophysics Data System (ADS)

    Le, Thom; Cao, Diem Kieu; Pham, Thanh Vy; Huynh, Tan Dat; Ta, Nhat Thuy Anh; Nguyen, Ngoc Thao Linh; Nguyen, Huu Thanh; Le, Hue Huong; Bui, Anh Vo; Truong, Dieu-Hien

    2018-04-01

    Callisia fragrans is a wonder herb with many medicinal properties such as burn, dental diseases, cancer diseases and arthritis in folk medicine. It is noted that the phytochemical constituents and antimicrobial activity of traditional plants depend on not only the extracting method but also the solvent used for extraction. In this study, the effect of five extraction solvents (i.e., distilled water, 80% methanol, 80% ethanol, 80% ethyl acetate, and 80% chloroform) on yield, total phenolic content (TPC) and total flavonoid content (TFC) of Callisia leaves was determined. Besides, changes in anti-Lactobacillus fermentum activity of C. fragrans freeze-dried extract was also evaluated using disk-diffusion method. The recovery percentage of extractable yield of fresh leaves are ranged from 11.93% w/w for distilled water extract to 16.60% w/w for aqueous ethanol extracts. The yield of 80% aqueous methanol extract (16.27% w/w) is only slightly less than that of the ethanol extract. Significant differences were observed among TPC and TFC obtaining by 80% methanol (0.0522% and 0.0335% w/w, respectively) compared to other solvents (p < 0.05). TPC and TFC of C. fragrans extracts increase in the following order: distilled water < 80% chloroform < 80% ethyl acetate < 80% ethanol < 80% methanol. The results revealed that 80% aqueous methanol Calissia extracts has moderate inhibition (9.0 mm of inhibition zone for 1.5 mg/mL of extracts) of L. fermentum compared to standard antibacterial agent. Based on the study results, it can be concluded that the yield, TPC and TFC of C. frgrans extract varied with the extracting solvent. It also showed that Callisia extracts can prevent dental caries by inhibiting the growth of L. fermentum, towards new insights for treatment of dental caries.

  18. Assessment of Multiple Solvents for Extraction and Direct GC-MS Determination of the Phytochemical Inventory of Sansevieria Extrafoliar Nectar Droplets.

    PubMed

    Gaylor, Michael O; Juntunen, Hope L; Hazelwood, Donna; Videau, Patrick

    2018-04-01

    Considerable effort has been devoted to analytical determinations of sugar and amino acid constituents of plant nectars, with the primary aim of understanding their ecological roles, yet few studies have reported more exhaustive organic compound inventories of plant nectars or extrafoliar nectars. This work evaluated the efficacy of four solvents (ethyl acetate, dichloromethane, toluene and hexane) to extract the greatest number of organic compound classes and unique compounds from extrafoliar nectar drops produced by Sansevieria spp. Aggregation of the results from each solvent revealed that 240 unique compounds were extracted in total, with 42.5% of those detected in multiple extracts. Aliphatic hydrocarbons dominated in all but the ethyl acetate extracts, with 44 unique aliphatic hydrocarbons detected in dichloromethane (DCM) extracts, followed by 41, 19 and 8 in hexane, toluene and ethyl acetate extracts, respectively. Hexane extracted the most unique compounds (79), followed by DCM (73), ethyl acetate (56) and toluene (32). Integrated total ion chromatographic peak areas of extracted compound classes were positively correlated with numbers of unique compounds detected within those classes. In addition to demonstrating that multi-solvent extraction with direct GC-MS detection is a suitable analytical approach for determining secondary nectar constituents, to the best of our knowledge, this study also represents: (i) the first attempt to inventory the secondary phytochemical constituents of Sansevieria spp. extrafoliar nectar secretions and (ii) the largest organic solvent extractable compound inventory reported for any plant matrix to date.

  19. Solvent for the simultaneous recovery of radionuclides from liquid radioactive wastes

    DOEpatents

    Romanovskiy, Valeriy Nicholiavich; Smirnov, Igor V.; Babain, Vasiliy A.; Todd, Terry A.; Brewer, Ken N.

    2002-01-01

    The present invention relates to solvents, and methods, for selectively extracting and recovering radionuclides, especially cesium and strontium, rare earths and actinides from liquid radioactive wastes. More specifically, the invention relates to extracting agent solvent compositions comprising complex organoboron compounds, substituted polyethylene glycols, and neutral organophosphorus compounds in a diluent. The preferred solvent comprises a chlorinated cobalt dicarbollide, diphenyl-dibutylmethylenecarbamoylphosphine oxide, PEG-400, and a diluent of phenylpolyfluoroalkyl sulfone. The invention also provides a method of using the invention extracting agents to recover cesium, strontium, rare earths and actinides from liquid radioactive waste.

  20. Method for the simultaneous recovery of radionuclides from liquid radioactive wastes using a solvent

    DOEpatents

    Romanovskiy, Valeriy Nicholiavich; Smirnov, Igor V.; Babain, Vasiliy A.; Todd, Terry A.; Brewer, Ken N.

    2001-01-01

    The present invention relates to solvents, and methods, for selectively extracting and recovering radionuclides, especially cesium and strontium, rare earths and actinides from liquid radioactive wastes. More specifically, the invention relates to extracting agent solvent compositions comprising complex organoboron compounds, substituted polyethylene glycols, and neutral organophosphorus compounds in a diluent. The preferred solvent comprises a chlorinated cobalt dicarbollide, diphenyl-dibutylmethylenecarbamoylphosphine oxide, PEG-400, and a diluent of phenylpolyfluoroalkyl sulfone. The invention also provides a method of using the invention extracting agents to recover cesium, strontium, rare earths and actinides from liquid radioactive waste.

  1. Antifungal activity of extracts from Piper aduncum leaves prepared by different solvents and extraction techniques against dermatophytes Trichophyton rubrum and Trichophyton interdigitale.

    PubMed

    Santos, Maximillan Leite; Magalhães, Chaiana Froés; da Rosa, Marcelo Barcellos; de Assis Santos, Daniel; Brasileiro, Beatriz Gonçalves; de Carvalho, Leandro Machado; da Silva, Marcelo Barreto; Zani, Carlos Leomar; de Siqueira, Ezequias Pessoa; Peres, Rodrigo Loreto; Andrade, Anderson Assunção

    2013-12-01

    The effects of different solvents and extraction techniques upon the phytochemical profile and anti-Trichophyton activity of extracts from Piper aduncum leaves were evaluated. Extract done by maceration method with ethanol has higher content of sesquiterpenes and antifungal activity. This extract may be useful as an alternative treatment for dermatophytosis.

  2. Antifungal activity of extracts from Piper aduncum leaves prepared by different solvents and extraction techniques against dermatophytes Trichophyton rubrum and Trichophyton interdigitale

    PubMed Central

    Santos, Maximillan Leite; Magalhães, Chaiana Froés; da Rosa, Marcelo Barcellos; de Assis Santos, Daniel; Brasileiro, Beatriz Gonçalves; de Carvalho, Leandro Machado; da Silva, Marcelo Barreto; Zani, Carlos Leomar; de Siqueira, Ezequias Pessoa; Peres, Rodrigo Loreto; Andrade, Anderson Assunção

    2013-01-01

    The effects of different solvents and extraction techniques upon the phytochemical profile and anti-Trichophyton activity of extracts from Piper aduncum leaves were evaluated. Extract done by maceration method with ethanol has higher content of sesquiterpenes and antifungal activity. This extract may be useful as an alternative treatment for dermatophytosis. PMID:24688522

  3. Principles of Stagewise Separation Process Calculations: A Simple Algebraic Approach Using Solvent Extraction.

    ERIC Educational Resources Information Center

    Crittenden, Barry D.

    1991-01-01

    A simple liquid-liquid equilibrium (LLE) system involving a constant partition coefficient based on solute ratios is used to develop an algebraic understanding of multistage contacting in a first-year separation processes course. This algebraic approach to the LLE system is shown to be operable for the introduction of graphical techniques…

  4. NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR ANALYSIS OF VOLATILE ORGANIC COMPOUNDS COLLECTED WITH A PASSIVE SAMPLER (BCO-L-17.1)

    EPA Science Inventory

    The purpose of this SOP is to describe the methodology used for the analysis of the 3M OVM 3500 Organic Vapor Monitors for volatile organic compounds (VOCs), using solvent extraction and standard gas chromatography/mass spectrometry (GC/MS) analysis procedures. This procedure was...

  5. Microwave-assisted extraction of polycyclic aromatic compounds from coal.

    PubMed

    Kerst, M; Andersson, J T

    2001-08-01

    Microwave-assisted extraction (MAE) of polycyclic aromatic compounds (PACs) from coal is shown to give the same pattern of compounds as Soxhlet extraction. MAE requires only 10 mL solvent and 10 min extraction time whereas Soxhlet uses 200 mL and takes 24 h. Although the yields were lower, dichloromethane (DCM) was preferred to pyridine, N-methyl-2-pyrrolidone (NMP), and NMP with CS2 because the pattern of the PACs is shown to be independent of solvent and DCM is a much more convenient solvent to work with.

  6. CHLORINATED SOLVENT CONTAMINATED SOILS AND GROUNDWATER: FIELD APPLICATION OF THE SOLVENT EXTRACTION RESIDUAL BIOTREATMENT TECHNOLOGY

    EPA Science Inventory

    A pilot scale demonstration of the Solvent Extraction Residual Biotreatment (SERB) technology was conducted at the former Sage's Dry Cleaner site in Jacksonville, FL. The SERB technology is a treatment train approach to complete site restoration, which combines an active in situ...

  7. AJIPHASE®: A Highly Efficient Synthetic Method for One-Pot Peptide Elongation in the Solution Phase by an Fmoc Strategy.

    PubMed

    Takahashi, Daisuke; Inomata, Tatsuji; Fukui, Tatsuya

    2017-06-26

    We previously reported an efficient peptide synthesis method, AJIPHASE®, that comprises repeated reactions and isolations by precipitation. This method utilizes an anchor molecule with long-chain alkyl groups as a protecting group for the C-terminus. To further improve this method, we developed a one-pot synthesis of a peptide sequence wherein the synthetic intermediates were isolated by solvent extraction instead of precipitation. A branched-chain anchor molecule was used in the new process, significantly enhancing the solubility of long peptides and the operational efficiency compared with the previous method, which employed precipitation for isolation and a straight-chain aliphatic group. Another prerequisite for this solvent-extraction-based strategy was the use of thiomalic acid and DBU for Fmoc deprotection, which facilitates the removal of byproducts, such as the fulvene adduct. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Extraction and identification of cyclobutanones from irradiated cheese employing a rapid direct solvent extraction method.

    PubMed

    Tewfik, Ihab

    2008-01-01

    2-Alkylcyclobutanones (cyclobutanones) are accepted as chemical markers for irradiated foods containing lipid. However, current extraction procedures (Soxhlet-florisil chromatography) for the isolation of these markers involve a long and tedious clean-up regime prior to gas chromatography-mass spectrophotometry identification. This paper outlines an alternative isolation and clean-up method for the extraction of cyclobutanones in irradiated Camembert cheese. The newly developed direct solvent extraction method enables the efficient screening of large numbers of food samples and is not as resource intensive as the BS EN 1785:1997 method. Direct solvent extraction appears to be a simple, robust method and has the added advantage of a considerably shorter extraction time for the analysis of foods containing lipid.

  9. Microwave-assisted extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb.

    PubMed

    Zhang, Fan; Yang, Yi; Su, Ping; Guo, Zhenku

    2009-01-01

    Euonymus alatus (Thunb.) has been used as one of traditional Chinese medicines for several thousand years. Conventional methods for the extraction of rutin and quercetin from E. alatus, including solvent extraction, Soxhlet extraction and heat reflux extraction are characterised by long extraction times and consumption of large amounts of solvents. To develop a simple and rapid method for the extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb using microwave-assisted extraction (MAE) technique. MAE experiments were performed with a multimode microwave extraction system. The experimental variables that affect the MAE process, such as the concentration of ethanol solution, extractant volume, microwave power and extraction time were optimised. Yields were determined by HPLC. The results were compared with that obtained by classical Soxhlet and ultrasonic-assisted extraction (UAE). From the optimised conditions for MAE of rutin and quercetin it can be concluded that the solvent is 50% ethanol (v/v) solution, the extractant volume is 40 mL, microwave power is 170 W and irradiation time is 6 min. Compared with Soxhlet extraction and ultrasonic extraction, microwave extraction is a rapid method with a higher yield and lower solvent consumption. The results showed that MAE can be used as an efficient and rapid method for the extraction of the active components from plants.

  10. Protein Solvent-Accessibility Prediction by a Stacked Deep Bidirectional Recurrent Neural Network.

    PubMed

    Zhang, Buzhong; Li, Linqing; Lü, Qiang

    2018-05-25

    Residue solvent accessibility is closely related to the spatial arrangement and packing of residues. Predicting the solvent accessibility of a protein is an important step to understand its structure and function. In this work, we present a deep learning method to predict residue solvent accessibility, which is based on a stacked deep bidirectional recurrent neural network applied to sequence profiles. To capture more long-range sequence information, a merging operator was proposed when bidirectional information from hidden nodes was merged for outputs. Three types of merging operators were used in our improved model, with a long short-term memory network performing as a hidden computing node. The trained database was constructed from 7361 proteins extracted from the PISCES server using a cut-off of 25% sequence identity. Sequence-derived features including position-specific scoring matrix, physical properties, physicochemical characteristics, conservation score and protein coding were used to represent a residue. Using this method, predictive values of continuous relative solvent-accessible area were obtained, and then, these values were transformed into binary states with predefined thresholds. Our experimental results showed that our deep learning method improved prediction quality relative to current methods, with mean absolute error and Pearson's correlation coefficient values of 8.8% and 74.8%, respectively, on the CB502 dataset and 8.2% and 78%, respectively, on the Manesh215 dataset.

  11. Determination of terpenoid content in pine by organic solvent extraction and fast-GC analysis

    DOE PAGES

    Harman-Ware, Anne E.; Sykes, Robert; Peter, Gary F.; ...

    2016-01-25

    Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts frommore » the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. In conclusion, diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.« less

  12. Fast automated dual-syringe based dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

    PubMed

    Guo, Liang; Tan, Shufang; Li, Xiao; Lee, Hian Kee

    2016-03-18

    An automated procedure, combining low density solvent based solvent demulsification dispersive liquid-liquid microextraction (DLLME) with gas chromatography-mass spectrometry analysis, was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Capitalizing on a two-rail commercial autosampler, fast solvent transfer using a large volume syringe dedicated to the DLLME process, and convenient extract collection using a small volume microsyringe for better GC performance were enabled. Extraction parameters including the type and volume of extraction solvent, the type and volume of dispersive solvent and demulsification solvent, extraction and demulsification time, and the speed of solvent injection were investigated and optimized. Under the optimized conditions, the linearity ranged from 0.1 to 50 μg/L, 0.2 to 50 μg/L, and 0.5 to 50 μg/L, depending on the analytes. Limits of detection were determined to be between 0.023 and 0.058 μg/L. The method was applied to determine PAHs in environmental water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. SOLVENT EXTRACTION PROCESS FOR THE RECOVERY OF METALS FROM PHOSPHORIC ACID

    DOEpatents

    Bailes, R.H.; Long, R.S.

    1958-11-01

    > A solvent extraction process is presented for recovering metal values including uranium, thorium, and other lanthanide and actinide elements from crude industrial phosphoric acid solutions. The process conslsts of contacting said solution with an immisclble organic solvent extractant containing a diluent and a material selected from the group consisting of mono and di alkyl phosphates, alkyl phosphonates and alkyl phosphites. The uranlum enters the extractant phase and is subsequently recovered by any of the methods known to the art. Recovery is improved if the phosphate solution is treated with a reducing agent such as iron or aluminum powder prior to the extraction step.

  14. Development of a rapid method for the sequential extraction and subsequent quantification of fatty acids and sugars from avocado mesocarp tissue.

    PubMed

    Meyer, Marjolaine D; Terry, Leon A

    2008-08-27

    Methods devised for oil extraction from avocado (Persea americana Mill.) mesocarp (e.g., Soxhlet) are usually lengthy and require operation at high temperature. Moreover, methods for extracting sugars from avocado tissue (e.g., 80% ethanol, v/v) do not allow for lipids to be easily measured from the same sample. This study describes a new simple method that enabled sequential extraction and subsequent quantification of both fatty acids and sugars from the same avocado mesocarp tissue sample. Freeze-dried mesocarp samples of avocado cv. Hass fruit of different ripening stages were extracted by homogenization with hexane and the oil extracts quantified for fatty acid composition by GC. The resulting filter residues were readily usable for sugar extraction with methanol (62.5%, v/v). For comparison, oil was also extracted using the standard Soxhlet technique and the resulting thimble residue extracted for sugars as before. An additional experiment was carried out whereby filter residues were also extracted using ethanol. Average oil yield using the Soxhlet technique was significantly (P < 0.05) higher than that obtained by homogenization with hexane, although the difference remained very slight, and fatty acid profiles of the oil extracts following both methods were very similar. Oil recovery improved with increasing ripeness of the fruit with minor differences observed in the fatty acid composition during postharvest ripening. After lipid removal, methanolic extraction was superior in recovering sucrose and perseitol as compared to 80% ethanol (v/v), whereas mannoheptulose recovery was not affected by solvent used. The method presented has the benefits of shorter extraction time, lower extraction temperature, and reduced amount of solvent and can be used for sequential extraction of fatty acids and sugars from the same sample.

  15. Effective recovery of poly-β-hydroxybutyrate (PHB) biopolymer from Cupriavidus necator using a novel and environmentally friendly solvent system.

    PubMed

    Fei, Tao; Cazeneuve, Stacy; Wen, Zhiyou; Wu, Lei; Wang, Tong

    2016-05-01

    This work demonstrates a significant advance in bioprocessing for a high-melting lipid polymer. A novel and environmental friendly solvent mixture, acetone/ethanol/propylene carbonate (A/E/P, 1:1:1 v/v/v) was identified for extracting poly-hydroxybutyrate (PHB), a high-value biopolymer, from Cupriavidus necator. A set of solubility curves of PHB in various solvents was established. PHB recovery of 85% and purity of 92% were obtained from defatted dry biomass (DDB) using A/E/P. This solvent mixture is compatible with water, and from non-defatted wet biomass, PHB recovery of 83% and purity of 90% were achieved. Water and hexane were evaluated as anti-solvents to assist PHB precipitation, and hexane improved recovery of PHB from biomass to 92% and the purity to 93%. A scale-up extraction and separation reactor was designed, built and successfully tested. Properties of PHB recovered were not significantly affected by the extraction solvent and conditions, as shown by average molecular weight (1.4 × 10(6) ) and melting point (175.2°C) not being different from PHB extracted using chloroform. Therefore, this biorenewable solvent system was effective and versatile for extracting PHB biopolymers. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:678-685, 2016. © 2016 American Institute of Chemical Engineers.

  16. Comparative Analysis of the Properties of Acid-Base Indicator of Rose (Rosa setigera), Allamanda (Allamanda cathartica), and Hibiscus (Hibiscus rosa-sinensis) Flowers

    PubMed Central

    Okoduwa, Stanley I. R.; Mbora, Lovina O.; Adu, Matthew E.; Adeyi, Ameh A.

    2015-01-01

    The need to develop effective alternative for synthetic indicators is the demand of present-day chemistry. The acid-base indicator properties of Rose (Rosa setigera), Allamanda (Allamanda cathartica), and Hibiscus (Hibiscus rosa-sinensis) flowers were examined. Colour pigments were extracted from the flowers via cold and solvent extraction using soxhlet extractor. The pH value of the extracts with wavelengths of absorption was determined using ultraviolet spectrophotometer. From the results obtained, all the extracts exhibited sharp contrast between their colours in acid and base. Their pH was found to be 5.5 for cold extract of Rose and 5.6 for solvent extraction, 5.24 for cold extract of a Hibiscus and 6.52 for solvent extraction, 5.35 for cold extract of Allamanda, and 5.45 for solvent extraction. The maximum wavelengths of absorption obtained for all the extract fall within the visible region of electromagnetic spectrum. These values are almost similar to that obtained from synthetic indicators. It is on these bases that we concluded that natural indicators could be an excellent replacement for synthetic indicators since they are cheap, readily available, simple to extract, not toxic, user and environmentally friendly. PMID:26819757

  17. Maximizing Lipid Yield in Neochloris oleoabundans Algae Extraction by Stressing and Using Multiple Extraction Stages with N-Ethylbutylamine as Switchable Solvent

    PubMed Central

    2017-01-01

    The extraction yield of lipids from nonbroken Neochloris oleoabundans was maximized by using multiple extraction stages and using stressed algae. Experimental parameters that affect the extraction were investigated. The study showed that with wet algae (at least) 18 h extraction time was required for maximum yield at room temperature and a solvent/feed ratio of 1:1 (w/w). For fresh water (FW), nonstressed, nonbroken Neochloris oleoabundans, 13.1 wt % of lipid extraction yield (based on dry algae mass) was achieved, which could be improved to 61.3 wt % for FW stressed algae after four extractions, illustrating that a combination of stressing the algae and applying the solvent N-ethylbutylamine in multiple stages of extraction results in almost 5 times higher yield and is very promising for further development of energy-efficient lipid extraction technology targeting nonbroken wet microalgae. PMID:28781427

  18. LPS-induced NO inhibition and antioxidant activities of ethanol extracts and their solvent partitioned fractions from four brown seaweeds

    NASA Astrophysics Data System (ADS)

    Cho, Myoung Lae; Lee, Dong-Jin; Lee, Hyi-Seung; Lee, Yeon-Ju; You, Sang Guan

    2013-12-01

    The nitric oxide inhibitory (NOI) and antioxidant (ABTS and DPPH radical scavenging effects with reducing power) activities of the ethanol (EtOH) extracts and solvent partitioned fractions from Scytosiphon lomentaria, Chorda filum, Agarum cribrosum, and Desmarestia viridis were investigated, and the correlation between biological activity and total phenolic (TP) and phlorotannin (TPT) content was determined by PCA analysis. The yield of EtOH extracts from four brown seaweeds ranged from 2.6 to 6.6% with the highest yield from D. viridis, and the predominant compounds in their solvent partitioned fractions had medium and/or less polarity. The TP and TPT content of the EtOH extracts were in the ranges of 25.0-44.1 mg GAE/g sample and 0.2-4.6 mg PG/g sample, respectively, which were mostly included in the organic solvent partitioned fractions. Strong NOI activity was observed in the EtOH extracts and their solvent partitioned fractions from D. viridis and C. filum. In addition, the EtOH extract and its solvent partitioned fractions of D. viridis exhibited little cytotoxicity to Raw 264.7 cells. The most potent ABTS and DPPH radical scavenging capacity was shown in the EtOH extracts and their solvent partitioned fractions from S. lomentaria and C. filum, and both also exhibited strong reducing ability. In the PCA analysis the content of TPT had a good correlation with DPPH ( r = 0.62), ABTS ( r = 0.69) and reducing power ( r = 0.65), however, an unfair correlation was observed between the contents of TP and TPT and NOI, suggesting that the phlorotannins might be responsible for the DPPH and ABTS radical scavenging activities.

  19. Use of solvent mixtures for total lipid extraction of Chlorella vulgaris and gas chromatography FAME analysis.

    PubMed

    Moradi-Kheibari, Narges; Ahmadzadeh, Hossein; Hosseini, Majid

    2017-09-01

    Lipid extraction is the bottleneck step for algae-based biodiesel production. Herein, 12 solvent mixture systems (mixtures of three non-polar and two polar organic solvents) were examined to evaluate their effects on the total lipid yield from Chlorella vulgaris (C. vulgaris). Moreover, the extraction yields of three solvent systems with maximum extraction efficiency of esterifiable lipids were determined by acidic transesterification and GC-FID analysis. Three solvent systems, which resulted in a higher extraction yield, were further subjected to fatty acid methyl ester (FAME) analysis. The total lipid extraction yields (based on dry biomass) were (38.57 ± 1.51), (25.33 ± 0.58), and (25.17 ± 1.14) %, for chloroform-methanol (1:2) (C1M2), hexane-methanol (1:2) (H1M2), and chloroform-methanol (2:1) (C2M1), respectively. The extraction efficiency of C1M2 was approximately 1.5 times higher than H1M2 and C2M1, whereas the FAME profile of extracted lipids by H1M2 and C1M2 were almost identical. Moreover, the esterifiable lipid extraction yields of (18.14 ± 2.60), (16.66 ± 0.35), and (13.22 ± 0.31) % (based on dry biomass) were obtained for C1M2, H1M2, and C2M1 solvent mixture systems, respectively. The biodiesel fuel properties produced from C. vulgaris were empirically predicted and compared to that of the EN 14214 and ASTM 6751 standard specifications.

  20. A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani

    Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

  1. A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

    DOE PAGES

    Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani; ...

    2017-07-11

    Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

  2. Impact of quality parameters on the recovery of putrescine and cadaverine in fish using methanol-hydrochloric acid solvent extraction.

    PubMed

    Richard, Nicole L; Pivarnik, Lori F; Ellis, P Christopher; Lee, Chong M

    2011-01-01

    Methanol (MeOH) extraction by AOAC Official Method 996.07 has resulted in low amine recoveries in fresh fish tissue. Addition of 25% 0.4 M HCl to the 75% methanol-water extraction solvent resulted in higher recoveries of putrescine and cadaverine. Average putrescine recovery increased from 55 to 92% in flounder, scup, bluefish, and salmon; from 92 to 98% in mackerel; and from 83 to 107% in processed mackerel. Average cadaverine recovery increased from 57 to 95% in flounder, scup, bluefish, and salmon; from 91 to 97% in mackerel; and from 92 to 108% in processed mackerel. Fish stored on ice for 12 days also showed differences between background concentrations determined with the two solvents. However, the values decreased with storage time, indicating that degradation of the protein matrix may cause more comparable measurements between the two solvents. However, consistently higher putrescine and cadaverine measurements were determined using MeOH-HCl. Although significant differences in the extraction of amines from the high-fat fish tissue were not seen between MeOH and MeOH-HCl, it would be ideal to have one solvent for biogenic amine extraction. This study confirms that MeOH-HCl is a better solvent for complete extraction and recovery of putrescine and cadaverine in fresh and processed fish tissues.

  3. Trace elements retained in washed nuclear fuel reprocessing solvents

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Gray, L.W.; MacMurdo, K.W.

    1979-09-01

    Analysis of purified TBP extractant from solvent extraction processes at Savannah River Plant showed several stable elements and several long-lived radioisotopes. Stable elements Al, Na, Br, Ce, Hg, and Sm are found in trace quantities in the solvent. The only stable metallic element consistently found in the solvent was Al, with a concentration which varies from about 30 ppM to about 10 ppM. The halogens Br and Cl appear to be found in the solvent systems as organo halides. Radionuclides found were principally /sup 106/Ru, /sup 129/I, /sup 3/H, /sup 235/U, and /sup 239/Pu. The /sup 129/I concentration was aboutmore » 1 ppM in the first solvent extraction cycle of each facility. In the other cycles, /sup 129/I concentration varied from about 0.1 to 0.5 ppM. Both /sup 129/I and /sup 3/H appear to be in the organic solvent as a result of exchange with hydrogen.« less

  4. Prayon process for wet acid purification

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Davister, A.; Peeterbroeck, M.

    Described is a process developed in Belgium which enables the upgrading technical phosphoric acid to feed and food grades. After laboratory and pilot tests, Prayon developed and patented a solvent extraction process using a mixture of di-isopropyl ether and tributyl phosphate as solvent. The purified phosphoric acid obtained complies with the quality requirements of the market and can be used for metal treatments, in the manufacture of pure phosphates, for cattle feed, by the fermentation industry, for beverages, etc. Among the advantages of this process are its simplicity of operation, its low power consumption, and minimal environmental pollution. Extensive technologicalmore » data are given.« less

  5. Extraction of orange peel's essential oil by solvent-free microwave extraction

    NASA Astrophysics Data System (ADS)

    Qadariyah, Lailatul; Amelia, Prilia Dwi; Admiralia, Cininta; Bhuana, Donny S.; Mahfud, Mahfud

    2017-05-01

    Sweet orange peel (Citrus sinensis) is part of orange plant that contains essential oils. Generally, taking essential oil from orange peel is still using hydrodistillation and steam-hydrodistillation method which still needs solvent and takes a long time to produce high quality essential oil. Therefore, the objectives of this experiment are to study the process of orange peel's essential oil extraction using Solvent Free Microwave Extraction (SFME) and to study the operating condition that effect an optimum yield and quality of the essential oil. In this experiment, extraction process with SFME method goes for 60 minutes at atmospheric pressure. Variables for SFME are: variation of orange peel condition (fresh and dry), ratio orange peel mass to distiller volume (0,1; 0,2; 0,3; 0,4 g/mL), orange peel size (±0,5; ±2; ±3,5 cm width), and microwave power (100, 264, 400 Watt). Moisture content of fresh peel is 71,4% and for dry peel is 17,37% which is obtained by sun drying. The result of this experiment will be analyzed with GC-MS, SEM, density, and miscibility in ethanol 90%. The optimum result obtained from this experiment based on the number of the yield under condition of fresh orange peel is at peel mass/distiller volume 0,1 g/mL, orange peel size ±3,5 cm width, and microwave power 400 Watt, results 1,6738% yield. The result of GC-MS for fresh orange peel shows that the dominant compound is Limonene 54,140% and for dry orange peel is Limonene 59,705%. The density obtained is around 0,8282-0,8530 g/mL and miscibility in ethanol 90% is 1:5.

  6. Microbial solubilization of phosphate

    DOEpatents

    Rogers, R.D.; Wolfram, J.H.

    1993-10-26

    A process is provided for solubilizing phosphate from phosphate containing ore by treatment with microorganisms which comprises forming an aqueous mixture of phosphate ore, microorganisms operable for solubilizing phosphate from the phosphate ore and maintaining the aqueous mixture for a period of time and under conditions operable to effect the microbial solubilization process. An aqueous solution containing soluble phosphorus can be separated from the reacted mixture by precipitation, solvent extraction, selective membrane, exchange resin or gravity methods to recover phosphate from the aqueous solution. 6 figures.

  7. Microbial solubilization of phosphate

    DOEpatents

    Rogers, Robert D.; Wolfram, James H.

    1993-01-01

    A process is provided for solubilizing phosphate from phosphate containing ore by treatment with microorganisms which comprises forming an aqueous mixture of phosphate ore, microorganisms operable for solubilizing phosphate from the phosphate ore and maintaining the aqueous mixture for a period of time and under conditions operable to effect the microbial solubilization process. An aqueous solution containing soluble phosphorous can be separated from the reacted mixture by precipitation, solvent extraction, selective membrane, exchange resin or gravity methods to recover phosphate from the aqueous solution.

  8. Deep Eutectic Solvent-Based Microwave-Assisted Method for Extraction of Hydrophilic and Hydrophobic Components from Radix Salviae miltiorrhizae.

    PubMed

    Chen, Jue; Liu, Mengjun; Wang, Qi; Du, Huizhi; Zhang, Liwei

    2016-10-17

    Deep eutectic solvents (DESs) have attracted significant attention as a promising green media. In this work, twenty-five kinds of benign choline chloride-based DESs with microwave-assisted methods were applied to quickly extract active components from Radix Salviae miltiorrhizae . The extraction factors, including temperature, time, power of microwave, and solid/liquid ratio, were investigated systematically by response surface methodology. The hydrophilic and hydrophobic ingredients were extracted simultaneously under the optimized conditions: 20 vol% of water in choline chloride/1,2-propanediol (1:1, molar ratio) as solvent, microwave power of 800 W, temperature at 70 °C, time at 11.11 min, and solid/liquid ratio of 0.007 g·mL -1 . The extraction yield was comparable to, or even better than, conventional methods with organic solvents. The microstructure alteration of samples before and after extraction was also investigated. The method validation was tested as the linearity of analytes ( r ² > 0.9997 over two orders of magnitude), precision (intra-day relative standard deviation (RSD) < 2.49 and inter-day RSD < 2.96), and accuracy (recoveries ranging from 95.04% to 99.93%). The proposed DESs combined with the microwave-assisted method provided a prominent advantage for fast and efficient extraction of active components, and DESs could be extended as solvents to extract and analyze complex environmental and pharmaceutical samples.

  9. Application of enzyme-linked immunosorbent assay for measurement of polychlorinated biphenyls from hydrophobic solutions: Extracts of fish and dialysates of semipermeable membrane devices: Chapter 26

    USGS Publications Warehouse

    Zajicek, James L.; Tillitt, Donald E.; Huckins, James N.; Petty, Jimmie D.; Potts, Michael E.; Nardone, David A.

    1996-01-01

    Determination of PCBs in biological tissue extracts by enzyme-linked immunosorbent assays (ELISAs) can be problematic, since the hydrophobic solvents used for their extraction and isolation from interfering biochemicals have limited compatibility with the polar solvents (e.g. methanol/water) and the immunochemical reagents used in ELISA. Our studies of these solvent effects indicate that significant errors can occur when microliter volumes of PCB containing extracts, in hydrophobic solvents, are diluted directly into methanol/water diluents. Errors include low recovery and excess variability among sub-samples taken from the same sample dilution. These errors are associated with inhomogeneity of the dilution, which is readily visualized by the use of a hydrophobic dye, Solvent Blue 35. Solvent Blue 35 is also used to visualize the evaporative removal of hydrophobic solvent and the dissolution of the resulting PCB/dye residue by pure methanol and 50% (v/v) methanol/water, typical ELISA diluents. Evaporative removal of isooctane by an ambient temperature nitrogen purge with subsequent dissolution in 100% methanol gives near quantitative recovery of model PCB congeners. We also compare concentrations of total PCBs from ELISA (ePCB) to their corresponding concentrations determined from capillary gas chromatography (GC) in selected fish sample extracts and dialysates of semipermeable membrane device (SPMD) passive samplers using an optimized solvent exchange procedure. Based on Aroclor 1254 calibrations, ePCBs (ng/mL) determined in fish extracts are positively correlated with total PCB concentrations (ng/mL) determined by GC: ePCB = 1.16 * total-cPCB - 5.92. Measured ePCBs (ng/3 SPMDs) were also positively correlated (r2 = 0.999) with PCB totals (ng/3 SPMDs) measured by GC for dialysates of SPMDs: ePCB = 1.52 * total PCB - 212. Therefore, this ELISA system for PCBs can be a rapid alternative to traditional GC analyses for determination of PCBs in extracts of biota or in SPMD dialysates.

  10. The influence of extractable organic matter on vitrinite reflectance suppression: A survey of kerogen and coal types

    USGS Publications Warehouse

    Barker, C.E.; Lewan, M.D.; Pawlewicz, M.J.

    2007-01-01

    The vitrinite reflectance suppression literature shows that while bitumen impregnation of the vitrinite group is often invoked as a significant contributor to suppression, its existence is not often supported by petrological evidence. This study examines bitumen impregnation as a factor in vitrinite suppression by comparing the vitrinite reflectance of source rock and coal samples before and after solvent-extraction. Bitumen, often defined as organic matter soluble or extractable in certain organic solvents, should be removed by Soxhlet method solvent extraction using chloroform. Removing the extractable bitumen should restore the suppressed reflectance to its true higher value. However, the solvent extracted samples averaged 0.014% Rv less than that of the unextracted samples. We conclude from these results and from other published data that reflectance suppression by bitumen impregnation in the vitrinite maceral group, above the huminite stage of gelification, is seemingly a rare phenomenon and whose effect on suppressing vitrinite reflectance is typically negligible. ?? 2006.

  11. Oil extraction from sheanut (Vitellaria paradoxa Gaertn C.F.) kernels assisted by microwaves.

    PubMed

    Nde, Divine B; Boldor, Dorin; Astete, Carlos; Muley, Pranjali; Xu, Zhimin

    2016-03-01

    Shea butter, is highly solicited in cosmetics, pharmaceuticals, chocolates and biodiesel formulations. Microwave assisted extraction (MAE) of butter from sheanut kernels was carried using the Doehlert's experimental design. Factors studied were microwave heating time, temperature and solvent/solute ratio while the responses were the quantity of oil extracted and the acid number. Second order models were established to describe the influence of experimental parameters on the responses studied. Under optimum MAE conditions of heating time 23 min, temperature 75 °C and solvent/solute ratio 4:1 more than 88 % of the oil with a free fatty acid (FFA) value less than 2, was extracted compared to the 10 h and solvent/solute ratio of 10:1 required for soxhlet extraction. Scanning electron microscopy was used to elucidate the effect of microwave heating on the kernels' microstructure. Substantial reduction in extraction time and volumes of solvent used and oil of suitable quality are the main benefits derived from the MAE process.

  12. Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

    PubMed

    Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

    2014-06-01

    Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

  13. Determination of phthalate esters in distillates by ultrasound-vortex-assisted dispersive liquid-liquid micro-extraction (USVADLLME) coupled with gas chromatography/mass spectrometry.

    PubMed

    Montevecchi, Giuseppe; Masino, Francesca; Zanasi, Luca; Antonelli, Andrea

    2017-04-15

    A method for the extraction of phthalate esters (PAEs) by Ultrasound-Vortex-Assisted Dispersive Liquid-Liquid Micro-Extraction (USVADLLME) approach was optimised and applied for the first time to a historical series of brandies. These contaminants are widely spread in the environment as a consequence of about half century of use in different fields of applications. The concern about these substances and the recent legal restrictions of China in distillates import need a quick and sensitive method for their quantification. The proposed method, moreover, is environmentally oriented due to the disposal of micro-quantities of solvent required. In fact, sub-ppm-limits of detection were achieved with a solvent volume as low as 160μL. The analysed samples were within the legal limits, except for some very ancient brandies whose contamination was probably due to a PAEs concentration effect as a consequence of long ageing and for the use of plastic pipelines no more operative. Copyright © 2016 Elsevier Ltd. All rights reserved.

  14. ALKYL PYROPHOSPHATE METAL SOLVENT EXTRACTANTS AND PROCESS

    DOEpatents

    Long, R.L.

    1958-09-30

    A process is presented for the recovery of uranium from aqueous mineral acidic solutions by solvent extraction. The extractant is a synmmetrical dialkyl pyrophosphate in which the alkyl substituents have a chain length of from 4 to 17 carbon atoms. Mentioned as a preferred extractant is dioctyl pyrophosphate. The uranium is precipitated irom the organic extractant phase with an agent such as HF, fluoride salts. alcohol, or ammonia.

  15. Stable Isotope-Assisted Evaluation of Different Extraction Solvents for Untargeted Metabolomics of Plants

    PubMed Central

    Doppler, Maria; Kluger, Bernhard; Bueschl, Christoph; Schneider, Christina; Krska, Rudolf; Delcambre, Sylvie; Hiller, Karsten; Lemmens, Marc; Schuhmacher, Rainer

    2016-01-01

    The evaluation of extraction protocols for untargeted metabolomics approaches is still difficult. We have applied a novel stable isotope-assisted workflow for untargeted LC-HRMS-based plant metabolomics , which allows for the first time every detected feature to be considered for method evaluation. The efficiency and complementarity of commonly used extraction solvents, namely 1 + 3 (v/v) mixtures of water and selected organic solvents (methanol, acetonitrile or methanol/acetonitrile 1 + 1 (v/v)), with and without the addition of 0.1% (v/v) formic acid were compared. Four different wheat organs were sampled, extracted and analysed by LC-HRMS. Data evaluation was performed with the in-house-developed MetExtract II software and R. With all tested solvents a total of 871 metabolites were extracted in ear, 785 in stem, 733 in leaf and 517 in root samples, respectively. Between 48% (stem) and 57% (ear) of the metabolites detected in a particular organ were found with all extraction mixtures, and 127 of 996 metabolites were consistently shared between all extraction agent/organ combinations. In aqueous methanol, acidification with formic acid led to pronounced pH dependency regarding the precision of metabolite abundance and the number of detectable metabolites, whereas extracts of acetonitrile-containing mixtures were less affected. Moreover, methanol and acetonitrile have been found to be complementary with respect to extraction efficiency. Interestingly, the beneficial properties of both solvents can be combined by the use of a water-methanol-acetonitrile mixture for global metabolite extraction instead of aqueous methanol or aqueous acetonitrile alone. PMID:27367667

  16. Extractables analysis of single-use flexible plastic biocontainers.

    PubMed

    Marghitoiu, Liliana; Liu, Jian; Lee, Hans; Perez, Lourdes; Fujimori, Kiyoshi; Ronk, Michael; Hammond, Matthew R; Nunn, Heather; Lower, Asher; Rogers, Gary; Nashed-Samuel, Yasser

    2015-01-01

    Studies of the extractable profiles of bioprocessing components have become an integral part of drug development efforts to minimize possible compromise in process performance, decrease in drug product quality, and potential safety risk to patients due to the possibility of small molecules leaching out from the components. In this study, an effective extraction solvent system was developed to evaluate the organic extractable profiles of single-use bioprocess equipment, which has been gaining increasing popularity in the biopharmaceutical industry because of the many advantages over the traditional stainless steel-based bioreactors and other fluid mixing and storage vessels. The chosen extraction conditions were intended to represent aggressive conditions relative to the application of single-use bags in biopharmaceutical manufacture, in which aqueous based systems are largely utilized. Those extraction conditions, along with a non-targeted analytical strategy, allowed for the generation and identification of an array of extractable compounds; a total of 53 organic compounds were identified from four types of commercially available single-use bags, the majority of which are degradation products of polymer additives. The success of this overall extractables analysis strategy was reflected partially by the effectiveness in the extraction and identification of a compound that was later found to be highly detrimental to mammalian cell growth. The usage of single-use bioreactors has been increasing in biopharmaceutical industry because of the appealing advantages that it promises regarding to the cleaning, sterilization, operational flexibility, and so on, during manufacturing of biologics. However, compared to its conventional counterparts based mainly on stainless steel, single-use bioreactors are more susceptible to potential problems associated with compound leaching into the bioprocessing fluid. As a result, extractable profiling of the single-use system has become essential in the qualification of such systems for its use in drug manufacturing. The aim of this study is to evaluate the effectiveness of an extraction solvent system developed to study the extraction profile of single-use bioreactors in which aqueous-based systems are largely used. The results showed that with a non-targeted analytical approach, the extraction solvent allowed the generation and identification of an array of extractable compounds from four commercially available single-use bioreactors. Most of extractables are degradation products of polymer additives, among which was a compound that was later found to be highly detrimental to mammalian cell growth. © PDA, Inc. 2015.

  17. Optimization and determination of polycyclic aromatic hydrocarbons in biochar-based fertilizers.

    PubMed

    Chen, Ping; Zhou, Hui; Gan, Jay; Sun, Mingxing; Shang, Guofeng; Liu, Liang; Shen, Guoqing

    2015-03-01

    The agronomic benefit of biochar has attracted widespread attention to biochar-based fertilizers. However, the inevitable presence of polycyclic aromatic hydrocarbons in biochar is a matter of concern because of the health and ecological risks of these compounds. The strong adsorption of polycyclic aromatic hydrocarbons to biochar complicates their analysis and extraction from biochar-based fertilizers. In this study, we optimized and validated a method for determining the 16 priority polycyclic aromatic hydrocarbons in biochar-based fertilizers. Results showed that accelerated solvent extraction exhibited high extraction efficiency. Based on a Box-Behnken design with a triplicate central point, accelerated solvent extraction was used under the following optimal operational conditions: extraction temperature of 78°C, extraction time of 17 min, and two static cycles. The optimized method was validated by assessing the linearity of analysis, limit of detection, limit of quantification, recovery, and application to real samples. The results showed that the 16 polycyclic aromatic hydrocarbons exhibited good linearity, with a correlation coefficient of 0.996. The limits of detection varied between 0.001 (phenanthrene) and 0.021 mg/g (benzo[ghi]perylene), and the limits of quantification varied between 0.004 (phenanthrene) and 0.069 mg/g (benzo[ghi]perylene). The relative recoveries of the 16 polycyclic aromatic hydrocarbons were 70.26-102.99%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Highly selective solid-phase extraction and large volume injection for the robust gas chromatography-mass spectrometric analysis of TCA and TBA in wines.

    PubMed

    Insa, S; Anticó, E; Ferreira, V

    2005-09-30

    A reliable solid-phase extraction (SPE) method for the simultaneous determination of 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA) in wines has been developed. In the proposed procedure 50 mL of wine are extracted in a 1 mL cartridge filled with 50 mg of LiChrolut EN resins. Most wine volatiles are washed up with 12.5 mL of a water:methanol solution (70%, v/v) containing 1% of NaHCO3. Analytes are further eluted with 0.6 mL of dichloromethane. A 40 microL aliquot of this extract is directly injected into a PTV injector operated in the solvent split mode, and analysed by gas chromatography (GC)-ion trap mass spectrometry using the selected ion storage mode. The solid-phase extraction, including sample volume and rinsing and elution solvents, and the large volume GC injection have been carefully evaluated and optimized. The resulting method is precise (RSD (%) < 6% at 100 ng L(-1)), sensitive (LOD were 0.2 and 0.4 ng/L for TCA and TBA, respectively), robust (the absolute recoveries of both analytes are higher than 80% and consistent wine to wine) and friendly to the GC-MS system (the extract is clean, simple and free from non-volatiles).

  19. Fundamental Chemical Kinetic And Thermodynamic Data For Purex Process Models

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Taylor, R.J.; Fox, O.D.; Sarsfield, M.J.

    2007-07-01

    To support either the continued operations of current reprocessing plants or the development of future fuel processing using hydrometallurgical processes, such as Advanced Purex or UREX type flowsheets, the accurate simulation of Purex solvent extraction is required. In recent years we have developed advanced process modeling capabilities that utilize modern software platforms such as Aspen Custom Modeler and can be run in steady state and dynamic simulations. However, such advanced models of the Purex process require a wide range of fundamental data including all relevant basic chemical kinetic and thermodynamic data for the major species present in the process. Thismore » paper will summarize some of these recent process chemistry studies that underpin our simulation, design and testing of Purex solvent extraction flowsheets. Whilst much kinetic data for actinide redox reactions in nitric acid exists in the literature, the data on reactions in the diluted TBP solvent phase is much rarer. This inhibits the accurate modelization of the Purex process particularly when species show a significant extractability in to the solvent phase or when cycling between solvent and aqueous phases occurs, for example in the reductive stripping of Pu(IV) by ferrous sulfamate in the Magnox reprocessing plant. To support current oxide reprocessing, we have investigated a range of solvent phase reactions: - U(IV)+HNO{sub 3}; - U(IV)+HNO{sub 2}; - U(IV)+HNO{sub 3} (Pu catalysis); - U(IV)+HNO{sub 3} (Tc catalysis); - U(IV)+ Np(VI); - U(IV)+Np(V); - Np(IV)+HNO{sub 3}; - Np(V)+Np(V); Rate equations have been determined for all these reactions and kinetic rate constants and activation energies are now available. Specific features of these reactions in the TBP phase include the roles of water and hydrolyzed intermediates in the reaction mechanisms. In reactions involving Np(V), cation-cation complex formation, which is much more favourable in TBP than in HNO{sub 3}, also occurs and complicates the redox chemistry. Whilst some features of the redox chemistry in TBP appear similar to the corresponding reactions in aqueous HNO{sub 3}, there are notable differences in rates, the forms of the rate equations and mechanisms. Secondly, to underpin the development of advanced single cycle flowsheets using the complexant aceto-hydroxamic acid, we have also characterised in some detail its redox chemistry and solvent extraction behaviour with both Np and Pu ions. We find that simple hydroxamic acids are remarkably rapid reducing agents for Np(VI). They also reduce Pu(VI) and cause a much slower reduction of Pu(IV) through a complex mechanism involving acid hydrolysis of the ligand. AHA is a strong hydrophilic and selective complexant for the tetravalent actinide ions as evidenced by stability constant and solvent extraction data for An(IV), M(III) and U(VI) ions. This has allowed the successful design of U/Pu+Np separation flowsheets suitable for advanced fuel cycles. (authors)« less

  20. Subcritical Fluid Extraction of Chinese Quince Seed: Optimization and Product Characterization.

    PubMed

    Wang, Li; Wu, Min; Liu, Hua-Min; Ma, Yu-Xiang; Wang, Xue-De; Qin, Guang-Yong

    2017-03-25

    Chinese quince seed (CQS) is an underutilized oil source and a potential source of unsaturated fatty acids and α-tocopherol-rich oil. Subcritical fluid (SCF) extraction is executed at lower pressures and temperatures than the pressures and temperatures used in supercritical fluid extraction. However, no studies on the SCF extraction of CQS oil are reported. Therefore, the objective of this study was to evaluate the use of SCF for the extraction of CQS oil and to compare the use of SCF with the classical Soxhlet (CS) and supercritical CO₂ (SC-CO₂) extraction methods. Response surface methodology (RSM) was used to investigate the extraction conditions: temperature (45-65 °C), time (30-50 min), and solvent/solid ratio (5-15 mL/g). The optimization results showed that the highest yield (27.78%) was obtained at 56.18 °C, 40.20 min, and 12.57 mL/g. The oil extracted by SCF had a higher unsaturated fatty acid content (86.37%-86.75%), higher α-tocopherol content (576.0-847.6 mg/kg), lower acid value (3.97 mg/g), and lower peroxide value (0.02 meq O₂/kg) than extractions using CS and SC-CO 2 methods. The SCF-defatted meal of oilseed exhibited the highest nitrogen solubility index (49.64%) and protein dispersibility index (50.80%), demonstrating that SCF extraction was a promising and efficient technique as an alternative to CS and SC-CO 2 methods, as very mild operating conditions and an eco-friendly solvent can be used in the process with maximum preservation of the quality of the meal.

  1. Carbon based thirty six atom spheres

    DOEpatents

    Piskoti, Charles R.; Zettl, Alex K.; Cohen, Marvin L.; Cote, Michel; Grossman, Jeffrey C.; Louie, Steven G.

    2005-09-06

    A solid phase or form of carbon is based on fullerenes with thirty six carbon atoms (C.sub.36). The C.sub.36 structure with D.sub.6h symmetry is one of the two most energetically favorable, and is conducive to forming a periodic system. The lowest energy crystal is a highly bonded network of hexagonal planes of C.sub.36 subunits with AB stacking. The C.sub.36 solid is not a purely van der Waals solid, but has covalent-like bonding, leading to a solid with enhanced structural rigidity. The solid C.sub.36 material is made by synthesizing and selecting out C.sub.36 fullerenes in relatively large quantities. A C.sub.36 rich fullerene soot is produced in a helium environment arc discharge chamber by operating at an optimum helium pressure (400 torr). The C.sub.36 is separated from the soot by a two step process. The soot is first treated with a first solvent, e.g. toluene, to remove the higher order fullerenes but leave the C.sub.36. The soot is then treated with a second solvent, e.g. pyridine, which is more polarizable than the first solvent used for the larger fullerenes. The second solvent extracts the C.sub.36 from the soot. Thin films and powders can then be produced from the extracted C.sub.36. Other materials are based on C.sub.36 fullerenes, providing for different properties.

  2. Simultaneous saccharification and extractive fermentation of lignocellulosic materials into lactic acid in a two-zone fermentor-extractor system.

    PubMed

    Iyer, P V; Lee, Y Y

    1999-01-01

    Simultaneous saccharification and extractive fermentation of lignocellulosic materials into lactic acid was investigated using a two-zone bioreactor. The system is composed of an immobilized cell reactor, a separate column reactor containing the lignocellulosic substrate and a hollow-fiber membrane. It is operated by recirculating the cell free enzyme (cellulase) solution from the immobilized cell reactor to the column reactor through the membrane. The enzyme and microbial reactions thus occur at separate locations, yet simultaneously. This design provides flexibility in reactor operation as it allows easy separation of the solid substrate from the microorganism, in situ removal of the product and, if desired, different temperatures in the two reactor sections. This reactor system was tested using pretreated switchgrass as the substrate. It was operated under a fed-batch mode with continuous removal of lactic acid by solvent extraction. The overall lactic acid yield obtainable from this bioreactor system is 77% of the theoretical.

  3. Unique reversibility in extraction mechanism of U compared to solvent extraction for sorption of U(VI) and Pu(IV) by a novel solvent impregnated resin containing trialkyl phosphine oxide functionalized ionic liquid.

    PubMed

    Paramanik, M; Panja, S; Dhami, P S; Yadav, J S; Kaushik, C P; Ghosh, S K

    2018-07-15

    Novel Solvent Impregnated Resin (SIR) material was prepared by impregnating a trialkyl phosphine oxide functionalized ionic liquid (IL) into an inert polymeric material XAD-7. A series of SIR materials were prepared by varying the IL quantity. Sorption of both U(VI) and Pu(IV) were found to increase with increasing IL concentration in SIR up to an optimum IL concentration of 435 mg g -1 of SIR beyond which no effect of IL concentration was observed. A change of mechanism of sorption for U(VI) by SIR was observed in comparison to solvent extraction. The dependency of U(VI) sorption with nitric acid concentration showed a reverse trend compared to solvent extraction studies while for Pu(IV) the trend remained same as observed with solvent extraction. Sorption of both the radionuclides was found to follow pseudo second order mechanism and Langmuir adsorption isotherm. Distribution co-efficient measurements on IL impregnated SIR showed highly selective sorption of U(VI) and Pu(IV) over other trivalent f-elements and fission products from nitric acid medium. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. Prevalence of pesticides in postconsumer agrochemical polymeric packaging.

    PubMed

    Eras, J; Costa, J; Vilaró, F; Pelacho, A M; Canela-Garayoa, R; Martin-Closas, L

    2017-02-15

    Pesticide remains contained in agrochemical packaging waste are a source of uncontrolled risk for human health; they are also a quality feedstock for the plastic recycling industry. Many governments have recently started to establish laws and regulations to develop systems for recovering and recycling the polymeric packages used for pesticides. There is also a demand in having a procedure to control the suitability of the pesticide packages to be reused. We have developed a two-step operation process to assess the pesticide residues in agricultural containers made of a variety of polymeric matrices. The procedure is based on an extraction with a solvent mixture followed by UPLC-MS/MS determination. Solvents for neutral pesticides were selected considering the Hildebrand solubility (δ) of solvents and polymers together with those estimated for the pesticides. The proposed technique is effective in recovering imbibed pesticides in polymeric matrices. Also, a simplified extraction procedure has been tested to become a routine method for these wastes. We have found that in many cases a significant amount of pesticides remain into the polymeric matrix, even after a standardized cleaning; the impact of releasing these hazardous compounds into the environment is to be of further consideration. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Fluid extraction

    DOEpatents

    Wai, Chien M.; Laintz, Kenneth E.

    1999-01-01

    A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated .beta.-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated .beta.-diketone and a trialkyl phosphate, or a fluorinated .beta.-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated .beta.-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

  6. Solvent jet desorption capillary photoionization-mass spectrometry.

    PubMed

    Haapala, Markus; Teppo, Jaakko; Ollikainen, Elisa; Kiiski, Iiro; Vaikkinen, Anu; Kauppila, Tiina J; Kostiainen, Risto

    2015-03-17

    A new ambient mass spectrometry method, solvent jet desorption capillary photoionization (DCPI), is described. The method uses a solvent jet generated by a coaxial nebulizer operated at ambient conditions with nitrogen as nebulizer gas. The solvent jet is directed onto a sample surface, from which analytes are extracted into the solvent and ejected from the surface in secondary droplets formed in collisions between the jet and the sample surface. The secondary droplets are directed into the heated capillary photoionization (CPI) device, where the droplets are vaporized and the gaseous analytes are ionized by 10 eV photons generated by a vacuum ultraviolet (VUV) krypton discharge lamp. As the CPI device is directly connected to the extended capillary inlet of the MS, high ion transfer efficiency to the vacuum of MS is achieved. The solvent jet DCPI provides several advantages: high sensitivity for nonpolar and polar compounds with limit of detection down to low fmol levels, capability of analyzing small and large molecules, and good spatial resolution (250 μm). Two ionization mechanisms are involved in DCPI: atmospheric pressure photoionization, capable of ionizing polar and nonpolar compounds, and solvent assisted inlet ionization capable of ionizing larger molecules like peptides. The feasibility of DCPI was successfully tested in the analysis of polar and nonpolar compounds in sage leaves and chili pepper.

  7. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F.; Taylor-Pashow, K.

    Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-556, MCU-15-557, and MCU-15-558), pulled on 03/16/2015 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-556-557-558 indicated a low concentration (~ 78 % of nominal) of the suppressor (TiDG) and concentrations of the extractant (MaxCalix), and of the modifier (CS-7SB) in the solvent that were slightly lower than nominal. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent in February 2015. Based on the current monthly sample, the levels of TiDG, MaxCalix, and modifier aremore » sufficient for continuing operation without adding a trim at this time. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). However, the p-nut vials that delivered the samples contained small (1 mm) droplets of oxidized modifier and amides (as detected by the FTIR analysis). In addition, up to 21 microgram of mercury per gram of solvent (or 17.4 µg/mL) was detected in this sample. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

  8. SUPPLEMENTAL ANALYSES FOR SOLVENT HOLD TANK SAMPLES MCU-11-314, MCU-11-315, MCU-11-316, MCU-11-317, MCU-11-318 AND MCU-11-319

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, T.; Washington, A; . Fondeur, F.

    2011-09-29

    Savannah River National Laboratory (SRNL) periodically analyses solvent samples from Modular Caustic-Side Solvent Extraction Unit (MCU) in support of continuing operations. A quarterly analysis of the solvent is required to maintain solvent composition within specifications. Analytical results of the analyses of Solvent Hold Tank (SHT) samples MCU-11-314, MCU-11-315, MCU-11-316, MCU-11-317, MCU-11-318 and MCU-11-319 have been previously reported. MCU has experienced a modest decline in cesium removal efficiency while processing the current feed, 'Macrobatch 3'. While the target decontamination factor (DF) is 200, the fiscal year 2011 DF average is 161. The results of the prior solvent analysis report did notmore » identify a specific factor that would correlate with the poor cesium decontamination beyond a low concentration of the suppressor, trioctylamine. New analyses of the quarterly sample are reported in this document, as well as a cross-check of {sup 137}Cs measurements for SRNL and F/H lab. Furthermore, in an attempt to discover the reason for the decline in DF at MCU, SRNL was tasked with analyzing numerous Caustic Wash Tank (CWT) and chemical feed samples.« less

  9. REMOVAL OF PCBS FROM A CONTAMINATED SOIL USING CF-SYSTEMS SOLVENT EXTRACTION PROCESS

    EPA Science Inventory

    The US EPA's START team in cooperation with EPA's SITE program evaluated a pilot scale solvent extraction process developed by CF-Systems. This process uses liquified propane to extract organic contaminants from soils, sludges, and sediments. A pilot-scale evaluation was conducte...

  10. RESOURCES CONSERVATIONS COMPANY - B.E.S.T. SOLVENT EXTRACTION TECHNOLOGY - APPLICATIONS ANALYSIS REPORT

    EPA Science Inventory

    This document is an evaluation of the performance of the Resources Conservation Company (RCC) Basic Extractive Sludge Treatment (B.E.S.T.®) solvent extraction technology and its applicability as a treatment technique for soils, sediments, and sludges contaminated with organics. B...

  11. Hydrometallurgical separation of rare earth elements, cobalt and nickel from spent nickel-metal-hydride batteries

    NASA Astrophysics Data System (ADS)

    Rodrigues, Luiz Eduardo Oliveira Carmo; Mansur, Marcelo Borges

    The separation of rare earth elements, cobalt and nickel from NiMH battery residues is evaluated in this paper. Analysis of the internal content of the NiMH batteries shows that nickel is the main metal present in the residue (around 50% in weight), as well as potassium (2.2-10.9%), cobalt (5.1-5.5%), rare earth elements (15.3-29.0%) and cadmium (2.8%). The presence of cadmium reveals that some Ni-Cd batteries are possibly labeled as NiMH ones. The leaching of nickel and cobalt from the NiMH battery powder with sulfuric acid is efficient; operating variables temperature and concentration of H 2O 2 has no significant effect for the conditions studied. A mixture of rare earth elements is separated by precipitation with NaOH. Finally, solvent extraction with D2EHPA (di-2-ethylhexyl phosphoric acid) followed by Cyanex 272 (bis-2,4,4-trimethylpentyl phosphinic acid) can separate cadmium, cobalt and nickel from the leach liquor. The effect of the main operating variables of both leaching and solvent extraction steps are discussed aiming to maximize metal separation for recycling purposes.

  12. Investigation of the pharmaceutical and pharmacological equivalence of different Hawthorn extracts.

    PubMed

    Vierling, W; Brand, N; Gaedcke, F; Sensch, K H; Schneider, E; Scholz, M

    2003-01-01

    Seven Hawthorn extracts were tested in isolated guinea pig aorta rings. The effect on noradrenaline- (10 microM) induced contraction was investigated. The extracts were prepared using ethanol (40 to 70% v/v), methanol (40 to 70% v/v), and water as the extraction solvents. The aqueous-alcoholic extracts displayed similar spectra of constituents. They were characterised by similar procyanidin, flavonoid, total vitexin and total phenols content and by similar TLC fingerprint chromatograms. The aqueous extract, however, showed a different fingerprint and a noticeably lower concentration of procyanidins, flavonoids and total phenols but a similar total vitexin content. All 7 extracts had a relaxant effect on the aorta precontracted by noradrenaline and led to relaxations to 44 until 29% of the initial values. The EC50 values of the aqueous-alcoholic extracts varied between 4.16 and 9.8 mg/l. The aqueous extract produced a similarly strong maximal relaxation as the other extracts, but the EC50, at 22.39 mg/l, was markedly higher. The results show that Hawthorn extracts with comparable quality profiles were obtained by using aqueous-alcoholic extraction solvents (40 to 70% ethanol or methanol). The extracts exerted comparable pharmacological effects. When using water as the extraction solvent, both, the spectrum of constituents and the pharmacological effect, deviated remarkably. It is thus possible to obtain bioequivalent extracts with comparable effect profiles by using 40 to 70% ethanol or methanol as the extraction solvent.

  13. Solvent Selection for Extraction of Neodymium Concentrates of Monazite Sand Processed Product

    NASA Astrophysics Data System (ADS)

    Setyadji, Moch; Purwani, MV

    2018-02-01

    The extraction of neodymium concentrates of monazite sand processed product has been done. The objective of this investigation was to determine the best solvent to separate Nd from Nd concentrate. As an aqueous phase was Nd(OH)3 concentrated in HNO3 and as solvent or the organic phase was trioctylamine (TOA). tryibuthyl phosphate (TBP). trioctylphosphine oxyde (TOPO) and di-ethyl hexyl phosphoric acid (D2EHPA) in kerosene. The investigated variables were HNO3 concentration. feed concentration. solvent concentration or solvent in kerosene. time and stirring speeds. From the investigation on the selection of solvent for the extraction of Nd(OH)3 concentrate with various solvents. it was concluded that the extraction of Nd could be carried out by using TBP or TOA. Extraction of Nd using TOA at the optimum HNO3 concentration of 2M. feed concentration of 5 gram/10 mL. TOA in kerosene concentration of 6 %. stirring time of 15 minutes. stirring speed of 200 rpm was chosen if the Y concentration in Nd concentrate is small. In these condition DNd obtained was 0.65; extraction efficiency of Nd (ENd)=37.10%. the concentrations of Nd2(C2O4)3 = 67.14%. Ce2(C2O4)3 = 1.79%. La2(C2O4)3 = 1.37% and Y2(C2O4)3 = 24.70%. Extraction of Nd using TBP at the optimum HNO3 concentration of 1M. feed concentration of 5 gram/10 m. the TBP concentration in kerosene of 15%. stirring time of 15 minutes and stirring speed of 200 rpm was chosen if the Ce concentration in Nd concentrate is small. In these condition DNd obtained was 0.20. extraction efficiency of Nd (ENd)=17%. concentration of Nd2(C2O4)3 = 70.84%. Ce2(C2O4)3=15.53%. La2(C2O4)3 = 0.00% and Y2(C2O4)3 = 8.63%.

  14. Sample Results From The Extraction, Scrub, And Strip Test For The Blended NGS Solvent

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Washington, A. L. II; Peters, T. B.

    This report summarizes the results of the extraction, scrub, and strip testing for the September 2013 sampling of the Next Generation Solvent (NGS) Blended solvent from the Modular Caustic Side-Solvent Extraction Unit (MCU) Solvent Hold Tank. MCU is in the process of transitioning from the BOBCalixC6 solvent to the NGS Blend solvent. As part of that transition, MCU has intentionally created a blended solvent to be processed using the Salt Batch program. This sample represents the first sample received from that blended solvent. There were two ESS tests performed where NGS blended solvent performance was assessed using either the Tankmore » 21 material utilized in the Salt Batch 7 analyses or a simulant waste material used in the V-5/V-10 contactor testing. This report tabulates the temperature corrected cesium distribution, or D Cs values, step recovery percentage, and actual temperatures recorded during the experiment. This report also identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. The calculated extraction D Cs values using the Tank 21H material and simulant are 59.4 and 53.8, respectively. The DCs values for two scrub and three strip processes for the Tank 21 material are 4.58, 2.91, 0.00184, 0.0252, and 0.00575, respectively. The D-values for two scrub and three strip processes for the simulant are 3.47, 2.18, 0.00468, 0.00057, and 0.00572, respectively. These values are similar to previous measurements of Salt Batch 7 feed with lab-prepared blended solvent. These numbers are considered compatible to allow simulant testing to be completed in place of actual waste due to the limited availability of feed material.« less

  15. Optimization of extraction conditions of some polyphenolic compounds from parsley leaves (Petroselinum crispum).

    PubMed

    Kuźma, Paula; Drużyńska, Beata; Obiedziński, Mieczysław

    2014-01-01

    Parsley leaf is a rich source of natural antioxidants, which serve a lot of functions in human body and prevent food from oxidation processes. The aim of the study was to investigate the influence of different extraction solvents and times of extraction on natural antioxidants content. Owing to the knowledge of the properties of extracted components and solvents, as well as their interactions, it is possible to achieve a high effectiveness of active compounds recovery. Three different extraction solvents (acetone 70% in water, methanol 80% in water and distilled water) and different times of extraction (30 and 60 minutes) were used to determine the efficiency of extraction of polyphenols and catechins, antioxidant activity against free radicals DPPH and ABTS and the ability to chelate ion Fe(2+) in dried parsley leaves. Other natural antioxidants contents in parsley leaves were also determined. In this study the best extraction solvent for polyphenols was acetone 70% and for catechins was distilled water. All extracts examined displayed the antioxidative activity, but water was the best solvent in the method of assaying the activity against ABTS(•+) and Fe(2+) ions chelating capability, whereas methanol turned out to be the least effective in this respect. Opposite results were observed in the case of determining the activity against DPPH(•). The prolongation of the extraction time enhanced or decreased antiradical activity in some cases. Additionally, important biologically active compounds in parsley leaves, such as vitamin C (248.31 mg/100 g dry matter), carotenoids (31.28 mg/100 g dry matter), chlorophyll (0.185 mg/g dry matter) were also analysed.

  16. Effect of different solvents extracts and mode of action of Loktanella spp. Gb03 on toxic dinoflagellate

    NASA Astrophysics Data System (ADS)

    Hameed, Anmar; Usup, Gires; Ahmad, Asmat

    2016-11-01

    This study was aimed to evaluate the algicidal activity of Loktanella sp. Gb-03 bacterial extracts against toxic dinoflagellate, using various polar and non-polar solvents. For this purpose, six different solvent extracts were prepared (i.e. methanol, ethyl acetate, hexane, chloroform, acetonitrile and water). Ratio of 1:100 (v:v) (extract to dinoflagellate culture) of each extract was used for preliminary algicidal activity screening against toxic dinoflagellate Coolia malaynesis. Dinoflagellate cells at the stationary phase (1.0 × 103 cells/ mL) were treated with 1% (v/v) of each extract by using 24-well microplate. The plates were then incubated for 24 hours at dinoflagellate culture condition (under a light intensity of 140 µmol m-2s-1 and 12:12 hours light:dark photoperiod). The result of algicidal activity screening showed that all 6 extracts from Loktanella sp. Gb-03 had different ranges of algicidal activity against the toxic dinoflagellates. Ethyl acetate extract showed the highest activity against C. malaynesis and also other harmful dinoflagellate (Alexandrium sp. Alexandrium leei, Alexandrium affine, Alexandrium tamiyavanichi, Alexandrium tamarense, Gambierdiscus belizeanus, and Ostreopsis). This study was the first to explore the algicidal activity of Loktanella sp. Gb-03 extracts against toxic dinoflagellate with ethyl acetate as the best solvent to extract algicidal active compounds.

  17. Feasibility of Surfactant-Free Supported Emulsion Liquid Membrane Extraction

    NASA Technical Reports Server (NTRS)

    Hu, Shih-Yao B.; Li, Jin; Wiencek, John M.

    2001-01-01

    Supported emulsion liquid membrane (SELM) is an effective means to conduct liquid-liquid extraction. SELM extraction is particularly attractive for separation tasks in the microgravity environment where density difference between the solvent and the internal phase of the emulsion is inconsequential and a stable dispersion can be maintained without surfactant. In this research, dispersed two-phase flow in SELM extraction is modeled using the Lagrangian method. The results show that SELM extraction process in the microgravity environment can be simulated on earth by matching the density of the solvent and the stripping phase. Feasibility of surfactant-free SELM (SFSELM) extraction is assessed by studying the coalescence behavior of the internal phase in the absence of the surfactant. Although the contacting area between the solvent and the internal phase in SFSELM extraction is significantly less than the area provided by regular emulsion due to drop coalescence, it is comparable to the area provided by a typical hollow-fiber membrane. Thus, the stripping process is highly unlikely to become the rate-limiting step in SFSELM extraction. SFSELM remains an effective way to achieve simultaneous extraction and stripping and is able to eliminate the equilibrium limitation in the typical solvent extraction processes. The SFSELM design is similar to the supported liquid membrane design in some aspects.

  18. Interlaboratory comparison of mutagenesis testing of coal fly ash derived from differenct coal conversion technologies

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Chrisp, C.; Hobbs, C.; Clark, R.

    1979-01-01

    This experiment showed that mutagenicity of fly ash derived from different coal conversion technologies, as determined by the Ames plate incorporation test, was similar in all three laboratories. The differences in mutagenic activity of each fly ash between laboratories with different solvent extraction methods were no greater than one order of magnitude. In addition, there were much smaller, but still significant differences in mutagenic activity between laboratories when the same solvent extract of a particular fly ash was tested in each laboratory. There were also significant differences in mutagenicity of the positive control mutagen (maximum of fivefold) between laboratories. Becausemore » of this difference in Ames test sensitivity between laboratories, the influence of the solvent extraction methods on differences in mutagenicity was not clear. However, the data suggested that either there were significant differences in the degree of sensitivity of Ames tests for different complex mixtures within each laboratory, or else there were differences in mutagen extraction efficiency between different solvent extraction methods. Both Ames test sensitivity and solvent extraction may be important. Further work would be necessary to separate the contribution of these two factors. An important aspect of further work would be to separate the contribution of the innate sensitivity of substrains of Ames tester strains in each laboratory from the possible effects of differences in Ames testing methodology. This could be done by testing the same extracts of fly ash and positive control mutagens with substrains of tester strains exchanged between laboratories. This work also implies that caution should be exercised in assuming that the same solvent would have the same efficiency for extraction of mutagens from different fly ashes even within the same laboratory.« less

  19. Selective mixed-bed solid phase extraction of atrazine herbicide from environmental water samples using molecularly imprinted polymer.

    PubMed

    Zarejousheghani, Mashaalah; Fiedler, Petra; Möder, Monika; Borsdorf, Helko

    2014-11-01

    A novel approach for the selective extraction of organic target compounds from water samples has been developed using a mixed-bed solid phase extraction (mixed-bed SPE) technique. The molecularly imprinted polymer (MIP) particles are embedded in a network of silica gel to form a stable uniform porous bed. The capabilities of this method are demonstrated using atrazine as a model compound. In comparison to conventional molecularly imprinted-solid phase extraction (MISPE), the proposed mixed-bed MISPE method in combination with gas chromatography-mass spectrometry (GC-MS) analysis enables more reproducible and efficient extraction performance. After optimization of operational parameters (polymerization conditions, bed matrix ingredients, polymer to silica gel ratio, pH of the sample solution, breakthrough volume plus washing and elution conditions), improved LODs (1.34 µg L(-1) in comparison to 2.25 µg L(-1) obtained using MISPE) and limits of quantification (4.5 µg L(-1) for mixed-bed MISPE and 7.5 µg L(-1) for MISPE) were observed for the analysis of atrazine. Furthermore, the relative standard deviations (RSDs) for atrazine at concentrations between 5 and 200 µg L(-1) ranged between 1.8% and 6.3% compared to MISPE (3.5-12.1%). Additionally, the column-to-column reproducibility for the mixed-bed MISPE was significantly improved to 16.1%, compared with 53% that was observed for MISPE. Due to the reduced bed-mass sorbent and at optimized conditions, the total amount of organic solvents required for conditioning, washing and elution steps reduced from more than 25 mL for conventional MISPE to less than 2 mL for mixed-bed MISPE. Besides reduced organic solvent consumption, total sample preparation time of the mixed-bed MISPE method relative to the conventional MISPE was reduced from more than 20 min to less than 10 min. The amount of organic solvent required for complete elution diminished from 3 mL (conventional MISPE) to less than 0.4 mL with the mixed-bed technique shows its inherent potential for online operation with an analytical instrument. In order to evaluate the selectivity and matrix effects of the developed mixed-bed MISPE method, it was applied as an extraction technique for atrazine from environmental wastewater and river water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Reutilization of mango byproducts: study of the effect of extraction solvent and temperature on their antioxidant properties.

    PubMed

    Dorta, Eva; Lobo, M Gloria; Gonzalez, Monica

    2012-01-01

    Mango biowastes, obtained after processing, contain large amounts of compounds with antioxidant activity that can be reused to reduce their environmental impact. The present study evaluates the effect of solvent (methanol, ethanol, acetone, water, methanol:water [1:1], ethanol:water [1:1], and acetone:water [1:1]), and temperature (25, 50, and 75 °C) on the efficiency of the extraction of antioxidants from mango peel and seed. Among the factors optimized, extraction solvent was the most important. The solvents that best obtained extracts with high antioxidant capacity were methanol, methanol:water, ethanol:water, and acetone:water (β-carotene test, antioxidant activity coefficient 173 to 926; thiobarbituric acid reactive substances test, inhibition ratio 15% to 89%; 2,2'-azino-bis-(3-ethylbenzothiazoline)-6-sulfonic acid ABTS(·+); and 2,2-diphenyl-1-picrylhydrazyl DPPH· scavenging, 7 to 22 and 8 to 28 g trolox equivalent antioxidant capacity [TE] per 100 g mango biowaste on a dry matter basis [DW]). Similarly, the flavonoid (0.21 to 1.4 g (+)-catechin equivalents per 100 g DW), tannin (3.8 to 14 g tannic acid equivalents per 100 g DW), and proanthocyanidin (0.23 to 7.8 g leucoanthocyanidin equivalents per 100 g DW) content was highest in the peel extracts obtained with methanol, ethanol:water, or acetone:water and in the seed extracts obtained with methanol or acetone:water. From the perspective of food security, it is advisable to choose ethanol (which also has a notable antioxidant content), ethanol:water, or acetone:water, as they are all solvents that can be used in compliance with good manufacturing practice. In general, increasing temperature improves the capacity of the extracts obtained from mango peel and seed to inhibit lipid peroxidation; however, its effect on the extraction of phytochemical compounds or on the capacity of the extracts to scavenge free radicals was negligible in comparison to that of the solvent. There are many antioxidant compounds in mango peel and seed, and they could be used as a natural and very inexpensive alternative to synthetic food additives. However, the conditions in which the antioxidants are extracted must be optimized. This work proves that conditions such as extraction solvent or temperature have a crucial impact on obtaining extracts rich in antioxidants from mango biowastes. © 2011 Institute of Food Technologists®

  1. Multi-response optimisation of ultrasound-assisted extraction for recovery of flavonoids from red grape skins using response surface methodology.

    PubMed

    Tomaz, Ivana; Maslov, Luna; Stupić, Domagoj; Preiner, Darko; Ašperger, Danijela; Karoglan Kontić, Jasminka

    2016-01-01

    For the characterisation of grape cultivars, the profile and content of flavonoids are important because these compounds impact grape and wine quality. To determine the correct profile and content of flavonoids, the use of robust, sensitive and reliable methods is necessary. The object of this research is to develop a new ultrasound-assisted extraction (UAE) method for the recovery of flavonoids from grape skins using response surface methodology. Optimisation of UAE was performed using a complementary study combining a Box-Behnken experimental design with qualitative analysis by high-performance liquid chromatography. Optimal extraction conditions were obtained using the extraction solvent composed of acetonitrile:water:formic acid (26:73:1, v/v/v) at an extraction temperature of 50 °C, an extraction time of 15 min in a single-extraction step and with a solid-to-solvent ratio of 1:80 g/mL. The calculated relative standard deviations for the optimal extraction method were very low, measuring less than 5%. This study demonstrates that numerous factors have strong effects on the extraction efficiency, including the type of organic modifier and its percentage in the extraction solvent, the number of extraction steps, the solid-to-solvent ratio, the extraction time and temperature and, finally, the particular nature of analyte and their position within the grape skin cell. Copyright © 2015 John Wiley & Sons, Ltd.

  2. Solvent hold tank sample results for MCU-17-150-152 (July 2017) and MCU-17-153-155 (August 2017): Quarterly report

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F.; Jones, D.

    A trend summary that includes the last two Solvent Hold Tank (SHT) monthly samples is shown; MCU- 17-150-152 (July SHT) and MCU-17-153-155 (August SHT). Since the last SHT sample sent for analysis was the August sample the chemical state of the solvent is best approximated by the chemical analysis of the August SHT sample (MCU-17-153-155). This report mainly focused on the chemical analysis of the August SHT sample. The analysis data from the July SHT sample are presented in the “trend” plots of this report. Analysis of the August SHT sample (MCU-17-153-155) indicated that the modifier (CS-7SB) was 2% belowmore » but the extractant (MaxCalix) concentration was at its nominal recommended level (169,000 mg/L and 46,400 mg/L respectively). The suppressor (TiDG) level has decreased since the last measurement taken while the Modular Caustic-Side Solvent Extraction unit (MCU) was operating in January 2017, but has remained steady in the range of 666 (observed in April) to 715 mg/L (observed in the August 2017 sample) since February 2017, well above the minimum recommended level (479 mg/L), but below the nominal level. The “flat” trends observed in the TiDG, MaxCalix, modifier, and Gamma measurement are consistent with the solvent being idle since January 10, 2017. A strong correlation between density and modifier concentration in the solvent continues to be observed in the SHT samples. This analysis confirms the Isopar™L addition to the solvent in January 2017. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time if the Modular Caustic-Side Solvent Extraction Unit (MCU) returns to processing radioactive liquid waste. Otherwise, the levels of these components will remain steady. A future Isopar™L trimming addition to the solvent is recommended when MCU resumes processing waste. Two unknown impurities related to the modifier (but not sec-butyl phenol: a modifier degradation product observed before) at the 290 and 110 mg/L levels were observed in the August SHT sample by the Gas - Chromatography-Mass Spectrometry (GC-MS) method. They were observed in a second GC-MS re-run with a new column. Their identification can’t be ascertained at this time. No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). Another impurity observed in the samples was mercury. Based on the August SHT sample, up to 23 ± 5 micrograms of mercury per mL of solvent was detected (the average of the Cold Vapor-Atomic Adsorption [CV-AA] and X-Ray Fluorescence [XRF] methods). The higher mercury concentration in the solvent (as determined in the last three-monthly samples) is possibly due to either a higher mercury concentration in Salt Batches 8 and 9 (Tank 49H) . The gamma level (~ 2.0E4 dpm/mL) measured in the August SHT samples was one order of magnitude lower than the gamma levels observed in the December 2016 and January 2017 SHT samples. A similar level was observed in the July SHT sample (MCU-SHT-150-152). The gamma level has remained consistently steady since January 10, 2017 when MCU stopped processing radioactive liquid waste. The laboratory will continue to monitor the quality of the solvent in particularly for any new impurities or degradation of the solvent components.« less

  3. Supercritical fluid technology: concepts and pharmaceutical applications.

    PubMed

    Deshpande, Praful Balavant; Kumar, G Aravind; Kumar, Averineni Ranjith; Shavi, Gopal Venkatesh; Karthik, Arumugam; Reddy, Meka Sreenivasa; Udupa, Nayanabhirama

    2011-01-01

    In light of environmental apprehension, supercritical fluid technology (SFT) exhibits excellent opportunities to accomplish key objectives in the drug delivery sector. Supercritical fluid extraction using carbon dioxide (CO(2)) has been recognized as a green technology. It is a clean and versatile solvent with gas-like diffusivity and liquid-like density in the supercritical phase, which has provided an excellent alternative to the use of chemical solvents. The present commentary provides an overview of different techniques using supercritical fluids and their future opportunity for the drug delivery industry. Some of the emerging applications of SFT in pharmaceuticals, such as particle design, drug solubilization, inclusion complex, polymer impregnation, polymorphism, drug extraction process, and analysis, are also covered in this review. The data collection methods are based on the recent literature related to drug delivery systems using SFT platforms. SFT has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This cutting-edge technology is growing predominantly to surrogate conventional unit operations in relevance to the pharmaceutical production process. Supercritical fluid technology has recently drawn attention in the field of pharmaceuticals. It is a distinct conception that utilizes the solvent properties of supercritical fluids above their critical temperature and pressure, where they exhibit both liquid-like and gas-like properties, which can enable many pharmaceutical applications. For example, the liquid-like properties provide benefits in extraction processes of organic solvents or impurities, drug solubilization, and polymer plasticization, and the gas-like features facilitate mass transfer processes. It has become a much more versatile and environmentally attractive technology that can handle a variety of complicated problems in pharmaceuticals. This review is focused on different techniques that use supercritical fluids and their opportunities for the pharmaceutical sector.

  4. Optimization of extraction of polysaccharides from fruiting body of Cordyceps militaris (L.) link using response surface methodology

    NASA Astrophysics Data System (ADS)

    Nguyen, Hoang Chinh; Thi, Dinh Huynh Mong; Pham, Dinh Chuong

    2018-04-01

    Polysaccharides from fruiting body of Cordyceps militaris (L.) Link possess various pharmaceutical activities. In this study, polysaccharides from the fruiting body of C. militaris were extracted with different solvents. Of those solvents tested, distilled water was identified as the most efficient solvent for the extraction, resulting in a significant increase in polysaccharides yield. Response surface methodology was then used to optimize the extraction conditions and establish a reliable mathematical model for prediction. A maximum polysaccharides yield of 11.07% was reached at a ratio of water to raw material of 23.2:1 mL/g, an extraction time of 76 min, and a temperature of 93.6°C. This study indicates that the obtained optimal extraction conditions are an efficient method for extraction of polysaccharides from the fruiting body of C. militaris.

  5. Evaluation of different solvent mixtures in esterifiable lipids extraction from microalgae Botryococcus braunii for biodiesel production.

    PubMed

    Hidalgo, Pamela; Ciudad, Gustavo; Navia, Rodrigo

    2016-02-01

    Non-polar and polar solvents as well as their mixtures were tested for the extraction of microalgae lipids and thus, to evaluate their effect on total and esterifiable lipids extraction yields with potential to be converted to biodiesel. The obtained results show an increase in lipids and esterifiable lipids extraction yields when non-polar and polar solvent mixtures were used. The higher esterifiable lipids extraction yield was 19.2%wt (based on dry biomass) using a chloroform-methanol mixture (75%v/v of methanol), corresponding to a 98.9%wt esterifiable lipids extraction. In addition, esterifiable lipids extraction yield of 18.9%wt (based on dry biomass) was obtained when a petroleum ether-methanol mixture (75%v/v of methanol) was used, corresponding to a 96.9%wt esterifiable lipids extraction. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. Assessing the Impact of Chlorinated-Solvent Sites on Metropolitan Groundwater Resources

    PubMed Central

    Brusseau, Mark L.; Narter, Matthew

    2014-01-01

    Chlorinated-solvent compounds are among the most common groundwater contaminants in the U.S.A. The majority of the many sites contaminated by chlorinated-solvent compounds are located in metropolitan areas, and most such areas have one or more chlorinated-solvent contaminated sites. Thus, contamination of groundwater by chlorinated-solvent compounds may pose a potential risk to the sustainability of potable water supplies for many metropolitan areas. The impact of chlorinated-solvent sites on metropolitan water resources was assessed for Tucson, AZ, by comparing the aggregate volume of extracted groundwater for all pump-and-treat systems associated with contaminated sites in the region to the total regional groundwater withdrawal. The analysis revealed that the aggregate volume of groundwater withdrawn for the pump-and-treat systems operating in Tucson, all of which are located at chlorinated-solvent contaminated sites, was 20% of the total groundwater withdrawal in the city for the study period. The treated groundwater was used primarily for direct delivery to local water supply systems or for reinjection as part of the pump-and-treat system. The volume of the treated groundwater used for potable water represented approximately 13% of the total potable water supply sourced from groundwater, and approximately 6% of the total potable water supply. This case study illustrates the significant impact chlorinated-solvent contaminated sites can have on groundwater resources and regional potable-water supplies. PMID:24116872

  7. Solvent Hold Tank Sample Results For MCU-15-750-751-752-: June Monthly Sample

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F.; Taylor-Pashow, K.

    2015-10-07

    Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-750, MCU-15-751, and MCU-15-752), pulled on 06/22/2015 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-750-751-752 indicated a low concentration (~ 49 % of nominal) of the suppressor (TiDG) and slightly lower than nominal concentrations of the extractant (MaxCalix), and of the modifier (Cs-7SB) in the solvent. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent in February 2015. Based on the current monthly sample, the levels of TiDG, MaxCalix, and modifier are sufficient formore » continuing operation without adding a trim at this time but it is recommended that an addition of TiDG, modifier and Isopar™L should be made in the near future. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). In addition, up to 13.9 micrograms of mercury per gram of solvent (or 11.5 µg/mL) was detected in this sample. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

  8. Comparison of ambient solvent extraction methods for the analysis of fatty acids in non-starch lipids of flour and starch

    PubMed Central

    Bahrami, Niloufar; Yonekura, Lina; Linforth, Robert; Carvalho da Silva, Margarida; Hill, Sandra; Penson, Simon; Chope, Gemma; Fisk, Ian Denis

    2014-01-01

    BACKGROUND Lipids are minor components of flours, but are major determinants of baking properties and end-product quality. To the best of our knowledge, there is no single solvent system currently known that efficiently extracts all non-starch lipids from all flours without the risk of chemical, mechanical or thermal damage. This paper compares nine ambient solvent systems (monophasic and biphasic) with varying polarities: Bligh and Dyer (BD); modified Bligh and Dyer using HCl (BDHCL); modified BD using NaCl (BDNaCl); methanol–chloroform–hexane (3:2:1, v/v); Hara and Radin (hexane–isopropanol, 3:2, v/v); water-saturated n-butanol; chloroform; methanol and hexane for their ability to extract total non-starch lipids (separated by lipid classes) from wheat flour (Triticum aestivum L.). Seven ambient extraction protocols were further compared for their ability to extract total non-starch lipids from three alternative samples: barley flour (Hordeum vulgare L.), maize starch (Zea mays L.) and tapioca starch (Manihot esculenta Crantz). RESULTS For wheat flour the original BD method and those containing HCl or NaCl tended to extract the maximum lipid and a significant correlation between lipid extraction yield (especially the glycolipids and phospholipids) and the polarity of the solvent was observed. For the wider range of samples BD and BD HCl repeatedly offered the maximum extraction yield and using pooled standardized (by sample) data from all flours, total non-starch lipid extraction yield was positively correlated with solvent polarity (r = 0.5682, P < 0.05) and water ratio in the solvent mixture (r = 0.5299, P < 0.05). CONCLUSION In general, BD-based methods showed better extraction yields compared to methods without the addition of water and, most interestingly, there was much greater method dependence of lipid yields in the starches when compared to the flour samples, which is due to the differences in lipid profiles between the two sample types (flours and starches). PMID:24132804

  9. Enantioseparation of Racemic Flurbiprofen by Aqueous Two-Phase Extraction With Binary Chiral Selectors of L-dioctyl Tartrate and L-tryptophan.

    PubMed

    Chen, Zhi; Zhang, Wei; Wang, Liping; Fan, Huajun; Wan, Qiang; Wu, Xuehao; Tang, Xunyou; Tang, James Z

    2015-09-01

    A novel method for chiral separation of flurbiprofen enantiomers was developed using aqueous two-phase extraction (ATPE) coupled with biphasic recognition chiral extraction (BRCE). An aqueous two-phase system (ATPS) was used as an extracting solvent which was composed of ethanol (35.0% w/w) and ammonium sulfate (18.0% w/w). The chiral selectors in ATPS for BRCE consideration were L-dioctyl tartrate and L-tryptophan, which were screened from amino acids, β-cyclodextrin derivatives, and L-tartrate esters. Factors such as the amounts of L-dioctyl tartrate and L-tryptophan, pH, flurbiprofen concentration, and the operation temperature were investigated in terms of chiral separation of flurbiprofen enantiomers. The optimum conditions were as follows: L-dioctyl tartrate, 80 mg; L-tryptophan, 40 mg; pH, 4.0; flurbiprofen concentration, 0.10 mmol/L; and temperature, 25 °C. The maximum separation factor α for flurbiprofen enantiomers could reach 2.34. The mechanism of chiral separation of flurbiprofen enantiomers is discussed and studied. The results showed that synergistic extraction has been established by L-dioctyl tartrate and L-tryptophan, which enantioselectively recognized R- and S-enantiomers in top and bottom phases, respectively. Compared to conventional liquid-liquid extraction, ATPE coupled with BRCE possessed higher separation efficiency and enantioselectivity without the use of any other organic solvents. The proposed method is a potential and powerful alternative to conventional extraction for separation of various enantiomers. © 2015 Wiley Periodicals, Inc.

  10. Fluoro-alcohol phase modifiers and process for cesium solvent extraction

    DOEpatents

    Bonnesen, Peter V.; Moyer, Bruce A.; Sachleben, Richard A.

    2003-05-20

    The invention relates to a class of phenoxy fluoro-alcohols, their preparation, and their use as phase modifiers and solvating agents in a solvent composition for the extraction of cesium from alkaline solutions. These phenoxy fluoro-alcohols comply with the formula: ##STR1## in which n=2 to 4; X represents a hydrogen or a fluorine atom, and R.sup.2 -R.sup.6 are hydrogen or alkyl substituents. These phenoxy fluoro-alcohol phase modifiers are a necessary component to a robust solvent composition and process useful for the removal of radioactive cesium from alkaline nuclear waste streams. The fluoro-alcohols can also be used in solvents designed to extract other cesium from acidic or neutral solutions.

  11. Alcohol based-deep eutectic solvent (DES) as an alternative green additive to increase rotenone yield

    NASA Astrophysics Data System (ADS)

    Othman, Zetty Shafiqa; Hassan, Nur Hasyareeda; Zubairi, Saiful Irwan

    2015-09-01

    Deep eutectic solvents (DESs) are basically molten salts that interact by forming hydrogen bonds between two added components at a ratio where eutectic point reaches a melting point lower than that of each individual component. Their remarkable physicochemical properties (similar to ionic liquids) with remarkable green properties, low cost and easy handling make them a growing interest in many fields of research. Therefore, the objective of pursuing this study is to analyze the potential of alcohol-based DES as an extraction medium for rotenone extraction from Derris elliptica roots. DES was prepared by a combination of choline chloride, ChCl and 1, 4-butanediol at a ratio of 1/5. The structure of elucidation of DES was analyzed using FTIR, 1H-NMR and 13C-NMR. Normal soaking extraction (NSE) method was carried out for 14 hours using seven different types of solvent systems of (1) acetone; (2) methanol; (3) acetonitrile; (4) DES; (5) DES + methanol; (6) DES + acetonitrile; and (7) [BMIM] OTf + acetone. Next, the yield of rotenone, % (w/w), and its concentration (mg/ml) in dried roots were quantitatively determined by means of RP-HPLC. The results showed that a binary solvent system of [BMIM] OTf + acetone and DES + acetonitrile was the best solvent system combination as compared to other solvent systems. It contributed to the highest rotenone content of 0.84 ± 0.05% (w/w) (1.09 ± 0.06 mg/ml) and 0.84 ± 0.02% (w/w) (1.03 ± 0.01 mg/ml) after 14 hours of exhaustive extraction time. In conclusion, a combination of the DES with a selective organic solvent has been proven to have a similar potential and efficiency as of ILs in extracting bioactive constituents in the phytochemical extraction process.

  12. METHOD FOR DISSOLVING ZIRCONIUM-URANIUM COMPOSITIONS

    DOEpatents

    Gens, T.A.

    1961-07-18

    A method is descrioed for treating a zirconium-- uranium composition to form a stable solution from which uranium and other values may be extracted by contacting the composition with at least a 4 molar aqueous solution of ammonium fluoride at a temperature of about 100 deg C, adding a peroxide, in incremental amounts, to the heated solution throughout the period of dissolution until all of the uranium is converted to soluble uranyl salt, adding nitric acid to the resultant solution to form a solvent extraction feed solution to convert the uranyl salt to a solvent extractable state, and thereafter recovering the uranium and other desired values from the feed solution by solvent extraction.

  13. Study of process variables in supercritical carbon dioxide extraction of soybeans.

    PubMed

    Wilkinson, Nikolas; Hilton, Ramsey; Hendry, Doug; Venkitasamy, Chandrasekar; Jacoby, William

    2014-01-01

    Soybean flakes were extracted using supercritical carbon dioxide at 48.3 MPa and 80 °C, which is a higher temperature than previously reported. Several operational parameters were explored to determine their effect on extractions. Flakes, as typically used in this industry, provided the best extraction performance. Particle size distributions were created through grinding. Reducing average particle diameters smaller than 0.069 mm had no appreciable effect on increasing extraction efficiencies. Exploration of flow rate indicated that a residence time of less than 60 s for the supercritical carbon dioxide would be sufficient for complete extractions. A solvent mass to load mass ratio of 10:1 was found to be sufficient for extraction of oils from soybean flakes. Increasing moisture in the soybeans led to decreasing extraction efficiency of oils. Finally, soybean hulls had no effect on extraction efficiency. Thus, the de-hulling procedure can be removed from the extraction process without decreasing extraction efficiency.

  14. Vegetable Oils as Alternative Solvents for Green Oleo-Extraction, Purification and Formulation of Food and Natural Products.

    PubMed

    Yara-Varón, Edinson; Li, Ying; Balcells, Mercè; Canela-Garayoa, Ramon; Fabiano-Tixier, Anne-Sylvie; Chemat, Farid

    2017-09-05

    Since solvents of petroleum origin are now strictly regulated worldwide, there is a growing demand for using greener, bio-based and renewable solvents for extraction, purification and formulation of natural and food products. The ideal alternative solvents are non-volatile organic compounds (VOCs) that have high dissolving power and flash point, together with low toxicity and less environmental impact. They should be obtained from renewable resources at a reasonable price and be easy to recycle. Based on the principles of Green Chemistry and Green Engineering, vegetable oils could become an ideal alternative solvent to extract compounds for purification, enrichment, or even pollution remediation. This review presents an overview of vegetable oils as solvents enriched with various bioactive compounds from natural resources, as well as the relationship between dissolving power of non-polar and polar bioactive components with the function of fatty acids and/or lipid classes in vegetable oils, and other minor components. A focus on simulation of solvent-solute interactions and a discussion of polar paradox theory propose a mechanism explaining the phenomena of dissolving polar and non-polar bioactive components in vegetable oils as green solvents with variable polarity.

  15. Investigating the effect of various extracting solvents on the potential use of red-apple skin (Malus domestica) as natural sensitizer for dye-sensitized solar cell

    NASA Astrophysics Data System (ADS)

    Saputro, Aldhi; Mizan, Adlan; Sofyan, Nofrijon; Yuwono, Akhmad Herman

    2017-03-01

    In the current investigation, the natural dye extracted from red-apple (Malus domestica) skin was used as natural sensitizer for dye sensitized solar cell (DSSC) application. The present study was specifically aimed at observing the effect of different solvents, i.e. deionized water, ethanol, and acidified ethanol, on the performance of the natural dye and thus the DSSC. For synthesis purposes, red-apple skin was peeled off, dried, crushed and furthermore extracted with ratio red-apple skin powder to solvent 1:20 w/v for 2 hours at 50°C under mechanical stirring. Subsequently, the resulting natural dyes with different solvents were examined by Fourier transform infrared (FTIR) to analyze their functional groups, UV-Vis spectroscopy to observe their absorption spectra for a wide range of wavelength, while TiO2 nanoparticle used as the semiconductor oxide layer in the device was characterized by field emission scanning electron microscope (FESEM). The FTIR results showed that the red-apple skin has anthocyanin group which functions as the sensitizer agent for photon energy absorption from the sunlight. The UV-Vis spectroscopy results showed that ethanol solvent has higher absorption of sunlight wavelength as compared to those of deionized water and acidified ethanol solvents. The performance test of the fabricated DSSC showed the prototype made of the red apple skin dye extracted by ethanol solvent can provide the highest open circuit voltage (Voc) up to 324 mV and efficiency around 0.046%. On the basis of investigation, it has been found that ethanol was the best solvent to extract anthocyanin from the red-apple skin.

  16. U-EXTRACTION--IMPROVEMENTS IN ELIMINATION OF Mo BY USE OF FERRIC ION

    DOEpatents

    Clark, H.M.; Duffey, D.

    1958-06-10

    An improved solvent extraction process is described whereby U may be extracted by a water immiscible organic solvent from an aqueous solution of uranyl nitrate. It has been found that Mo in the presence of phosphate ions appears to form a complex with the phosphate which extracts along with the U. This extraction of Mo may be suppressed by providing ferric ion in the solution prior to the extraction step. The ferric ion is preferably provided in the form of ferric nitrate.

  17. Immunomodulatory activities of different solvent extracts from Tricholoma matsutake (S. Ito et S. Imai) singer (higher basidiomycetes) on normal mice.

    PubMed

    Yin, Xiulian; You, Qinghong; Jiang, Zhonghai

    2012-01-01

    The immunomodulatory activities of different solvent extracts from the culinary-medicinal mushroom Tricholoma matsutake were studied in vivo in normal mice. The extracts were prepared using different solvents in an order of increasing polarity. The immunomodulatory activities were investigated by measuring the thymus and spleen index, phagocytic rate of macrophage phagocytosis, delayed-type hypersensitivity, plaque-forming cell, and proliferation of splenocytes. Results demonstrated that water extract (WE) and n-butyl alcohol extract (BAE) of T. matsutake could enhance the immunity of mice significantly compared with the control group. Main components of WE and BAE were polysaccharides, proteins, and flavonoids; we presume that these may be the main immunomodulating and immuno-enhancing agents in T. matsutake.

  18. Fundamental studies on the feasibility of deep eutectic solvents for the selective partition of glaucarubinone present in the roots of Simarouba glauca.

    PubMed

    Kholiya, Faisal; Bhatt, Nidhi; Rathod, Meena R; Meena, Ramavatar; Prasad, Kamalesh

    2015-07-14

    Several deep eutectic solvents prepared by the complexation of choline chloride as the hydrogen bond acceptor and hydrogen bond donors such as urea, thiourea, ethylene glycol, and glycerol were employed to partition glaucarubinone, an antimalarial compound present in roots of the plant, Simarouba glauca. Among all the solvents, the deep eutectic solvent consisting of the mixture of choline chloride and urea the most suitable to partition the antimalarial compound from the extract selectively. Analytical tools such as high-performance liquid chromatography and electrospray ionization mass spectrometry were used for characterizations, and glaucarubinone extracted from the roots of the plant by conventional solvent extraction method was used as a reference for comparison. The hydrogen and noncovalent bonds formed between glaucarubinone and the deep eutectic solvents could be responsible for the selective partition of the drug molecule. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Effect of HEH[EHP] impurities on the ALSEP solvent extraction process

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Holfeltz, Vanessa E.; Campbell, Emily L.; Peterman, Dean R.

    In solvent extraction processes, organic phase impurities can negatively impact separation factors, hydrolytic performance, and overall system robustness. This affects the process-level viability of a separation concept and necessitates knowledge of the behavior and mechanisms to control impurities in the solvent. The most widespread way through which impurities are introduced into a system is through impure extractants and/or diluents used to prepare the solvent, and often development of new purification schemes to achieve the desired level of purity is needed. In this work, the acidic extractant, 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (HEH[EHP])—proposed for application in extractive processes aimed at separating trivalentmore » minor actinides from lanthanides and other fission products—is characterized with respect to its common impurities and their impact on Am(III) stripping in the Actinide Lanthanide SEParation (ALSEP) system. To control impurities in HEH[EHP], existing purification technologies commonly applied for the acidic organophosphorus reagents are reviewed, and a new method specific to HEH[EHP] purification is presented.« less

  20. Supercritical-Fluid Extraction of Oil From Tar Sands

    NASA Technical Reports Server (NTRS)

    Compton, L. E.

    1982-01-01

    New supercritical solvent mixtures have been laboratory-tested for extraction of oil from tar sands. Mixture is circulated through sand at high pressure and at a temperature above critical point, dissolving organic matter into the compressed gas. Extract is recovered from sand residues. Low-temperature super-critical solvents reduce energy consumption and waste-disposal problems.

  1. Spectroscopic, calorimetric and structural analyses of the effects of hydrothermal treatment of rice beans and the extraction solvent on starch characteristics.

    PubMed

    González-Cruz, Leopoldo; Montañez-Soto, José Luis; Conde-Barajas, Eloy; Negrete-Rodríguez, María de la Luz Xochilt; Flores-Morales, Areli; Bernardino-Nicanor, Aurea

    2018-02-01

    The modification of the starches extracted from rice beans both with and without hydrothermal treatment was evaluated via scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and Fourier transform infrared (FT-IR) and Raman spectroscopy. SEM indicated that the starch granules of rice beans exhibit wide variation in granule shape, showing the greatest size and modification of the surface when extracted with ethanol. It was found that the extraction solvent had no significant effect on the onset (T o ) and peak (T p ) temperatures of the starch, whereas hydrothermal treatment of rice beans decreased the T o , T p and ΔH of the starch. The modification of FT-IR spectra showed that hydrothermal treatment of rice beans and the solvent used in the extraction of starch affected starch crystallinity, mainly when ethanol was used. Raman spectroscopy revealed that the smaller changes in the starch bonds were due to the solvent used for starch extraction but that hydrothermal treatment disturbed all bonds in the starch. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Dispersive liquid-liquid microextraction based on the solidification of floating organic droplet for the determination of polychlorinated biphenyls in aqueous samples.

    PubMed

    Dai, Liping; Cheng, Jing; Matsadiq, Guzalnur; Liu, Lu; Li, Jun-Kai

    2010-08-03

    In the proposed method, an extraction solvent with a lower toxicity and density than the solvents typically used in dispersive liquid-liquid microextraction was used to extract seven polychlorinated biphenyls (PCBs) from aqueous samples. Due to the density and melting point of the extraction solvent, the extract which forms a layer on top of aqueous sample can be collected by solidifying it at low temperatures, which form a layer on top of the aqueous sample. Furthermore, the solidified phase can be easily removed from the aqueous phase. Based on preliminary studies, 1-undecanol was selected as the extraction solvent, and a series of parameters that affect the extraction efficiency were systematically investigated. Under the optimized conditions, enrichment factors for PCBs ranged between 494 and 606. Based on a signal-to-noise ratio of 3, the limit of detection for the method ranged between 3.3 and 5.4 ng L(-1). Good linearity, reproducibility and recovery were also obtained. 2010 Elsevier B.V. All rights reserved.

  3. Comparison of magnesium sulfate and sodium sulfate for removal of water from pesticide extracts of foods.

    PubMed

    Schenck, Frank J; Callery, Patrick; Gannett, Peter M; Daft, Jonathan R; Lehotay, Steven J

    2002-01-01

    Water-miscible solvents, such as acetone and acetonitrile, effectively extract both polar and nonpolar pesticide residues from nonfatty foods. The addition of sodium chloride to the resulting acetonitrile-water or acetone-water extract (salting out) results in the separation of the water from the organic solvent. However, the organic solvent layer (pesticide extract) still contains some residual water, which can adversely affect separation procedures that follow, such as solid-phase extraction and/or gas chromatography. Drying agents, such as sodium sulfate or magnesium sulfate, are used to remove the water from the organic extracts. In the present study, we used nuclear magnetic resonance spectroscopy to study the composition of the phases resulting from salting out and to compare the effectiveness of sodium sulfate and magnesium sulfate as drying agents. The study showed that considerable amounts of water remained in the organic phase after phase separation. Sodium sulfate was a relatively ineffective drying agent, removing little or no residual water from the organic solvent. Magnesium sulfate proved to be a much more effective drying agent.

  4. Deterred drug abuse using superabsorbent polymers.

    PubMed

    Mastropietro, David J; Muppalaneni, Srinath; Omidian, Hossein

    2016-11-01

    This study aimed to determine whether selected superabsorbent polymers (SAPs) could be used as a suitable alternative to thwart extraction, filtration, and syringeability attempts for abuse. Many abuse-deterrent formulations (ADFs) rely on high molecular weight polymers such as poly(ethylene oxide) to provide crush and extraction resistance. However, these polymers suffer from slow dissolution kinetics, and are susceptible to a variety of abuse conditions. Several commercially available SAPs were evaluated for swelling behavior in extraction solvents, and tableting properties. Post-compaction abuse properties were evaluated by recoverable volume and syringeability after solvent extraction. Drug release and percent drug extraction were conducted using tramadol HCl as a model drug. Certain SAPs had the ability to rapidly imbibe solvent and effectively stop extraction processes in a variety of solvents, including water and water/alcohol mixtures. Tablets containing SAP and drug showed no effect on drug release in vitro. SAPs possess adequate properties for tableting, and maintain their high and fast swelling properties after compaction. The fast and extensive interactions of SAPs with aqueous medium are a major advantage over non-crosslinked high molecular weight viscosifying agents such as poly(ethylene oxide).

  5. Gradient x Isocratic Elution CCC on the Isolation of Verbascoside and Other Phenylethanoids: Influence of the Complexity of the Matrix.

    PubMed

    Leitão, Gilda Guimarães; Pinto, Shaft Correa; de Oliveira, Danilo Ribeiro; Timoteo, Patrícia; Guimarães, Michelle Guedes; Cordova, Wilmer H Perera; Leitão, Suzana Guimarães

    2015-11-01

    Verbascoside is a phenylethanoid glycoside widely distributed in nature, especially among the order Lamiales, occurring in numerous plants that are constituents of folk medicine preparations. This natural compound, previously isolated by our group from the ethyl acetate extract of Lantana trifolia using the gradient approach in countercurrent chromatography, was now isolated from the butanol extract of the same plant and from Lippia alba f. intermedia (Verbenaceae) using countercurrent chromatography in either gradient or isocratic elution modes. The ethyl acetate extract of L. alba, rich in phenylethanoids and flavonoids, was fractionated using countercurrent chromatography in the step-gradient elution approach. The four-step solvent system was composed of n-hexane-ethyl acetate-n-butanol-water (4 : 10 : X : 10), where X = 1 (solvent system A), 3 (solvent system B), 5 (solvent system C), and 7 (solvent system D), and allowed for the isolation of verbascoside along with other phenylethanoids and flavonoids from both plants. Verbascoside and 2'-O-β-apiosylverbascoside were further isolated from the n-butanol extract of L. trifolia using the solvent system ethyl acetate-n-butanol-water 10 : 2 : 10 on an isocratic run. The difference in the complexity of the two plant extracts demanded different purification steps, which included a second high-speed countercurrent chromatography purification using the isocratic elution mode. Georg Thieme Verlag KG Stuttgart · New York.

  6. Effects of processing parameters in the sonic assisted water extraction (SAWE) of 6-gingerol.

    PubMed

    Syed Jaapar, Syaripah Zaimah; Morad, Noor Azian; Iwai, Yoshio; Nordin, Mariam Firdhaus Mad

    2017-09-01

    The use of water in subcritical conditions for extraction has several drawbacks. These include the safety features, higher production costs and possible degradation of the bioactive compounds. To overcome these problems, sonic energy and an entrainer were used as external interventions to decrease the polarity of water at milder operating conditions. The effect of low (28kHz) and high (800kHz) frequencies of sonication in the extraction of the main ginger bioactive compound (6-gingerol) were compared. Six parameters were studied: mean particle size (MPS, mm), time of extraction, applied power, sample to solvent ratio (w/v), temperature of extraction, and the percentage of entrainer. The optimum conditions for high frequency SAWE prototype were MPS 0.89-1.77mm, 45min, 40W applied power, 1:30 (w/v), 45°C, and 15% of ethanol as entrainer. Two-way analysis of variance (ANOVA) gave the most significant parameter, which was power with F (1, 45.07), p<2.50×10 -9 . Although the effect of low frequency was stronger than high frequency, at the optimum conditions of the sample to solvent ratio 1:30 (w/v) with 700mL solvent and temperature 45°C, the concentration and recovery of 6-gingerol from high frequency of SAWE prototype was 2.69 times higher than at low frequency of SAWE. It was found that although the effects of high frequency (800kHz) were negligible in other studies, it could extract suitable compounds, such as 6-gingerol, at lower temperature. Therefore, the effects of sonication, which cause an enlargement in the cell wall of the ginger plant matrix, were observed using a Scanning Electron Microscope (SEM). It was found that the applied power of sonication was the most significant parameter compared to the other parameters. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. [Extraction of lambda-cyhalothrin from aqueous dioxan solutions].

    PubMed

    Shormanov, V K; Chigareva, E N; Belousova, O V

    2011-01-01

    The results of extraction of lambda-cigalotrin from dioxan aqueous solutions by hydrophobic organic solvents are presented. It is shown that the degree of extraction depends on the nature of the extractant, the water to dioxan ratio, and saturation of the water-dioxan layer with the electrolyte. The highest efficiency of lambda-cigalotrin extraction was achieved using chlorophorm as a solvent under desalination conditions. The extraction factor was calculated necessary to obtain the desired amount of lambda-cigalotrin from the water-dioxan solution (4:1) with the help of the extractants being used.

  8. Isolation and characterization of hydrophobic compounds from carbohydrate matrix of Pistacia atlantica.

    PubMed

    Samavati, Vahid; Adeli, Mostafa

    2014-01-30

    The present work is focused on the optimization of hydrophobic compounds extraction process from the carbohydrate matrix of Iranian Pistacia atlantica seed at laboratory level using ultrasonic-assisted extraction. Response surface methodology (RSM) was used to optimize oil seed extraction yield. Independent variables were extraction temperature (30, 45, 60, 75 and 90°C), extraction time (10, 15, 20, 25, 30 and 35 min) and power of ultrasonic (20, 40, 60, 80 and 100 W). A second order polynomial equation was used to express the oil extraction yield as a function of independent variables. The responses and variables were fitted well to each other by multiple regressions. The optimum extraction conditions were as follows: extraction temperature of 75°C, extraction time of 25 min, and power of ultrasonic of 80 W. A comparison between seed oil composition extracted by ultrasonic waves under the optimum operating conditions determined by RSM for oil yield and by organic solvent was reported. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Extraction of metals using supercritical fluid and chelate forming legand

    DOEpatents

    Wai, Chien M.; Laintz, Kenneth E.

    1998-01-01

    A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated .beta.-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated .beta.-diketone and a trialkyl phosphate, or a fluorinated .beta.-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated .beta.-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

  10. Extraction of metals using supercritical fluid and chelate forming ligand

    DOEpatents

    Wai, C.M.; Laintz, K.E.

    1998-03-24

    A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated {beta}-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated {beta}-diketone and a trialkyl phosphate, or a fluorinated {beta}-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated {beta}-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process. 7 figs.

  11. Solvent Extraction Separation of Trivalent Americium from Curium and the Lanthanides

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Jensen, Mark P.; Chiarizia, Renato; Ulicki, Joseph S.

    2015-02-27

    The sterically constrained, macrocyclic, aqueous soluble ligand N,N'-bis[(6-carboxy-2-pyridyl)methyl]-1,10-diaza-18-crown-6 (H2BP18C6) was investigated for separating americium from curium and all the lanthanides by solvent extraction. Pairing H2BP18C6, which favors complexation of larger f-element cations, with acidic organophosphorus extractants that favor extraction of smaller f-element cations, such as bis-(2-ethylhexyl)phosphoric acid (HDEHP) or (2-ethylhexyl)phosphonic acid mono(2-ethylhexyl) ester (HEH[EHP]), created solvent extraction systems with good Cm/Am selectivity, excellent trans-lanthanide selectivity (Kex,Lu/Kex,La = 108), but poor selectivity for Am against the lightest lanthanides. However, using an organic phase containing both a neutral extractant, N,N,N’,N’-tetra(2-ethylhexyl)diglycolamide (TEHDGA), and HEH[EHP] enabled rejection of the lightest lanthanides during loading ofmore » the organic phase from aqueous nitric acid, eliminating their interference in the americium stripping stages. In addition, although it is a macrocyclic ligand, H2BP18C6 does not significantly impede the mass transfer kinetics of the HDEHP solvent extraction system« less

  12. Effect of solvent type and high pressure treatment on the extraction of Gomphrena globosa L. bioactive compounds

    NASA Astrophysics Data System (ADS)

    Fernandes, L.; Ramalhosa, E.; Pereira, J. A.; Casal, S.; Saraiva, J. A.

    2017-10-01

    The present study aimed to compare the influence of different extraction solvents (water, methanol, water:acetone (6:4, v/v)), methods (heating (37 °C, 30 min) or high pressure (HP) (300 or 500 MPa) and extraction time (7.5 or 15 min)) on flavonoids, hydrolysable tannins and antioxidant activity (Total Reducing Capacity (TRC), DPPH Free Radical Scavenging Activity and Reducing Power) of Gomphrena globosa L. flower extracts. The water:acetone extracts obtained by heating had the highest values of flavonoids, hydrolysable tannins and antioxidant activity. When applying HP, variable results were obtained. Still, the application of HP to water allowed to extract more hydrolysable tannins, as well as to obtain extracts with higher antioxidant activity than with heating, but no significant alterations were observed with methanol. In conclusion, both solvent and extraction method influence the content of bioactive compounds, being HP treatment a promising method to obtain enriched aqueous extracts in line with the principles of green-chemistry.

  13. Selective Extraction of Flavonoids from Sophora flavescens Ait. by Mechanochemistry.

    PubMed

    Zhang, Qihong; Yu, Jingbo; Wang, Yingyao; Su, Weike

    2016-07-29

    Flavonoids from Sophora flavescens were selectively extracted by mechanochemical-promoted extraction technology (MPET) after using response surface methodology to determine the optimal extraction parameters. The highest yield of 35.17 mg/g was achieved by grinding the roots with Na₂CO₃ (15%) at 440 rpm/min for 17.0 min and water was used as the sole solvent with a ratio of solvent to solid material of 25 mL/g. Flavonoids prepared by MPET demonstrated relatively higher antioxidant activities in subsequent DPPH and hydroxyl radical scavenging assays. Main constituents in the extracts, including kurarinol, kushenol I/N and kurarinone, were characterized by HPLC-MS/MS, indicating good selective extraction by MPET. Physicochemical property changes of powder during mechanochemical milling were identified by scanning electron microscopy, X-ray powder diffraction, and UV-Vis diffuse-reflectance spectroscopy. Compared with traditional extraction methods, MPET possesses notable advantages of higher selectivity, lower extraction temperature, shorter extraction time, and organic solvent free properties.

  14. Combination of Antioxidants from Different Sources Could Offer Synergistic Benefits: A Case Study of Tea and Ginger Blend.

    PubMed

    Makanjuola, Solomon A; Enujiugha, Victor N; Omoba, Olufunmilayo S; Sanni, David M

    2015-11-01

    Tea and ginger are plants with high antioxidant potential. Combinations of antioxidants from different sources could also produce synergistic antioxidant effects. This study investigated the influence of solvent on antioxidant content of tea, ginger, and tea + ginger blends. Under the investigated extraction conditions, water was the most effective extraction solvent to maximise peroxide scavenging and iron chelating activity of tea, ginger, and their blends. Aqueous ethanol was the most effective solvent to maximise ABTS radical scavenging activity and ethanol was the best solvent to maximise DPPH radical scavenging activity. A good multivariate regression model that explains the relationship between the total flavonoid content of the extracts and their antioxidant activities was obtained (R2 and Q2 of 0.93 and 0.83, respectively). Extracts of tea-ginger blends exhibited synergistic effects in their ABTS and DPPH radical scavenging activity.

  15. Microwave- and ultrasound-assisted extraction of vanillin and its quantification by high-performance liquid chromatography in Vanilla planifolia.

    PubMed

    Sharma, Anuj; Verma, Subash Chandra; Saxena, Nisha; Chadda, Neetu; Singh, Narendra Pratap; Sinha, Arun Kumar

    2006-03-01

    Microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and conventional extraction of vanillin and its quantification by HPLC in pods of Vanilla planifolia is described. A range of nonpolar to polar solvents were used for the extraction of vanillin employing MAE, UAE and conventional methods. Various extraction parameters such as nature of the solvent, solvent volume, time of irradiation, microwave and ultrasound energy inputs were optimized. HPLC was performed on RP ODS column (4.6 mm ID x 250 mm, 5 microm, Waters), a photodiode array detector (Waters 2996) using gradient solvent system of ACN and ortho-phosphoric acid in water (0.001:99.999 v/v) at 25 degrees C. Regression equation revealed a linear relationship (r2 > 0.9998) between the mass of vanillin injected and the peak areas. The detection limit (S/N = 3) and limit of quantification (S/N = 10) were 0.65 and 1.2 microg/g, respectively. Recovery was achieved in the range 98.5-99.6% for vanillin. Maximum yield of vanilla extract (29.81, 29.068 and 14.31% by conventional extraction, MAE and UAE, respectively) was found in a mixture of ethanol/water (40:60 v/v). Dehydrated ethanolic extract showed the highest amount of vanillin (1.8, 1.25 and 0.99% by MAE, conventional extraction and UAE, respectively).

  16. Selective extraction of high-value phenolic compounds from distillation wastewater of basil (Ocimum basilicum L.) by pressurized liquid extraction.

    PubMed

    Pagano, Imma; Sánchez-Camargo, Andrea Del Pilar; Mendiola, Jose Antonio; Campone, Luca; Cifuentes, Alejandro; Rastrelli, Luca; Ibañez, Elena

    2018-01-31

    During the essential oil steam distillation from aromatic herbs, huge amounts of distillation wastewaters (DWWs) are generated. These by-products represent an exceptionally rich source of phenolic compounds such as rosmarinic acid (RA) and caffeic acid (CA). Herein, the alternative use of dried basil DWWs (dDWWs) to perform a selective extraction of RA and CA by pressurized liquid extraction (PLE) employing bio-based solvent was studied. To select the most suitable solvent for PLE, the theoretical modelling of Hansen solubility parameters (HSP) was carried out. This approach allows reducing the list of candidate to two solvents: ethanol and ethyl lactate. Due to the composition of the sample, mixtures of water with those solvents were also tested. An enriched PLE extract in RA (23.90 ± 2.06 mg/g extract) with an extraction efficiency of 75.89 ± 16.03% employing a water-ethanol mixture 25:75 (% v/v) at 50°C was obtained. In the case of CA, a PLE extract with 2.42 ± 0.04 mg/g extract, having an extraction efficiency of 13.86 ± 4.96% using ethanol absolute at 50°C was achieved. DWWs are proposed as new promising sources of natural additives and/or functional ingredients for cosmetic, nutraceutical, and food applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. An RF-Powered Micro-Reactor for Efficient Extraction and Hydrolysis

    NASA Astrophysics Data System (ADS)

    Scott, V.

    2014-12-01

    An RF sample-processing micro-reactor that was developed as part of potential in situ Exploration Missions to inner- and outer-planetary bodies was designed to utilize aqueous solutions subjected to 60 GHz radiation at 730 mW of input power to extract target organic compounds and molecular and inorganic ions as well as to hydrolyze complex polymeric materials. Successful identification and characterization of these molecules relies on the sample-processing techniques utilized alongside state-of-the-art detection and analysis. For mass and power restrictions put on space exploration missions, smaller and more efficient instruments are highly desirable. The RF micro-reactor potentially offers a simplified alternative to the typical gold-standard extractions that often use solvents, chemicals, and conditions that can vary wildly and depend on the targeted molecules. Instead, this instrument uses a single solvent ­— water — that can be "tuned" under the different experimental conditions, leveraging the operating principles of the Sub-Critical Water Extractor. Proof-of-concept experiments examining the hydrolysis of glycosidic and peptide bonds were successful in demonstrating the RF micro-reactor's capabilities. Progress toward coupling the reactor with a micro-scale sample-handling system enabling slurry delivery has been made and preliminary results on heterogeneous reactions and extractions will be presented.

  18. Application of saponin biosurfactant and its recovery in the MEUF process for removal of methyl violet from wastewater.

    PubMed

    Samal, Kulbhushan; Das, Chandan; Mohanty, Kaustubha

    2017-12-01

    The potential of saponin, a biosurfactant, in the micellar enhanced ultrafiltration (MEUF) process was tested systematically for removal of methyl violet from wastewater. For this, the aqueous extract of reetha (Sapindus mukorossi) pericarp which contains saponin was used as the biosurfactant. First, the micellar solubilization of methyl violet in saponin micelles was investigated in terms of molar solubilization power (SP) of saponin. It was observed that the adsorption of methyl violet on the agglomerates of saponin micelles was mainly responsible for the enhanced solubilization. The Gibbs free energy of solubilization (calculated as -29.63 kJ mol -1 ) suggested that process was feasible and spontaneous. The MEUF experiments were performed in batch as well as continuous mode using saponin biosurfactant, and the effect of operating parameters on permeate flux and solute retention were evaluated. The removal of methyl violet in MEUF process was >99% achieved with 10 kDa polyethersulfone (PES) membrane for feed dye concentration of 250 mg L -1 at studied conditions. Finally, the saponin in permeate was recovered using n-heptane and n-butanol by solvent extraction process. The solvent n-butanol showed better extraction efficiency as compared to n-heptane for saponin extraction. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Ferrofluid of magnetic clay and menthol based deep eutectic solvent: Application in directly suspended droplet microextraction for enrichment of some emerging contaminant explosives in water and soil samples.

    PubMed

    Zarei, Ali Reza; Nedaei, Maryam; Ghorbanian, Sohrab Ali

    2018-06-08

    In this work, for the first time, ferrofluid of magnetic montmorillonite nanoclay and deep eutectic solvent was prepared and coupled with directly suspended droplet microextraction. Incorporation of ferrofluid in a miniaturized sample preparation technique resulted in achieving high extraction efficiency while developing a green analytical method. The prepared ferrofluid has strong sorbing properties and hydrophobic characteristics. In this method, a micro-droplet of ferrofluid was suspended into the vortex of a stirring aqueous solution and after completing the extraction process, was easily separated from the solution by a magnetic rod without any operational problems. The predominant experimental variables affecting the extraction efficiency of explosives were evaluated. Under optimal conditions, the limits of detection were in the range 0.22-0.91 μg L -1 . The enrichment factors were between 23 and 93 and the relative standard deviations were <10%. The relative recoveries were ranged from 88 to 104%. This method was successfully applied for the extraction and preconcentration of explosives in water and soil samples, followed their determination by high performance liquid chromatography with ultraviolet detection (HPLC-UV). Copyright © 2018 Elsevier B.V. All rights reserved.

  20. Optimization of microwave-assisted extraction conditions for preparing lignan-rich extract from Saraca asoca bark using Box-Behnken design.

    PubMed

    Mishra, Shikha; Aeri, Vidhu

    2016-07-01

    Lyoniside is the major constituent of Saraca asoca Linn. (Caesalpiniaceae) bark. There is an immediate need to develop an efficient method to isolate its chemical constituents, since it is a therapeutically important plant. A rapid extraction method for lyoniside based on microwave-assisted extraction of S. asoca bark was developed and optimized using response surface methodology (RSM). Lyoniside was analyzed and quantified by high-performance liquid chromatography coupled with ultraviolet detection (HPLC-UV). The extraction solvent ratio (%), material solvent ratio (g/ml) and extraction time (min) were optimized using Box-Behnken design (BBD) to obtain the highest extraction efficiency. The optimal conditions were the use of 1:30 material solvent ratio with 70:30 mixture of methanol:water for 10 min duration. The optimized microwave-assisted extraction yielded 9.4 mg/g of lyoniside content in comparison to reflux extraction under identical conditions which yielded 4.2 mg/g of lyoniside content. Under optimum conditions, the experimental values agreed closely with the predicted values. The analysis of variance (ANOVA) indicated a high goodness-of-fit model and the success of the RSM method for optimizing lyoniside extraction from the bark of S. asoca. All the three variables significantly affected the lyoniside content. Increased polarity of solvent medium enhances the lyoniside yield. The present study shows the applicability of microwave-assisted extraction in extraction of lyoniside from S. asoca bark.

  1. Determination of rutin and quercetin in Chinese herbal medicine by ionic liquid-based pressurized liquid extraction-liquid chromatography-chemiluminescence detection.

    PubMed

    Wu, Hongwei; Chen, Meilan; Fan, Yunchang; Elsebaei, Fawzi; Zhu, Yan

    2012-01-15

    A novel ionic liquid-based pressurized liquid extraction (IL-PLE) procedure coupled with high performance liquid chromatography (HPLC) tandem chemiluminescence (CL) detection capable of quantifying trace amounts of rutin and quercetin in four Chinese medicine plants including Flos sophorae Immaturus, Crateagus pinnatifida Bunge, Hypericum japonicum Thunb and Folium Mori was described in this paper. To avoid environmental pollution and toxicity to the operators, ionic liquids (ILs), 1-alkyl-3-methylimidazolium chloride ([C(n)mim][Cl]) aqueous solutions were used in the PLE procedure as extractants replacing traditional organic solvents. In addition, chemiluminescence detection was utilized for its minimal interference from endogenous components of complex matrix. Parameters affecting extraction and analysis were carefully optimized. Compared with the conventional ultrasonic-assisted extraction (UAE) and heat-reflux extraction (HRE), the optimized method achieved the highest extraction efficiency in the shortest extraction time with the least solvent consumption. The applicability of the proposed method to real sample was confirmed. Under the optimized conditions, good reproducibility of extraction performance was obtained and good linearity was observed with correlation coefficients (r) between 0.9997 and 0.9999. The detection limits of rutin and quercetin (LOD, S/N=3) were 1.1×10(-2)mg/L and 3.8×10(-3)mg/L, respectively. The average recoveries of rutin and quercetin for real samples were 93.7-105% with relative standard deviation (RSD) lower than 5.7%. To the best of our knowledge, this paper is the first contribution to utilize a combination of IL-PLE with chemiluminescence detection. And the experimental results indicated that the proposed method shows a promising prospect in extraction and determination of rutin and quercetin in medicinal plants. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Effect of solvent polarity levels on separation of xanthone and coumarin from Calophyllum inophyllum leaves extract

    NASA Astrophysics Data System (ADS)

    Susanto, D. F.; Hapsari, S.; Trilutfiani, Z.; Borhet, A.; Aparamarta, H. W.; Widjaja, A.; Gunawan, S.

    2018-03-01

    Calophyllum inophyllum has various benefits that can be utilized from root, stem, leaf, until seed. C. inophyllum leaves contain many bioactive compounds, such as xanthone and coumarin which are useful as antioxidant, and inhibitors of enzyme activity from HIV virus. The aim of this research was to investigate the effect of solvent polarity levels on the separation of xanthone and coumarin compounds contained in the crude extract of C. inophyllum leaves. Crude leaves extract was obtained by percolation method. Moreover, Liquid Liquid Extraction (LLE) was used for separating xanthone and coumarin compounds. It was performed by methanol (polar solvent) and hexane (non-polar solvent) with solvent ratio of 1. Methanol concentration in water used were 20%, 50%, 80%, and 100%. Each fraction obtained was tested qualitatively using Thin Layer Chromatography (TLC) and quantitatively using Gas Chromatography (GC) to analyze xanthone and coumarin. The best separation result was obtained by using 50% methanol. In this results, coumarin and xanthones were separated in methanol fraction (81.18% recovery) and in hexane fraction (81.91% recovery), respectively.

  3. Headspace single drop microextraction versus dispersive liquid-liquid microextraction using magnetic ionic liquid extraction solvents.

    PubMed

    An, Jiwoo; Rahn, Kira L; Anderson, Jared L

    2017-05-15

    A headspace single drop microextraction (HS-SDME) method and a dispersive liquid-liquid microextraction (DLLME) method were developed using two tetrachloromanganate ([MnCl 4 2- ])-based magnetic ionic liquids (MIL) as extraction solvents for the determination of twelve aromatic compounds, including four polyaromatic hydrocarbons, by reversed phase high-performance liquid chromatography (HPLC). The analytical performance of the developed HS-SDME method was compared to the DLLME approach employing the same MILs. In the HS-SDME approach, the magnetic field generated by the magnet was exploited to suspend the MIL solvent from the tip of a rod magnet. The utilization of MILs in HS-SDME resulted in a highly stable microdroplet under elevated temperatures and long extraction times, overcoming a common challenge encountered in traditional SDME approaches of droplet instability. The low UV absorbance of the [MnCl 4 2- ]-based MILs permitted direct analysis of the analyte enriched extraction solvent by HPLC. In HS-SDME, the effects of ionic strength of the sample solution, temperature of the extraction system, extraction time, stir rate, and headspace volume on extraction efficiencies were examined. Coefficients of determination (R 2 ) ranged from 0.994 to 0.999 and limits of detection (LODs) varied from 0.04 to 1.0μgL -1 with relative recoveries from lake water ranging from 70.2% to 109.6%. For the DLLME method, parameters including disperser solvent type and volume, ionic strength of the sample solution, mass of extraction solvent, and extraction time were studied and optimized. Coefficients of determination for the DLLME method varied from 0.997 to 0.999 with LODs ranging from 0.05 to 1.0μgL -1 . Relative recoveries from lake water samples ranged from 68.7% to 104.5%. Overall, the DLLME approach permitted faster extraction times and higher enrichment factors for analytes with low vapor pressure whereas the HS-SDME approach exhibited better extraction efficiencies for analytes with relatively higher vapor pressure. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Determination of Parameters for the Supercritical Extraction of Antioxidant Compounds from Green Propolis Using Carbon Dioxide and Ethanol as Co-Solvent.

    PubMed

    Machado, Bruna Aparecida Souza; Barreto, Gabriele de Abreu; Costa, Aline Silva; Costa, Samantha Serra; Silva, Rejane Pina Dantas; da Silva, Danielle Figuerêdo; Brandão, Hugo Neves; da Rocha, José Luiz Carneiro; Nunes, Silmar Baptista; Umsza-Guez, Marcelo Andres; Padilha, Francine Ferreira

    2015-01-01

    The aim of this study was to determine the best processing conditions to extract Brazilian green propolis using a supercritical extraction technology. For this purpose, the influence of different parameters was evaluated such as S/F (solvent mass in relation to solute mass), percentage of co-solvent (1 and 2% ethanol), temperature (40 and 50°C) and pressure (250, 350 and 400 bar) using supercritical carbon dioxide. The Global Yield Isotherms (GYIs) were obtained through the evaluation of the yield, and the chemical composition of the extracts was also obtained in relation to the total phenolic compounds, flavonoids, antioxidant activity and 3,5-diprenyl-4-hydroxicinnamic acid (Artepillin C) and acid 4-hydroxycinnamic (p-coumaric acid). The best results were identified at 50°C, 350 bar, 1% ethanol (co-solvent) and S/F of 110. These conditions, a content of 8.93±0.01 and 0.40±0.05 g/100 g of Artepillin C and p-coumaric acid, respectively, were identified indicating the efficiency of the extraction process. Despite of low yield of the process, the extracts obtained had high contents of relevant compounds, proving the viability of the process to obtain green propolis extracts with important biological applications due to the extracts composition.

  5. Removal of iron interferences by solvent extraction for geochemical analysis by atomic-absorption spectrophotometry

    USGS Publications Warehouse

    Zhou, L.; Chao, T.T.; Sanzolone, R.F.

    1985-01-01

    Iron is a common interferent in the determination of many elements in geochemical samples. Two approaches for its removal have been taken. The first involves removal of iron by extraction with methyl isobutyl ketone (MIBK) from hydrochloric acid medium, leaving the analytes in the aqueous phase. The second consists of reduction of iron(III) to iron(II) by ascorbic acid to minimize its extraction into MIBK, so that the analytes may be isolated by extraction. Elements of interest can then be determined using the aqueous solution or the organic extract, as appropriate. Operating factors such as the concentration of hydrochloric acid, amounts of iron present, number of extractions, the presence or absence of a salting-out agent, and the optimum ratio of ascorbic acid to iron have been determined. These factors have general applications in geochemical analysis by atomic-absorption spectrophotometry. ?? 1985.

  6. Optimization of microwave assisted extraction (MAE) and soxhlet extraction of phenolic compound from licorice root.

    PubMed

    Karami, Zohreh; Emam-Djomeh, Zahra; Mirzaee, Habib Allah; Khomeiri, Morteza; Mahoonak, Alireza Sadeghi; Aydani, Emad

    2015-06-01

    In present study, response surface methodology was used to optimize extraction condition of phenolic compounds from licorice root by microwave application. Investigated factors were solvent (ethanol 80 %, methanol 80 % and water), liquid/solid ratio (10:1-25:1) and time (2-6 min). Experiments were designed according to the central composite rotatable design. The results showed that extraction conditions had significant effect on the extraction yield of phenolic compounds and antioxidant capacities. Optimal condition in microwave assisted method were ethanol 80 % as solvent, extraction time of 5-6 min and liquid/solid ratio of 12.7/1. Results were compared with those obtained by soxhlet extraction. In soxhlet extraction, Optimum conditions were extraction time of 6 h for ethanol 80 % as solvent. Value of phenolic compounds and extraction yield of licorice root in microwave assisted (MAE), and soxhlet were 47.47 mg/g and 16.38 %, 41.709 mg/g and 14.49 %, respectively. These results implied that MAE was more efficient extracting method than soxhlet.

  7. Comparison of extraction techniques of robenidine from poultry feed samples.

    PubMed

    Wilga, Joanna; Wasik, Agata Kot-; Namieśnik, Jacek

    2007-10-31

    In this paper, effectiveness of six different commonly applied extraction techniques for the determination of robenidine in poultry feed has been compared. The sample preparation techniques included shaking, Soxhlet, Soxtec, ultrasonically assisted extraction, microwave - assisted extraction and accelerated solvent extraction. Comparison of these techniques was done with respect to the recovery extraction, temperature and time, reproducibility and solvent consumption. Every single extract was subjected to clean - up using aluminium oxide column (Pasteur pipette filled with 1g of aluminium oxide), from which robenidine was eluted with 10ml of methanol. The eluate from the clean-up column was collected in a volumetric flask, and finally it was analysed by HPLC-DAD-MS. In general, all extraction techniques were capable of isolating of robenidine from poultry feed, but the recovery obtained using modern extraction techniques was higher than that obtained using conventional techniques. In particular, accelerated solvent extraction was more superior to other techniques, which highlights the advantages of this sample preparation technique. However, in routine analysis, shaking and ultrasonically assisted extraction is still the preferred method for the solution of robenidine and other coccidiostatics.

  8. Selection of propolis Tetragonula sp. extract solvent with flavonoids and polyphenols concentration and antioxidant activity parameters

    NASA Astrophysics Data System (ADS)

    Christina, Daisy; Hermansyah, Heri; Wijanarko, Anondho; Rohmatin, Etin; Sahlan, Muhamad; Pratami, Diah Kartika; Mun'im, Abdul

    2018-02-01

    Antioxidants are inhibitory compounds that can inhibit auto oxidation reaction by binding to free radicals and highly reactive molecules. The human body needs antioxidant. Antioxidants can be obtained from a variety of natural ingredients, including propolis. Propolis is the natural sap of the bees, obtained from the herbs around the honeycomb. Ethanol is the solvent that often used to extract propolis. Although it has many advantages, ethanol also has weaknesses such as intolerance to alcohol by some people. Therefore, this research was to extract propolis Tetragonula sp. coarse (C) and soft (S) using four varieties of organic solvent, i.e. olive oil (OO), virgin coconut oil (VCO), propylene glycol (PG), and lecithin (L). It was expected to get the best solvent in extracting propolis. The selection of the best solvent was determined by total flavonoids and polyphenols content assay and antioxidant activity. At each test, the absorbance value read by a microplate reader. Flavonoids content assay is using AlCl3 method with best result on rough-VCO propolis extract of 2509,767 ± 615,02 µg/mL. Polyphenols content assay was using Folin Ciocalteu method with the best results on soft-VCO propolis extract of 1391 ± 171.47 µg/mL. Antioxidant activity assay is using DPPH method with best result on soft-VCO propolis extract with IC50 value of 1,559 ± 0,222 µg/mL.

  9. Evaluation of the effect of extraction solvent and organ selection on the chemical profile of Astragalus spinosus using HPTLC- multivariate image analysis.

    PubMed

    Shawky, Eman; Selim, Dina A

    2017-09-01

    The evaluation of extraction protocols for untargeted and targeted metabolomics was implemented for root and aerial organs of Astragalus spinosus in this work. The efficiency and complementarity of commonly used extraction solvents, namely petroleum ether, methylene chloride, ethyl acetate and n-butanol were considered for method evaluation using chemometric techniques in conjunction with new, simple, and fast high performance thin layer chromatography (HPTLC) method for fingerprint analysis by extracting information from a digitalized HPTLC plate using ImageJ software. A targeted approach was furtherly implemented by developing and validating an HPTLC method allowing the quantification of three saponin glycosides. The results of untargeted and targeted principle component analysis (PCA) and hierarchical cluster analysis (HCA) revealed that the apparent saponins profile seems to depend on a combined effect of matrix composition and the properties of the selected solvent for extraction, where both the biological matrix of the investigated plant organs, as well as the extraction solvent can influence the precision of metabolite abundances. Although, the aerial part is frequently discarded as waste, it is shown hereby that it has similar chemical profile compared to the medicinal part, roots, yet a different extraction solvents pattern is recognized between the two organs which can be attributed to the differences in the composition, permeability or accessibility of the sample matrix/organ tissues, rather than the chemical structures of the detected metabolites. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. An Efficient Strategy Based on Liquid-Liquid Extraction with Three-Phase Solvent System and High Speed Counter-Current Chromatography for Rapid Enrichment and Separation of Epimers of Minor Bufadienolide from Toad Meat.

    PubMed

    Zou, Denglang; Zhu, Xuelin; Zhang, Fan; Du, Yurong; Ma, Jianbin; Jiang, Renwang

    2018-01-31

    This study presents an efficient strategy based on liquid-liquid extraction with three-phase solvent system and high speed counter-current chromatography for rapid enrichment and separation of epimers of minor bufadienolide from toad meat. The reflux extraction conditions were optimized by response surface methodology first, and a novel three-phase solvent system composed of n-hexane/methyl acetate/acetonitrile/water (3:6:5:5, v/v) was developed for liquid-liquid extraction of the crude extract. This integrative extraction process could enrich minor bufadienolide from complex matrix efficiently and minimize the loss of minor targets induced by repeated extraction with different kinds of organic solvents occurring in the classical liquid two-phase extraction. As a result, four epimers of minor bufadienolide were greatly enriched in the middle phase and total content of these epimers of minor bufadienolide was increased from 3.25% to 46.23%. Then, the enriched four epimers were separated by HSCCC with a two-phase solvent system composed of chloroform/methanol/water (4:2:2, v/v) successfully. Furthermore, we tested Na + ,K + -ATPase (NKA) inhibitory effect of the four epimers. 3β-Isomers of bufadienolide showed stronger (>8-fold) inhibitory activity than 3α-isomers. The characterization of minor bufadienolide in toad meat and their significant difference of inhibitory effect on NKA would promote the further quantitative analysis and safety evaluation of toad meat as a food source.

  11. Study of optimal extraction conditions for achieving high yield and antioxidant activity of tomato seed oil.

    PubMed

    Shao, Dongyan; Atungulu, Griffiths G; Pan, Zhongli; Yue, Tianli; Zhang, Ang; Li, Xuan

    2012-08-01

    Value of tomato seed has not been fully recognized. The objectives of this research were to establish suitable processing conditions for extracting oil from tomato seed by using solvent, determine the impact of processing conditions on yield and antioxidant activity of extracted oil, and elucidate kinetics of the oil extraction process. Four processing parameters, including time, temperature, solvent-to-solid ratio and particle size were studied. A second order model was established to describe the oil extraction process. Based on the results, increasing temperature, solvent-to-solid ratio, and extraction time increased oil yield. In contrast, larger particle size reduced the oil yield. The recommended oil extraction conditions were 8 min of extraction time at temperature of 25 °C, solvent-to-solids ratio of 5/1 (v/w) and particle size of 0.38 mm, which gave oil yield of 20.32% with recovery rate of 78.56%. The DPPH scavenging activity of extracted oil was not significantly affected by the extraction parameters. The inhibitory concentration (IC(50) ) of tomato seed oil was 8.67 mg/mL which was notably low compared to most vegetable oils. A 2nd order model successfully described the kinetics of tomato oil extraction process and parameters of extraction kinetics including initial extraction rate (h), equilibrium concentration of oil (C(s) ), and the extraction rate constant (k) could be precisely predicted with R(2) of at least 0.957. The study revealed that tomato seed which is typically treated as a low value byproduct of tomato processing has great potential in producing oil with high antioxidant capability. The impact of processing conditions including time, temperature, solvent-to-solid ratio and particle size on yield, and antioxidant activity of extracted tomato seed oil are reported. Optimal conditions and models which describe the extraction process are recommended. The information is vital for determining the extraction processing conditions for industrial production of high quality tomato seed oil. Journal of Food Science © 2012 Institute of Food Technologists® No claim to original US government works.

  12. Deep eutectic solvent based gas-assisted dispersive liquid-phase microextraction combined with gas chromatography and flame ionization detection for the determination of some pesticide residues in fruit and vegetable samples.

    PubMed

    Farajzadeh, Mir Ali; Sattari Dabbagh, Masoumeh; Yadeghari, Adeleh

    2017-05-01

    In this study, a gas-assisted dispersive liquid-phase microextraction method using a deep eutectic solvent as the extraction solvent combined with gas chromatography and flame ionization detection was developed for the extraction and determination of some pesticide residues in vegetable and fruit juice samples. In this method, choline chloride and 4-chlorophenol at a molar ratio of 1:2 were mixed. By heating and vortexing, a clear, water-immiscible, and homogeneous liquid was formed. The obtained deep eutectic solvent was added to an aqueous solution of the analytes in a conical test tube. Air was bubbled into the aqueous solution and a cloudy solution was obtained. During this step, the analytes were extracted into the fine droplets of the extraction solvent. After centrifugation, an aliquot of the settled phase was injected into the separation system. Under the optimum extraction conditions, enrichment factors, and extraction recoveries were obtained in the ranges of 247-355 and 49-71%, respectively. The obtained values for the limits of detection and quantification were in the ranges of 0.24-1.4 and 0.71-4.2 μg/L, respectively. The proposed method is simple, fast, efficient, and inexpensive. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Solvent Hold Tank Sample Results for MCU-16-1247-1248-1249: August 2016 Monthly Sample

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F. F.; Jones, D. H.

    Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-1247-1248-1249), pulled on 08/22/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1247-1248-1249 indicated the Isopar™L concentration is above its nominal level (101%). The extractant (MaxCalix) and the modifier (CS-7SB) are 7% and 9 % below their nominal concentrations. The suppressor (TiDG) is 63% below its nominal concentration. This analysis confirms the solvent may require the addition of TiDG, and possibly of modifier and MaxCalix to restore then to nominal levels. Based on the current monthly sample, the levelsmore » of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. At the time of writing this report, A solvent trim batch containing TiDG, modifier and MaxCalix, was added to the SHT (October 2016) and expect the concentration of these components to be at their nominal values.« less

  14. SLURRY SOLVENT EXTRACTION PROCESS FOR THE RECOVERY OF METALS FROM SOLID MATERIALS

    DOEpatents

    Grinstead, R.R.

    1959-01-20

    A solvent extraction process is described for recovering uranium from low grade uranium bearing minerals such as carnotit or shale. The finely communited ore is made up as an aqueous slurry containing the necessary amount of acid to solubilize the uranium and simultaneously or subsequently contacted with an organic solvent extractant such as the alkyl ortho-, or pyro phosphoric acids, alkyl phosphites or alkyl phosphonates in combination with a diluent such as kerosene or carbon tetrachlorids. The extractant phase is separated from the slurry and treated by any suitable process to recover the uranium therefrom. One method for recovering the uranium comprises treating the extract with aqueous HF containing a reducing agent such as ferrous sulfate, which reduces the uranium and causes it to be precipitated as uranium tetrafluoride.

  15. Development of a Supported Emulsion Liquid Membrane System for Propionic Acid Separation in a Microgravity Environment

    NASA Technical Reports Server (NTRS)

    Li, Jin; Hu, Shih-Yao B.; Wiencek, John M.

    2001-01-01

    Perstractive fermentation is a good way to increase the productivity of bioreactors. Using Propionibacteria as the model system, the feasibility of using supported emulsion liquid membrane (SELM) for perstractive fermentation is assessed in this study. Five industrial solvents were considered as the solvent for preparing the SELM. The more polar a solvent is, the higher the partition coefficient. However, toxicity of a solvent also increases with its polarity. CO-1055 (industrial decanol/octanol blend) has the highest partition coefficient toward propionic acid among the solvents that has no molecular toxicity toward Propionibacteria. A preliminary extraction study was conducted using tetradecane as solvent in a hydrophobic hollow fiber contactor. The result confirmed that SELM eliminates the equilibrium limitation of conventional liquid-liquid extraction, and allows the use of a non-toxic solvent with low partition coefficient.

  16. Silybum marianum pericarp yields enhanced silymarin products.

    PubMed

    AbouZid, Sameh F; Chen, Shao-Nong; McAlpine, James B; Friesen, J Brent; Pauli, Guido F

    2016-07-01

    An improved method for the purification of silymarin, the flavonolignan complex from the fruits of milk thistle, Silybum marianum, is reported. The method enables a more efficient extraction of silymarin from the pericarp after it has been separated mechanically from the rest of the fruits. Accelerated solvent extraction (ASE) was employed for each extraction procedure. Quantitation of the eight major silymarin components in the pericarp extract was compared to that of the whole fruit extract using two orthogonal analytical methods. The pericarp extract showed higher silymarin content (2.24-fold by HPLC and 2.12-fold by qHNMR) than whole fruit extract using acetone as an extraction solvent following defatting with hexane. Furthermore, the mg/g recovery of silymarin major components was not diminished by eliminating the hexane defatting step from the pericarp extraction procedure. The efficiencies of acetone, ethanol, and methanol as extraction solvents were compared. Methanol pericarp extract showed the highest content of the silymarin major components, 2.72-fold higher than an extract prepared from the whole fruits using acetone. Finally, all of the major silymarin components showed a higher w/w content in the pericarp extract than in a commercial extract. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Solvent extraction separation of Th-227 and Ac-225 in room temperature ionic liquids

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Bell, Jason R; Boll, Rose Ann; Dai, Sheng

    2012-01-01

    The solvent extractions of Th-227 and Ac-225 from the aqueous phase into ionic liquids (ILs) were investigated by using N,N,N ,N - tetraoctyldiglycolamide (TODGA) or di(2-ethylhexyl)phosphoric acid (HDEHP) as an extractant. Four ionic liquids, 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide ([C4mim][NTf2]), 1-butyl-3-methylimidazolium bis(perfluoroethanesulfonyl)imide ([C4mim][BETI]), 1-butyl-2,3-trimethyleneimidazolium (trifluoromethanesulfonyl)imide [BuI5][NTf2], and 1-benzyl pyridinium bis(trifluoromethanesulfonyl)imide ([PhCH2Py][NTf2]) were used as extraction solvents for separation of Th-227 and Ac-225 in this study. Excellent extraction efficiencies and selectivities were found for Th-227/Ac-225 when HDEHP was used as an extractant in these ionic liquids. The effects of different extractant concentrations in ionic liquids and acidities of the aqueous phase on extraction efficienciesmore » and selectivities of Th-227/Ac-225 are also presented in this article.« less

  18. Compound Specific Extraction of Camptothecin from Nothapodytes nimmoniana and Piperine from Piper nigrum Using Accelerated Solvent Extractor

    PubMed Central

    Upadhya, Vinayak; Pai, Sandeep R.; Sharma, Ajay K.; Hegde, Harsha V.; Kholkute, Sanjiva D.; Joshi, Rajesh K.

    2014-01-01

    Effects of varying temperatures with constant pressure of solvent on extraction efficiency of two chemically different alkaloids were studied. Camptothecin (CPT) from stem of Nothapodytes nimmoniana (Grah.) Mabb. and piperine from the fruits of Piper nigrum L. were extracted using Accelerated Solvent Extractor (ASE). Three cycles of extraction for a particular sample cell at a given temperature assured complete extraction. CPT and piperine were determined and quantified by using a simple and efficient UFLC-PDA (245 and 343 nm) method. Temperature increased efficiency of extraction to yield higher amount of CPT, whereas temperature had diminutive effect on yield of piperine. Maximum yield for CPT was achieved at 80°C and for piperine at 40°C. Thus, the study determines compound specific extraction of CPT from N. nimmoniana and piperine from P. nigrum using ASE method. The present study indicates the use of this method for simple, fast, and accurate extraction of the compound of interest. PMID:24527258

  19. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Thompson, G H; Thompson, M C

    Solvent extraction of /sup 237/Np and /sup 238/Pu from irradiated neptunium is being investigated as a possible replacement for the currently used anion exchange process at the Savannah River Plant. Solvent extraction would reduce separations costs and waste volume and increase the production rate. The major difficulty in solvent extraction processing is maintaining neptunium and plutonium in the extractable IV or VI valence states during initial extraction. This study investigated the stability of these states. Results show that: The extractable M(IV) valence states of neptunium and plutonium are mutually unstable in plant dissolver solution (2 g/l /sup 237/Np, 0.4 g/lmore » /sup 238/Pu, 1.2M Al/sup 3 +/, 4.6M NO/sub 3//sup -/, and 1M H/sup +/). The reaction rates producing inextractable species from extractable M(IV) or M(VI) are fast enough that greater than or equal to 99.9 percent extractable species in /sup 237/Np--/sup 238/Pu mixtures cannot be maintained for a practicable processing period (24 hours).« less

  20. Effects of process parameters on peanut skins extract and CO2 diffusivity by supercritical fluid extraction

    NASA Astrophysics Data System (ADS)

    Putra, N. R.; Yian, L. N.; Nasir, H. M.; Idham, Z. Binti; Yunus, M. A. C.

    2018-03-01

    Peanut skins (Arachis hypogea) are an agricultural waste product which has received much attention because they contain high nutritional values and can be potentially utilized in difference industries. At present, only a few studies have been conducted to study the effects of parameters on the peanut skins oil extraction. Therefore, this study aimed to determine the best extraction condition in order to obtain the highest extract yield using supercritical carbon dioxide (SC-CO2) with co-solvent Ethanol as compared to Soxhlet extraction method. Diffusivity of carbon dioxide in supercritical fluid extraction was determined using Crank model. The mean particle size used in this study was 425 µm. The supercritical carbon dioxide was performed at temperature (40 – 70 °C), flow rate of co-solvent ethanol (0 - 7.5% Vethanol/Vtotal), and extraction pressure (10 – 30 MPa) were used in this studies. The results showed that the percentage of oil yields and effective diffusivity increase as the pressure, rate of co-solvent, and temperature increased.

  1. Salting-out assisted liquid-liquid extraction with the aid of experimental design for determination of benzimidazole fungicides in high salinity samples by high-performance liquid chromatography.

    PubMed

    Wen, Yingying; Li, Jinhua; Yang, Fangfang; Zhang, Weiwei; Li, Weiran; Liao, Chunyang; Chen, Lingxin

    2013-03-15

    A novel method for the simultaneous separation and determination of four benzimidazole fungicides (i.e., carbendazim, fuberidazole, thiophanate-methyl and thiophanate) in high salinity samples was developed by using salting-out assisted liquid-liquid extraction (SALLE) via water-miscible acetonitrile as the extractant coupled with high-performance liquid chromatography. Box-Behnken design and response surface were employed to assist the optimization of SALLE conditions, including volume of salting-out solvent, the pH of sample solution and salting-out solvent as variable factors. The optimal salting-out parameters were obtained as follows: 2 mL of acetonitrile was added to 2 mL of sample solution with pH=4 and then 2 mL salting-out solvent containing 5 mol L(-1) sodium chloride at a pH of 7 was added to the solution for extraction. This procedure afforded a convenient and cost-saving operation with good cleanup ability for the benzimidazole fungicides, such as good linear relationships (R>0.996) between peak area and concentration from 2.5 ng mL(-1) to 500 ng mL(-1), low limits of detection between 0.14 ng mL(-1) and 0.38 ng mL(-1) and the intra-day precisions of retention time below 1.0%. The method recoveries obtained at fortified three concentrations for three seawater samples ranged from 60.4% to 99.1%. The simple, rapid and eco-benign SALLE based method proved potentially applicable for trace benzimidazole fungicides analysis in high salinity samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. Subcritical-Water Extraction of Organics from Solid Matrices

    NASA Technical Reports Server (NTRS)

    Amashukeli, Xenia; Grunthaner, Frank; Patrick, Steven; Kirby, James; Bickler, Donald; Willis, Peter; Pelletier, Christine; Bryson, Charles

    2009-01-01

    An apparatus for extracting organic compounds from soils, sands, and other solid matrix materials utilizes water at subcritical temperature and pressure as a solvent. The apparatus, called subcritical water extractor (SCWE), is a prototype of subsystems of future instrumentation systems to be used in searching for organic compounds as signs of past or present life on Mars. An aqueous solution generated by an apparatus like this one can be analyzed by any of a variety of established chromatographic or spectroscopic means to detect the dissolved organic compound( s). The apparatus can be used on Earth: indeed, in proof-of-concept experiments, SCWE was used to extract amino acids from soils of the Atacama Desert (Chile), which was chosen because the dryness and other relevant soil conditions there approximate those on Mars. The design of the apparatus is based partly on the fact that the relative permittivity (also known as the dielectric constant) of liquid water varies with temperature and pressure. At a temperature of 30 C and a pressure of 0.1 MPa, the relative permittivity of water is 79.6, due to the strong dipole-dipole electrostatic interactions between individual molecular dipoles. As the temperature increases, increasing thermal energy causes increasing disorientation of molecular dipoles, with a consequent decrease in relative permittivity. For example, water at a temperature of 325 C and pressure of 20 MPa has a relative permittivity of 17.5, which is similar to the relative permittivities of such nonpolar organic solvents as 1-butanol (17.8). In the operation of this apparatus, the temperature and pressure of water are adjusted so that the water can be used in place of commonly used organic solvents to extract compounds that have dissimilar physical and chemical properties.

  3. SOLVENT EXTRACTION PROCESS FOR URANIUM RECOVERY

    DOEpatents

    Clark, H.M.; Duffey, D.

    1958-06-17

    A process is described for extracting uranium from uranium ore, wherein the uranium is substantially free from molybdenum contamination. In a solvent extraction process for recovering uranium, uranium and molybdenum ions are extracted from the ore with ether under high acidity conditions. The ether phase is then stripped with water at a lower controiled acidity, resaturated with salting materials such as sodium nitrate, and reextracted with the separation of the molybdenum from the uranium without interference from other metals that have been previously extracted.

  4. Occupational exposure to complex mixtures of volatile organic compounds in ambient air: desorption from activated charcoal using accelerated solvent extraction can replace carbon disulfide?

    PubMed

    Fabrizi, Giovanni; Fioretti, Marzia; Rocca, Lucia Mainero

    2013-01-01

    A desorption study of 57 volatile organic compounds (VOCs) has been conducted by use of accelerated solvent extraction (ASE) and gas chromatography-mass spectrometry. Different solvents were tested to extract activated charcoal tubes with the objective of replacing carbon disulfide, used in official methods, because of its highly toxic health and environmental effects. Extraction conditions, for example temperature and number of cycles, were investigated and optimized. The definitive extraction procedure selected was use of acetone at 150 °C and two consecutive extraction cycles at a pressure of 1,500 psi. Considering a sample volume of 0.005 Nm(3), corresponding to a sampling time of 8 h at a flow rate of 0.01 L min(-1), the method was validated over the concentration range 65-26,300 μg Nm(-3). The lowest limit of quantification was 6 μg Nm(-3), and recovery for the 93 % of analytes ranged from 65 to 102 %. For most of the compounds, relative standard deviations were less than 15 % for inter and intra-day precision. Uncertainty of measurement was also determined: the relative expanded uncertainty was always below 29.6 %, except for dichlorodifluoromethane. This work shows that use of friendlier solvent, for example acetone, coupled with use of ASE, can replace use of CS(2) for chemical removal of VOCs from activated charcoal. ASE has several advantages over traditional solvent-extraction methods, including shorter extraction time, minimum sample manipulation, high reproducibility, and less extraction discrimination. No loss of sensitivity occurs and there is also a salutary effect on bench workers' health and on the smell of laboratory air.

  5. Integrated microwave processing system for the extraction of organophosphorus pesticides in fresh vegetables.

    PubMed

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-03-01

    A simple and efficient integrated microwave processing system (IMPS) was firstly assembled and validated for the extraction of organophosphorus pesticides in fresh vegetables. Two processes under microwave irradiation, dynamic microwave-assisted extraction (DMAE) and microwave-accelerated solvent elution (MASE), were integrated for simplifying the pretreatment of the sample. Extraction, separation, enrichment and elution were finished in a simple step. The organophosphorus pesticides were extracted from the fresh vegetables into hexane with DMAE, and then the extract was directly introduced into the enrichment column packed with active carbon fiber (ACF). Subsequently, the organophosphorus pesticides trapped on the ACF were eluted with ethyl acetate under microwave irradiation. No further filtration or cleanup was required before analysis of the eluate by gas chromatography-mass spectrometry. Some experimental parameters affecting extraction efficiency were investigated and optimized, such as microwave output power, kind and volume of extraction solvent, extraction time, amount of sorbent, elution microwave power, kind and volume of elution solvent, elution solvent flow rate. Under the optimized conditions, the recoveries were in the range of 71.5-105.2%, and the relative standard deviations were lower than 11.6%. The experiment results prove that the present method is a simple and effective sample preparation method for the determination of pesticides in solid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. [Study on new extraction technology of astragaloside IV].

    PubMed

    Sun, Haiyan; Guan, Su; Huang, Min

    2005-08-01

    To explore the possibility and the optimal extraction technology of astragaloside IV by SFE-CO2. According the content of astragaloside IV, the optimum extraction technology parameters such as extraction temperature, pressure, extraction time, velocity of fluid and co-solvent were investigated and the result was compared with that of water extraction. The optimum technical parameters were as follows: Extracting pressure 40 Mpa, temperature 45 degrees C, extracting time 2h, co-solvent was 95% ethanol and its dosage was 4ml/g, the ratio of CO2 fluid was 10 kg/kg x h. Extraction technology of astragaloside IV by SFE-CO2 is reliable, stable.

  7. Subcritical water extraction of organic matter from sedimentary rocks.

    PubMed

    Luong, Duy; Sephton, Mark A; Watson, Jonathan S

    2015-06-16

    Subcritical water extraction of organic matter containing sedimentary rocks at 300°C and 1500 psi produces extracts comparable to conventional solvent extraction. Subcritical water extraction of previously solvent extracted samples confirms that high molecular weight organic matter (kerogen) degradation is not occurring and that only low molecular weight organic matter (free compounds) are being accessed in analogy to solvent extraction procedures. The sedimentary rocks chosen for extraction span the classic geochemical organic matter types. A type I organic matter-containing sedimentary rock produces n-alkanes and isoprenoidal hydrocarbons at 300°C and 1500 psi that indicate an algal source for the organic matter. Extraction of a rock containing type II organic matter at the same temperature and pressure produces aliphatic hydrocarbons but also aromatic compounds reflecting the increased contributions from terrestrial organic matter in this sample. A type III organic matter-containing sample produces a range of non-polar and polar compounds including polycyclic aromatic hydrocarbons and oxygenated aromatic compounds at 300°C and 1500 psi reflecting a dominantly terrestrial origin for the organic materials. Although extraction at 300°C and 1500 psi produces extracts that are comparable to solvent extraction, lower temperature steps display differences related to organic solubility. The type I organic matter produces no products below 300°C and 1500 psi, reflecting its dominantly aliphatic character, while type II and type III organic matter contribute some polar components to the lower temperature steps, reflecting the chemical heterogeneity of their organic inventory. The separation of polar and non-polar organic compounds by using different temperatures provides the potential for selective extraction that may obviate the need for subsequent preparative chromatography steps. Our results indicate that subcritical water extraction can act as a suitable replacement for conventional solvent extraction of sedimentary rocks, but can also be used for any organic matter containing mineral matrix, including soils and recent sediments, and has the added benefit of tailored extraction for analytes of specific polarities. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

  8. FIELD EVALUATION OF THE SOLVENT EXTRACTION RESIDUAL BIOTREATMENT (SERB) TECHNOLOGY

    EPA Science Inventory

    The Solvent Extraction Residual Biotreatment (SERB) technology was demonstrated at the former Sage's Dry Cleaner site in Jacksonville, FL where an area of PCE (tetrachloroethylene) contamination was identified. The SERB technology is a treatment train approach to complete site...

  9. Process for extracting technetium from alkaline solutions

    DOEpatents

    Moyer, Bruce A.; Sachleben, Richard A.; Bonnesen, Peter V.

    1995-01-01

    A process for extracting technetium values from an aqueous alkaline solution containing at least one alkali metal hydroxide and at least one alkali metal nitrate, the at least one alkali metal nitrate having a concentration of from about 0.1 to 6 molar. The solution is contacted with a solvent consisting of a crown ether in a diluent for a period of time sufficient to selectively extract the technetium values from the aqueous alkaline solution. The solvent containing the technetium values is separated from the aqueous alkaline solution and the technetium values are stripped from the solvent.

  10. Alternative oil extraction methods from Echium plantagineum L. seeds using advanced techniques and green solvents.

    PubMed

    Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

    2018-04-01

    The edible oil processing industry involves large losses of organic solvent into the atmosphere and long extraction times. In this work, fast and environmentally friendly alternatives for the production of echium oil using green solvents are proposed. Advanced extraction techniques such as Pressurized Liquid Extraction (PLE), Microwave Assisted Extraction (MAE) and Ultrasound Assisted Extraction (UAE) were evaluated to efficiently extract omega-3 rich oil from Echium plantagineum seeds. Extractions were performed with ethyl acetate, ethanol, water and ethanol:water to develop a hexane-free processing method. Optimal PLE conditions with ethanol at 150 °C during 10 min produced a very similar oil yield (31.2%) to Soxhlet using hexane for 8 h (31.3%). UAE optimized method with ethanol at mild conditions (55 °C) produced a high oil yield (29.1%). Consequently, advanced extraction techniques showed good lipid yields and furthermore, the produced echium oil had the same omega-3 fatty acid composition than traditionally extracted oil. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.

    PubMed

    Carro, N; García, I; Ignacio, M-C; Llompart, M; Yebra, M-C; Mouteira, A

    2002-10-01

    A sample-preparation procedure (extraction and saponification) using microwave energy is proposed for determination of organochlorine pesticides in oyster samples. A Plackett-Burman factorial design has been used to optimize the microwave-assisted extraction and mild saponification on a freeze dried sample spiked with a mixture of aldrin, endrin, dieldrin, heptachlor, heptachorepoxide, isodrin, transnonachlor, p, p'-DDE, and p, p'-DDD. Six variables: solvent volume, extraction time, extraction temperature, amount of acetone (%) in the extractant solvent, amount of sample, and volume of NaOH solution were considered in the optimization process. The results show that the amount of sample is statistically significant for dieldrin, aldrin, p, p'-DDE, heptachlor, and transnonachlor and solvent volume for dieldrin, aldrin, and p, p'-DDE. The volume of NaOH solution is statistically significant for aldrin and p, p'-DDE only. Extraction temperature and extraction time seem to be the main factors determining the efficiency of extraction process for isodrin and p, p'-DDE, respectively. The optimized procedure was compared with conventional Soxhlet extraction.

  12. Extraction and GC determination of volatile aroma compounds from extracts of three plant species of the Apiaceae family

    NASA Astrophysics Data System (ADS)

    Stan, M.; Soran, M. L.; Varodi, C.; Lung, I.; Copolovici, L.; MǎruÅ£oiu, C.

    2013-11-01

    Parsley (Petroselinum crispum), dill (Anethum graveolens) and celery (Apium graveolens), three aromatic plants belonging to the Apiaceae (Umbelliferae) botanical family, were selected as sources of essential or volatile oils. Essential oils are composed of a large diversity of volatile aroma compounds. Plant-derived essential oils and extracts have long been used as natural agents in food preservation, pharmaceuticals and medicinal therapies. In the present study, the plant extracts from leaves of parsley, dill and celery, were obtained by maceration, ultrasound-assisted extraction and microwave-assisted extraction. All extractions were performed at 30°C, using different solvents (ethanol, diethyl ether, n-hexane) and solvent mixtures (1:1, v/v). The most effective solvent system for the extraction of volatile aroma compounds was diethyl ether - n-hexane (1:1, v/v). Extraction efficiency and determination of aroma volatiles were performed by GC-FID and GC-MS, respectively. The major volatile compounds present in plant extracts were myristicin, α-phellandrene, β-phellandrene, 1,3,8-p-menthatriene, apiol, dill ether and allyl phenoxyacetate.

  13. Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

    PubMed

    Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

    2015-09-01

    In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Radiolytic Treatment of the Next-Generation Caustic-Side Solvent Extraction (NGS) Solvent and its Effect on the NGS Process

    DOE PAGES

    Roach, Benjamin D.; Williams, Neil J.; Duncan, Nathan C.; ...

    2014-12-01

    We show in this work that the solvent used in the Next Generation Caustic-Side Solvent Extraction (NGS) process can withstand a radiation dose well in excess of the dose it would receive in multiple years of treating legacy salt waste at the US Department of Energy Savannah River Site. The solvent was subjected to a maximum of 50 kGy of gamma radiation while in dynamic contact with each of the aqueous phases of the current NGS process, namely SRS-15 (a highly caustic waste simulant), sodium hydroxide scrub solution (0.025 M), and boric acid strip solution (0.01 M). Bench-top testing ofmore » irradiated solvent confirmed that irradiation has inconsequential impact on the extraction, scrubbing, and stripping performance of the solvent up to 13 times the estimated 0.73 kGy/y annual absorbed dose. Lastly, stripping performance is the most sensitive step to radiation, deteriorating more due to buildup of p-sec-butylphenol (SBP) and possibly other proton-ionizable products than to degradation of the guanidine suppressor, as shown by chemical analyses.« less

  15. Radiolytic Treatment of the Next-Generation Caustic-Side Solvent Extraction (NGS) Solvent and its Effect on the NGS Process

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Roach, Benjamin D.; Williams, Neil J.; Duncan, Nathan C.

    We show in this work that the solvent used in the Next Generation Caustic-Side Solvent Extraction (NGS) process can withstand a radiation dose well in excess of the dose it would receive in multiple years of treating legacy salt waste at the US Department of Energy Savannah River Site. The solvent was subjected to a maximum of 50 kGy of gamma radiation while in dynamic contact with each of the aqueous phases of the current NGS process, namely SRS-15 (a highly caustic waste simulant), sodium hydroxide scrub solution (0.025 M), and boric acid strip solution (0.01 M). Bench-top testing ofmore » irradiated solvent confirmed that irradiation has inconsequential impact on the extraction, scrubbing, and stripping performance of the solvent up to 13 times the estimated 0.73 kGy/y annual absorbed dose. Lastly, stripping performance is the most sensitive step to radiation, deteriorating more due to buildup of p-sec-butylphenol (SBP) and possibly other proton-ionizable products than to degradation of the guanidine suppressor, as shown by chemical analyses.« less

  16. A pilot scale ultrasonic system to enhance extraction processes with dense gases

    NASA Astrophysics Data System (ADS)

    Riera, E.; Blasco, M.; Tornero, A.; Casas, E.; Roselló, C.; Simal, S.; Acosta, V. M.; Gallego-Juárez, J. A.

    2012-05-01

    The use of dense gases (supercritical fluids) as extracting agents has been attracting wide interest for years. In particular, supercritical carbon dioxide is considered nowadays as a green and very useful solvent. Nevertheless, the extraction process has a slow dynamics. Power ultrasound represents an efficient way for accelerating and enhancing the kinetics of the process by producing strong agitation and turbulence, compressions and decompressions, and heating in the media. For this purpose, a device prototype for using ultrasound in supercritical media was developed, tested and validated in extraction processes of oil from grounded almonds (55% oil content, wet basis and 3-4 mm particle size) in a 5 L extraction unit. An amount of 1500 g of grounded almonds was placed in a cylindrical basket during the trials inside the dense gas extractor (DGE) where solvent was introduced at different flow rates, pressures and temperatures. In all cases the ultrasonic energy confirmed the enhancement and acceleration of the almond oil extraction kinetics using supercritical CO2. Presently the power ultrasound effect in such a process is being deeply analyzed in a 5 L extraction unit before scaling-up a new ultrasonic system. This technology, still under development, has been designed for a bigger dense gas pilot-plant consisting of two extractors (20 L capacity), two separation units and has the possibility of operating at a pressure up to 50 MPa. The goal of this work is to study the effect of high-power ultrasound coupled to dense gas extraction inside the basket with the product, and to present a prototype for the use of power ultrasound in extraction processes with dense gases inside a new 20 L extractor unit.

  17. Organic Separation Test Results

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Russell, Renee L.; Rinehart, Donald E.; Peterson, Reid A.

    2014-09-22

    Separable organics have been defined as “those organic compounds of very limited solubility in the bulk waste and that can form a separate liquid phase or layer” (Smalley and Nguyen 2013), and result from three main solvent extraction processes: U Plant Uranium Recovery Process, B Plant Waste Fractionation Process, and Plutonium Uranium Extraction (PUREX) Process. The primary organic solvents associated with tank solids are TBP, D2EHPA, and NPH. There is concern that, while this organic material is bound to the sludge particles as it is stored in the tanks, waste feed delivery activities, specifically transfer pump and mixer pump operations,more » could cause the organics to form a separated layer in the tank farms feed tank. Therefore, Washington River Protection Solutions (WRPS) is experimentally evaluating the potential of organic solvents separating from the tank solids (sludge) during waste feed delivery activities, specifically the waste mixing and transfer processes. Given the Hanford Tank Waste Treatment and Immobilization Plant (WTP) waste acceptance criteria per the Waste Feed Acceptance Criteria document (24590-WTP-RPT-MGT-11-014) that there is to be “no visible layer” of separable organics in the waste feed, this would result in the batch being unacceptable to transfer to WTP. This study is of particular importance to WRPS because of these WTP requirements.« less

  18. Influence of sample processing on the analysis of carotenoids in maize.

    PubMed

    Rivera, Sol; Canela, Ramon

    2012-09-21

    We performed a number of tests with the aim to develop an effective extraction method for the analysis of carotenoid content in maize seed. Mixtures of methanol-ethyl acetate (6:4, v/v) and methanol-tetrahydrofuran (1:1, v/v) were the most effective solvent systems for carotenoid extraction from maize endosperm under the conditions assayed. In addition, we also addressed sample preparation prior to the analysis of carotenoids by liquid chromatography (LC). The LC response of extracted carotenoids and standards in several solvents was evaluated and results were related to the degree of solubility of these pigments. Three key factors were found to be important when selecting a suitable injection solvent: compatibility between the mobile phase and injection solvent, carotenoid polarity and content in the matrix.

  19. Extraction of polycyclic aromatic hydrocarbons and organochlorine pesticides from soils: a comparison between Soxhlet extraction, microwave-assisted extraction and accelerated solvent extraction techniques.

    PubMed

    Wang, Wentao; Meng, Bingjun; Lu, Xiaoxia; Liu, Yu; Tao, Shu

    2007-10-29

    The methods of simultaneous extraction of polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs) from soils using Soxhlet extraction, microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) were established, and the extraction efficiencies using the three methods were systemically compared from procedural blank, limits of detection and quantification, method recovery and reproducibility, method chromatogram and other factors. In addition, soils with different total organic carbon contents were used to test the extraction efficiencies of the three methods. The results showed that the values obtained in this study were comparable with the values reported by other studies. In some respects such as method recovery and reproducibility, there were no significant differences among the three methods for the extraction of PAHs and OCPs. In some respects such as procedural blank and limits of detection and quantification, there were significant differences among the three methods. Overall, ASE had the best extraction efficiency compared to MAE and Soxhlet extraction, and the extraction efficiencies of MAE and Soxhlet extraction were comparable to each other depending on the property such as TOC content of the studied soil. Considering other factors such as solvent consumption and extraction time, ASE and MAE are preferable to Soxhlet extraction.

  20. Effects of carbonization and solvent-extraction on change in fuel characteristics of sewage sludge.

    PubMed

    Park, Sang-Woo; Jang, Cheol-Hyeon

    2011-09-01

    Urban sewage sludge was carbonized at 300-500°C for 1h, and combustible components were extracted through the solvent-extraction process. N-methyl-2-pyrrolidinone (NMP) was used as the solvent for extraction, and the extraction temperature was fixed at 360°C. The atomic ratios of the solvent-extracted sludge of CS300 (ECS300) were shown to be 1.04 for H/C and 0.11 for O/C, which represented the characteristics of its coal band. Thus, its coal band was similar to that of a high-rank fuel such as bituminous coal. FT-IR analysis showed that the absorbance band of ECS300 was considerably different from that of dried sludge (RS) or the carbonized sludge at 300°C (CS300) but similar to that of coal, although the ash content absorbance band of 800-1200 cm(-1) was of very low intensity. The combustion profile showed that combustion of ESC300 occurred at a temperature higher than the ignition temperature (T(i)) or maximum weight loss rate (DTG(max)) of coal. Copyright © 2011 Elsevier Ltd. All rights reserved.

  1. Optimization of microwave-assisted extraction of polyphenols from Myrtus communis L. leaves.

    PubMed

    Dahmoune, Farid; Nayak, Balunkeswar; Moussi, Kamal; Remini, Hocine; Madani, Khodir

    2015-01-01

    Phytochemicals, such as phenolic compounds, are of great interest due to their health-benefitting antioxidant properties and possible protection against inflammation, cardiovascular diseases and certain types of cancer. Maximum retention of these phytochemicals during extraction requires optimised process parameter conditions. A microwave-assisted extraction (MAE) method was investigated for extraction of total phenolics from Myrtus communis leaves. The total phenolic capacity (TPC) of leaf extracts at optimised MAE conditions was compared with ultrasound-assisted extraction (UAE) and conventional solvent extraction (CSE). The influence of extraction parameters including ethanol concentration, microwave power, irradiation time and solvent-to-solid ratio on the extraction of TPC was modeled by using a second-order regression equation. The optimal MAE conditions were 42% ethanol concentration, 500 W microwave power, 62 s irradiation time and 32 mL/g solvent to material ratio. Ethanol concentration and liquid-to-solid ratio were the significant parameters for the extraction process (p<0.01). Under the MAE optimised conditions, the recovery of TPC was 162.49 ± 16.95 mg gallic acidequivalent/gdry weight(DW), approximating the predicted content (166.13 mg GAE/g DW). When bioactive phytochemicals extracted from Myrtus leaves using MAE compared with UAE and CSE, it was also observed that tannins (32.65 ± 0.01 mg/g), total flavonoids (5.02 ± 0.05 mg QE/g) and antioxidant activities (38.20 ± 1.08 μg GAE/mL) in MAE extracts were higher than the other two extracts. These findings further illustrate that extraction of bioactive phytochemicals from plant materials using MAE method consumes less extraction solvent and saves time. Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Low solvent, low temperature method for extracting biodiesel lipids from concentrated microalgal biomass.

    PubMed

    Olmstead, Ian L D; Kentish, Sandra E; Scales, Peter J; Martin, Gregory J O

    2013-11-01

    An industrially relevant method for disrupting microalgal cells and preferentially extracting neutral lipids for large-scale biodiesel production was demonstrated on pastes (20-25% solids) of Nannochloropsis sp. The highly resistant Nannochloropsis sp. cells. were disrupted by incubation for 15 h at 37°C followed by high pressure homogenization at 1200 ± 100 bar. Lipid extraction was performed by twice contacting concentrated algal paste with minimal hexane (solvent:biomass ratios (w/w) of <2:1 and <1.3:1) in a stirred vessel at 35°C. Cell disruption prior to extraction increased lipid recovery 100-fold, with yields of 30-50% w/w obtained in the first hexane contact, and a further 6.5-20% in the second contact. The hexane preferentially extracted neutral lipids over glyco- and phospholipids, with up to 86% w/w of the neutral lipids recovered. The process was effective on wet concentrated paste, required minimal solvent and moderate temperature, and did not require difficult to recover polar solvents. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Headspace, volatile and semi-volatile organic compounds diversity and radical scavenging activity of ultrasonic solvent extracts from Amorpha fruticosa honey samples.

    PubMed

    Jerković, Igor; Marijanović, Zvonimir; Kezić, Janja; Gugić, Mirko

    2009-07-27

    Volatile organic compounds of Amorpha fruticosa honey samples were isolated by headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE), followed by gas chromatography and mass spectrometry analyses (GC, GC-MS), in order to obtain complementary data for overall characterization of the honey aroma. The headspace of the honey was dominated by 2-phenylethanol (38.3-58.4%), while other major compounds were trans- and cis-linalool oxides, benzaldehyde and benzyl alcohol. 2-Phenylethanol (10.5-16.8%) and methyl syringate (5.8-8.2%) were the major compounds of ultrasonic solvent extracts, with an array of small percentages of linalool, benzene and benzoic acid derivatives, aliphatic hydrocarbons and alcohols, furan derivatives and others. The scavenging ability of the series of concentrations of the honey ultrasonic solvent extracts and the corresponding honey samples was tested by a DPPH (1,1-diphenyl-2-picrylhydrazyl) assay. Approximately 25 times lower concentration ranges (up to 2 g/L) of the extracts exhibited significantly higher free radical scavenging potential with respect to the honey samples.

  4. Optimization of extraction parameters of pentacyclic triterpenoids from Swertia chirata stem using response surface methodology.

    PubMed

    Pandey, Devendra Kumar; Kaur, Prabhjot

    2018-03-01

    In the present investigation, pentacyclic triterpenoids were extracted from different parts of Swertia chirata by solid-liquid reflux extraction methods. The total pentacyclic triterpenoids (UA, OA, and BA) in extracted samples were determined by HPTLC method. Preliminary studies showed that stem part contains the maximum pentacyclic triterpenoid and was chosen for further studies. Response surface methodology (RSM) has been employed successfully by solid-liquid reflux extraction methods for the optimization of different extraction variables viz., temperature ( X 1 35-70 °C), extraction time ( X 2 30-60 min), solvent composition ( X 3 20-80%), solvent-to-solid ratio ( X 4 30-60 mlg -1 ), and particle size ( X 5 3-6 mm) on maximum recovery of triterpenoid from stem parts of Swertia chirata . A Plackett-Burman design has been used initially to screen out the three extraction factors viz., particle size, temperature, and solvent composition on yield of triterpenoid. Moreover, central composite design (CCD) was implemented to optimize the significant extraction parameters for maximum triterpenoid yield. Three extraction parameters viz., mean particle size (3 mm), temperature (65 °C), and methanol-ethyl acetate solvent composition (45%) can be considered as significant for the better yield of triterpenoid A second-order polynomial model satisfactorily fitted the experimental data with the R 2 values of 0.98 for the triterpenoid yield ( p  < 0.001), implying good agreement between the experimental triterpenoid yield (3.71%) to the predicted value (3.79%).

  5. Electro-driven extraction of inorganic anions from water samples and water miscible organic solvents and analysis by ion chromatography.

    PubMed

    Nojavan, Saeed; Bidarmanesh, Tina; Memarzadeh, Farkhondeh; Chalavi, Soheila

    2014-09-01

    A simple electromembrane extraction (EME) procedure combined with ion chromatography (IC) was developed to quantify inorganic anions in different pure water samples and water miscible organic solvents. The parameters affecting extraction performance, such as supported liquid membrane (SLM) solvent, extraction time, pH of donor and acceptor solutions, and extraction voltage were optimized. The optimized EME conditions were as follows: 1-heptanol was used as the SLM solvent, the extraction time was 10 min, pHs of the acceptor and donor solutions were 10 and 7, respectively, and the extraction voltage was 15 V. The mobile phase used for IC was a combination of 1.8 mM sodium carbonate and 1.7 mM sodium bicarbonate. Under these optimized conditions, all anions had enrichment factors ranging from 67 to 117 with RSDs between 7.3 and 13.5% (n = 5). Good linearity values ranging from 2 to 1200 ng/mL with coefficients of determination (R(2) ) between 0.987 and 0.999 were obtained. The LODs of the EME-IC method ranged from 0.6 to 7.5 ng/mL. The developed method was applied to different samples to evaluate the feasibility of the method for real applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Displacement-dispersive liquid-liquid microextraction based on solidification of floating organic drop of trace amounts of palladium in water and road dust samples prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Ghanbarian, Maryam; Afzali, Daryoush; Mostafavi, Ali; Fathirad, Fariba

    2013-01-01

    A new displacement-dispersive liquid-liquid microextraction method based on the solidification of floating organic drop was developed for separation and preconcentration of Pd(ll) in road dust and aqueous samples. This method involves two steps of dispersive liquid-liquid microextraction based on solidification. In Step 1, Cu ions react with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which is extracted by dispersive liquid-liquid microextraction based on a solidification procedure using 1-undecanol (extraction solvent) and ethanol (dispersive solvent). In Step 2, the extracted complex is first dispersed using ethanol in a sample solution containing Pd ions, then a dispersive liquid-liquid microextraction based on a solidification procedure is performed creating an organic drop. In this step, Pd(ll) replaces Cu(ll) from the pre-extracted Cu-DDTC complex and goes into the extraction solvent phase. Finally, the Pd(ll)-containing drop is introduced into a graphite furnace using a microsyringe, and Pd(ll) is determined using atomic absorption spectrometry. Several factors that influence the extraction efficiency of Pd and its subsequent determination, such as extraction and dispersive solvent type and volume, pH of sample solution, centrifugation time, and concentration of DDTC, are optimized.

  7. Superfund Innovative Technology Evaluation: Demonstration Bulletin: Organic Extraction Utilizing Solvents

    EPA Science Inventory

    This technology utilizes liquified gases as the extracting solvent to remove organics, such as hydrocarbons, oil and grease, from wastewater or contaminated sludges and soils. Carbon dioxide is generally used for aqueous solutions, and propane is used for sediment, sludges and ...

  8. Solvent Extraction for Vegetable Oil Production: National Emission Standards for Hazardous Air Pollutants (NESHAP)

    EPA Pesticide Factsheets

    The EPA has identified solvent extraction for vegetable oil production processes as major sources of a single hazardous air pollutant (HAP), n-hexane. Learn more about the rule requirements and regulations, as well as find compliance help

  9. Pressurized solvent extraction of pure food grade starch

    USDA-ARS?s Scientific Manuscript database

    A commercial pressurized solvent extractor was used to remove lipid and non-lipid material from cornstarch using n-propanol/water and ethanol/water mixtures. Yields and chemical composition of the extract fractions were determined. Cornstarch samples were characterized using pasting properties and...

  10. Steam distillation/drop-by-drop extraction with gas chromatography-mass spectrometry for fast determination of volatile components in jujube (Ziziphus jujuba Mill.) extract.

    PubMed

    Sun, Shi-Hao; Chai, Guo-Bi; Li, Peng; Xie, Jian-Ping; Su, Yue

    2017-10-13

    Jujube extract is commonly used as a food additive and flavoring. The unique jujube aroma and the mild sweet aroma of the extract are critical factors that determine product quality and affect consumer acceptability. The aroma changes with changes in the extraction condition, which is typically dependent on the characteristics of volatile oils in the extract. Despite their importance, the volatile oils of jujube extract have received less attention compared with the soluble components. So, an appropriate qualitative and quantitative method for determination of the volatile oils is vitally important for quality control of the product. A method coupling steam distillation/drop-by-drop extraction with gas chromatography-mass spectrometry (S3DE/GC-MS) was developed to determine the volatile components of jujube extract. Steam distillation was coupled with solvent extraction; the resulting condensate containing volatile components from jujube extract was drop-by-drop extracted using 2 mL of methyl tertiary butyl ether. The solvent served two purposes. First, the solvent extracted the volatile components from the condensate. Second, the volatile components were pre-concentrated by drop-by-drop accumulation in the solvent. As a result, the extraction, separation, and concentration of analytes in the sample were simultaneously completed in one step. The main parameters affecting the S3DE procedure, such as the water steam bubbling rate, extraction solvent volume, sample weight and S3DE time, were optimized. The standard addition approach was essential to obtain accurate measurements by minimizing matrix effects. Good linearity (R 2  ≥ 0.9887) and good repeatability (RSDs ≤ 10.35%, n = 5) for 16 analytes in spiked standard analyte samples were achieved. With the S3DE/GC-MS method, seventy-six volatile compounds from jujube extract were identified and the content of 16 compounds was measured. The results were similar to those from simultaneous distillation extraction. The developed method was simple, fast, effective, sensitive, and provided an overall profile of the volatile components in jujube extract. Thus, this method can be used to determine the volatile components of extracts. Graphical abstract The diagram of steam distillation/drop-by-drop extraction device.

  11. PRELIMINARY EVALUATION OF DWPF IMPACTS OF BORIC ACID USE IN CESIUM STRIP FOR SWPF AND MCU

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Stone, M.

    2010-09-28

    A new solvent system is being evaluated for use in the Modular Caustic-Side Solvent Extraction Unit (MCU) and in the Salt Waste Processing Facility (SWPF). The new system includes the option to replace the current dilute nitric acid strip solution with boric acid. To support this effort, the impact of using 0.01M, 0.1M, 0.25M and 0.5M boric acid in place of 0.001M nitric acid was evaluated for impacts on the DWPF facility. The evaluation only covered the impacts of boric acid in the strip effluent and does not address the other changes in solvents (i.e., the new extractant, called MaxCalix,more » or the new suppressor, guanidine). Boric acid additions may lead to increased hydrogen generation during the SRAT and SME cycles as well as change the rheological properties of the feed. The boron in the strip effluent will impact glass composition and could require each SME batch to be trimmed with boric acid to account for any changes in the boron from strip effluent additions. Addition of boron with the strip effluent will require changes in the frit composition and could lead to changes in melt behavior. The severity of the impacts from the boric acid additions is dependent on the amount of boric acid added by the strip effluent. The use of 0.1M or higher concentrations of boric acid in the strip effluent was found to significantly impact DWPF operations while the impact of 0.01M boric acid is expected to be relatively minor. Experimental testing is required to resolve the issues identified during the preliminary evaluation. The issues to be addressed by the testing are: (1) Impact on SRAT acid addition and hydrogen generation; (2) Impact on melter feed rheology; (3) Impact on glass composition control; (4) Impact on frit production; and (5) Impact on melter offgas. A new solvent system is being evaluated for use in the Modular Caustic-Side Solvent Extraction Unit (MCU) and in the Salt Waste Processing Facility (SWPF). The new system includes the option to replace the current dilute nitric acid strip solution with boric acid. To support this effort, the impact of using 0.01M, 0.1M, 0.25M and 0.5M boric acid in place of 0.001M nitric acid was evaluated for impacts on the DWPF facility. The evaluation only covered the impacts of boric acid in the strip effluent and does not address the other changes in solvents (i.e., the new extractant, called MaxCalix, or the new suppressor, guanidine). Experimental testing with the improved solvent is required to determine the impact of any changes in the entrained solvent on DWPF processing.« less

  12. SOLVENT HOLD TANK SAMPLE RESULTS FOR MCU-11-1452, MCU-11-1453, MCU-11-1454, MCU-11-1455, MCU-11-1456 AND MCU-11-1457

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, T.; Fondeur, F.; Fink, S.

    Solvent Hold Tank (SHT) samples are sent to Savannah River National Laboratory (SRNL) to examine solvent composition changes over time. On December 5, 2011, Operations personnel delivered six samples from the SHT (MCU-11-1452 through -1457) for analysis. These samples are intended to verify that the solvent is within the specified composition range. The results from the analyses are presented in this document. Samples were received in p-nut vials containing {approx}10 mL each. Once taken into the Shielded Cells, the samples were combined. Samples were removed for analysis by density, semi-volatile organic analysis (SVOA), high performance liquid chromatography (HPLC), and Fourier-Transformmore » Infra-Red spectroscopy (FTIR). Details for the work are contained in a controlled laboratory notebook. Each of the six p-nut vials contained a single phase, with no apparent solids contamination or cloudiness. Table 1 contains the results of the analyses for the combined samples. A duplicate density measurement of the organic phase gave a result of 0.844 g/mL (1.2% residual standard deviation - RSD). Using the density as a starting point, we know that the Isopar{reg_sign} L should be slightly higher than nominal and the other components should be slightly lower than nominal. The results as a whole are internally consistent. All measurements indicate Isopar{reg_sign} L higher than nominal, and Modifier lower than nominal. The extractant result is higher than expected - given the other results, the extractant concentration should be under nominal values. Using the measured density as well as the Isopar{reg_sign} L and Modifier concentrations from the FTIR results, we calculate an extractant concentration of 6888 mg/L. This value is outside the analytical uncertainty of the reported HPLC value. Given the other results, this most likely indicates that the HPLC extractant result was biased high. When compared to the MCU density target of 0.845 g/mL, there is no need to add an Isopar{reg_sign} L trim. However, it is advisable to add sufficient trioctylamine (TOA) to return the solvent composition to within specifications as that component has declined to about 64% the concentration since the last analysis. The TOA measurement was performed twice, so the result is not an analytical aberration. TOA has not been added to the system since the previous quarterly sample in October 2011. As with the previous solvent sample results, these analyses indicate that the solvent does not require Isopar{reg_sign} L trimming at this time. However, addition of TOA is warranted. These findings indicate that the new protocols for solvent monitoring and control are yielding favorable results. Nevertheless, the deviation in the TOA concentration since the last analysis indicates continued periodic (i.e., quarterly) monitoring is recommended.« less

  13. Evaluation of extraction protocols for anti-diabetic phytochemical substances from medicinal plants.

    PubMed

    Okoduwa, Stanley Irobekhian Reuben; Umar, Ismaila A; James, Dorcas B; Inuwa, Hajara M; Habila, James D

    2016-12-15

    To examine the efficacy of three extraction techniques: Soxhlet-extraction (SE), cold-maceration (CM) and microwave-assisted-extraction (MAE) using 80% methanol as solvent. The study was performed on each of 50 g of Vernonia amygdalina (VA) and Occimum gratissimum (OG) leaves respectively. The percentage yield, duration of extraction, volume of solvent used, qualitative and quantitative phytoconstituents present was compared. The biological activities (hypoglycemic effect) were investigated using albino wistar rat model of diabetes mellitus ( n = 36) with a combined dose (1:1) of the two plants leaf extracts (250 mg/kg b.w.) from the three methods. The extracts were administered orally, once daily for 21 d. In this report, the percentage VA extract yield from MAE was highest (20.9% ± 1.05%) within 39 min using 250 mL of solvent, when compared to the CM (14.35% ± 0.28%) within 4320 min using 900 mL of solvent and SE (15.75% ± 0.71%) within 265 min using 500 mL of solvent. The percentage differences in OG extract yield between: MAE vs SE was 41.05%; MAE vs CM was 46.81% and SE vs CM was 9.77%. The qualitative chemical analysis of the two plants showed no difference in the various phytoconstituents tested, but differs quantitatively in the amount of the individual phytoconstituents, as MAE had significantly high yield ( P > 0.05) on phenolics, saponins and tannins. SE technique gave significantly high yield ( P > 0.05) on alkaloid, while CM gave significant high yield on flavonoids. The extracts from CM exhibited a significantly ( P > 0.05) better hypoglycemic activity within the first 14-d of treatment (43.3% ± 3.62%) when compared to MAE (36.5% ± 0.08%) and SE methods (33.3% ± 1.60%). However, the percentage hypoglycemic activity, 21 d post-treatment with 250 mg/kg b.w. extract from MAE was 72.6% ± 1.03% and it was more comparable to 10 mg/kg b.w. glibenclamide treated group (75.0% ± 0.73%), unlike the SE (69.5% ± 0.71%) and CM (69.1% ± 1.03%). CM technique produces extract with better hypoglycemic activity, whereas; MAE is a better option for high yield of phytoconstituents using less solvent within a short time.

  14. Evaluation of extraction protocols for anti-diabetic phytochemical substances from medicinal plants

    PubMed Central

    Okoduwa, Stanley Irobekhian Reuben; Umar, Ismaila A; James, Dorcas B; Inuwa, Hajara M; Habila, James D

    2016-01-01

    AIM To examine the efficacy of three extraction techniques: Soxhlet-extraction (SE), cold-maceration (CM) and microwave-assisted-extraction (MAE) using 80% methanol as solvent. METHODS The study was performed on each of 50 g of Vernonia amygdalina (VA) and Occimum gratissimum (OG) leaves respectively. The percentage yield, duration of extraction, volume of solvent used, qualitative and quantitative phytoconstituents present was compared. The biological activities (hypoglycemic effect) were investigated using albino wistar rat model of diabetes mellitus (n = 36) with a combined dose (1:1) of the two plants leaf extracts (250 mg/kg b.w.) from the three methods. The extracts were administered orally, once daily for 21 d. RESULTS In this report, the percentage VA extract yield from MAE was highest (20.9% ± 1.05%) within 39 min using 250 mL of solvent, when compared to the CM (14.35% ± 0.28%) within 4320 min using 900 mL of solvent and SE (15.75% ± 0.71%) within 265 min using 500 mL of solvent. The percentage differences in OG extract yield between: MAE vs SE was 41.05%; MAE vs CM was 46.81% and SE vs CM was 9.77%. The qualitative chemical analysis of the two plants showed no difference in the various phytoconstituents tested, but differs quantitatively in the amount of the individual phytoconstituents, as MAE had significantly high yield (P > 0.05) on phenolics, saponins and tannins. SE technique gave significantly high yield (P > 0.05) on alkaloid, while CM gave significant high yield on flavonoids. The extracts from CM exhibited a significantly (P > 0.05) better hypoglycemic activity within the first 14-d of treatment (43.3% ± 3.62%) when compared to MAE (36.5% ± 0.08%) and SE methods (33.3% ± 1.60%). However, the percentage hypoglycemic activity, 21 d post-treatment with 250 mg/kg b.w. extract from MAE was 72.6% ± 1.03% and it was more comparable to 10 mg/kg b.w. glibenclamide treated group (75.0% ± 0.73%), unlike the SE (69.5% ± 0.71%) and CM (69.1% ± 1.03%). CONCLUSION CM technique produces extract with better hypoglycemic activity, whereas; MAE is a better option for high yield of phytoconstituents using less solvent within a short time. PMID:28031778

  15. Development of a process for the extraction of {sup 137}Cs from acidic HLLW based on crown-calix extractant use of di-alkylamide modifier

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Alexova, J.; Sirova, M.; Rais, J.

    2008-07-01

    Within the framework of the ARTIST project of total fuel retreatment with ecological mixtures of solvents and extractants containing only C, H, O, and N atoms, a process segment of extraction of {sup 137}Cs from acidic stream was developed. The process with 25,27-Bis(1-octyloxy)calix[4]arene-crown- 6, DOC[4]C6, dissolved at its 0.01 M concentration in a mixture of 90 vol % 1-octanol and 10% dihexyl octanamide, DHOA was proposed as a viable variant due to its good multicycle performance, even with irradiated solvent, and due to the good chemical stability of the chosen combination of solvent mixture. (authors)

  16. Self-immobilization of poly(methyloctylsiloxane) on high-performance liquid chromatographic silica.

    PubMed

    Collins, Kenneth E; Bottoli, Carla B G; Vigna, Camila R M; Bachmann, Stefan; Albert, Klaus; Collins, Carol H

    2004-03-12

    Poly(methyloctylsiloxane) (PMOS) was deposited on HPLC silica by a solvent evaporation procedure and this material was then extracted, using a good solvent for the PMOS, after different time periods, to remove unretained liquid polymer. Solvent extraction data reveal changes which occur at ambient temperature as a function of the time interval between particle loading and extraction. The quantity of PMOS remaining on the silica after extraction, as determined by elemental analysis for carbon, is attributed to strongly adsorbed polymer. This phenomenon is termed self-immobilization. Solid-state 29Si NMR spectra indicate the formation of a silicon species with a different chemical shift than the original PMOS. These new signals are attributed to a combination of different adsorbed and chemically bonded groups.

  17. Techno-economic assessment of hybrid extraction and distillation processes for furfural production from lignocellulosic biomass.

    PubMed

    Nhien, Le Cao; Long, Nguyen Van Duc; Kim, Sangyong; Lee, Moonyong

    2017-01-01

    Lignocellulosic biomass is one of the most promising alternatives for replacing mineral resources to overcome global warming, which has become the most important environmental issue in recent years. Furfural was listed by the National Renewable Energy Laboratory as one of the top 30 potential chemicals arising from biomass. However, the current production of furfural is energy intensive and uses inefficient technology. Thus, a hybrid purification process that combines extraction and distillation to produce furfural from lignocellulosic biomass was considered and investigated in detail to improve the process efficiency. This effective hybrid process depends on the extracting solvent, which was selected based on a comprehensive procedure that ranged from solvent screening to complete process design. Various solvents were first evaluated in terms of their extraction ability. Then, the most promising solvents were selected to study the separation feasibility. Eventually, processes that used the three best solvents (toluene, benzene, and butyl chloride) were designed and optimized in detail using Aspen Plus. Sustainability analysis was performed to evaluate these processes in terms of their energy requirements, total annual costs (TAC), and carbon dioxide (CO 2 ) emissions. The results showed that butyl chloride was the most suitable solvent for the hybrid furfural process because it could save 44.7% of the TAC while reducing the CO 2 emissions by 45.5% compared to the toluene process. In comparison with the traditional purification process using distillation, this suggested hybrid extraction/distillation process can save up to 19.2% of the TAC and reduce 58.3% total annual CO 2 emissions. Furthermore, a sensitivity analysis of the feed composition and its effect on the performance of the proposed hybrid system was conducted. Butyl chloride was found to be the most suitable solvent for the hybrid extraction/distillation process of furfural production. The proposed hybrid sequence was more favorable than the traditional distillation process when the methanol fraction of the feed stream was <3% and more benefit could be obtained when that fraction decreased.

  18. Alcohol based-deep eutectic solvent (DES) as an alternative green additive to increase rotenone yield

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Othman, Zetty Shafiqa; Hassan, Nur Hasyareeda; Zubairi, Saiful Irwan

    Deep eutectic solvents (DESs) are basically molten salts that interact by forming hydrogen bonds between two added components at a ratio where eutectic point reaches a melting point lower than that of each individual component. Their remarkable physicochemical properties (similar to ionic liquids) with remarkable green properties, low cost and easy handling make them a growing interest in many fields of research. Therefore, the objective of pursuing this study is to analyze the potential of alcohol-based DES as an extraction medium for rotenone extraction from Derris elliptica roots. DES was prepared by a combination of choline chloride, ChCl and 1,more » 4-butanediol at a ratio of 1/5. The structure of elucidation of DES was analyzed using FTIR, {sup 1}H-NMR and {sup 13}C-NMR. Normal soaking extraction (NSE) method was carried out for 14 hours using seven different types of solvent systems of (1) acetone; (2) methanol; (3) acetonitrile; (4) DES; (5) DES + methanol; (6) DES + acetonitrile; and (7) [BMIM] OTf + acetone. Next, the yield of rotenone, % (w/w), and its concentration (mg/ml) in dried roots were quantitatively determined by means of RP-HPLC. The results showed that a binary solvent system of [BMIM] OTf + acetone and DES + acetonitrile was the best solvent system combination as compared to other solvent systems. It contributed to the highest rotenone content of 0.84 ± 0.05% (w/w) (1.09 ± 0.06 mg/ml) and 0.84 ± 0.02% (w/w) (1.03 ± 0.01 mg/ml) after 14 hours of exhaustive extraction time. In conclusion, a combination of the DES with a selective organic solvent has been proven to have a similar potential and efficiency as of ILs in extracting bioactive constituents in the phytochemical extraction process.« less

  19. Accelerated solvent extraction of carotenoids from: Tunisian Kaki (Diospyros kaki L.), peach (Prunus persica L.) and apricot (Prunus armeniaca L.).

    PubMed

    Zaghdoudi, Khalil; Pontvianne, Steve; Framboisier, Xavier; Achard, Mathilde; Kudaibergenova, Rabiga; Ayadi-Trabelsi, Malika; Kalthoum-Cherif, Jamila; Vanderesse, Régis; Frochot, Céline; Guiavarc'h, Yann

    2015-10-01

    Extraction of carotenoids from biological matrices and quantifications remains a difficult task. Accelerated solvent extraction was used as an efficient extraction process for carotenoids extraction from three fruits cultivated in Tunisia: kaki (Diospyros kaki L.), peach (Prunus persica L.) and apricot (Prunus armeniaca L.). Based on a design of experiment (DoE) approach, and using a binary solvent consisting of methanol and tetrahydrofuran, we could identify the best extraction conditions as being 40°C, 20:80 (v:v) methanol/tetrahydrofuran and 5 min of extraction time. Surprisingly and likely due to the high extraction pressure used (103 bars), these conditions appeared to be the best ones both for extracting xanthophylls such as lutein, zeaxanthin or β-cryptoxanthin and carotenes such as β-carotene, which present quite different polarities. Twelve surface responses were generated for lutein, zeaxanthin, β-cryptoxanthin and β-carotene in kaki, peach and apricot. Further LC-MS analysis allowed comparisons in carotenoids profiles between the fruits. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Measurement of polychlorinated biphenyls in solid waste such as transformer insulation paper by supercritical fluid extraction and gas chromatography electron capture detection.

    PubMed

    Chikushi, Hiroaki; Fujii, Yuka; Toda, Kei

    2012-09-21

    In this work, a method for measuring polychlorinated biphenyls (PCBs) in contaminated solid waste was investigated. This waste includes paper that is used in electric transformers to insulate electric components. The PCBs in paper sample were extracted by supercritical fluid extraction and analyzed by gas chromatography-electron capture detection. The recoveries with this method (84-101%) were much higher than those with conventional water extraction (0.08-14%), and were comparable to those with conventional organic solvent extraction. Limit of detection was 0.0074 mg kg(-1) and measurable up to 2.5 mg kg(-1) for 0.5 g of paper sample. Data for real insulation paper by the proposed method agreed well with those by the conventional organic solvent extraction. Extraction from wood and concrete was also investigated and good performance was obtained as well as for paper samples. The supercritical fluid extraction is simpler, faster, and greener than conventional organic solvent extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Forensic analysis of anthraquinone, azo, and metal complex acid dyes from nylon fibers by micro-extraction and capillary electrophoresis.

    PubMed

    Stefan, Amy R; Dockery, Christopher R; Nieuwland, Alexander A; Roberson, Samantha N; Baguley, Brittany M; Hendrix, James E; Morgan, Stephen L

    2009-08-01

    The extraction and separation of dyes present on textile fibers offers the possibility of enhanced discrimination between forensic trace fiber evidence. An automated liquid sample handling workstation was programmed to deliver varying solvent combinations to acid-dyed nylon samples, and the resulting extracts were analyzed by an ultraviolet/visible microplate reader to evaluate extraction efficiencies at different experimental conditions. Combinatorial experiments using three-component mixture designs varied three solvents (water, pyridine, and aqueous ammonia) and were employed at different extraction temperatures for various extraction durations. The extraction efficiency as a function of the three solvents (pyridine/ammonia/water) was modeled and used to define optimum conditions for the extraction of three subclasses of acid dyes (anthraquinone, azo, and metal complex) from nylon fibers. The capillary electrophoresis analysis of acid dye extracts is demonstrated using an electrolyte solution of 15 mM ammonium acetate in acetonitrile/water (40:60, v/v) at pH 9.3. Excellent separations and discriminating diode array spectra are obtained even for dyes of similar color.

  2. Chromatographic and mass spectrometric characterization of essential oils and extracts from Lippia (Verbenaceae) aromatic plants.

    PubMed

    Stashenko, Elena E; Martínez, Jairo R; Cala, Mónica P; Durán, Diego C; Caballero, Deyanira

    2013-01-01

    Analytical methodologies based on GC and HPLC were developed for the separation and quantification of carnosic acid, ursolic acid, caffeic acid, p-coumaric acid, rosmarinic acid, apigenin, luteolin, quercetin, kaempferol, naringenin, and pinocembrin. These methods were used to characterize essential oils and extracts obtained by solvent (methanol) and by supercritical fluid (CO(2)) extraction from stems and leaves of Lippia (Verbenaceae family) aromatic plants (Lippia alba, Lippia origanoides, Lippia micromera, Lippia americana, Lippia graveolens, and Lippia citriodora). Supercritical CO(2) extraction isolated solely pinocembrin and narigenin from three L. origanoides chemotypes. Solvent extracts possessed a more varied composition that additionally included apigenin, quercetin, and luteolin. Solvent extraction afforded higher overall flavonoid yields from all species in comparison with supercritical CO(2) extraction. Pinocembrin was determined in L. origanoides extract at a concentration of 30 mg/g of plant material, which is more than ten times higher than the amount at which polyphenols are regularly found in aromatic plant extracts. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Determination of zearalenone and its metabolites in endometrial cancer by coupled separation techniques.

    PubMed

    Gadzała-Kopciuch, Renata; Cendrowski, Krzysztof; Cesarz, Anna; Kiełbasa, Paweł; Buszewski, Bogusław

    2011-10-01

    This study presents a selective method of isolation of zearalenone (ZON) and its metabolite, α-zearalenol (α-ZOL), in neoplastically changed human tissue by accelerated solvent and ultrasonic extractions using a mixture of acetonitrile/water (84/16% v/v) as the extraction solvent. Extraction effectiveness was determined through the selection of parameters (composition of the solvent mixture, temperature, pressure, number of cycles) with tissue contamination at the level of nanograms per gram. The produced acetonitrile/water extracts were purified, and analytes were enriched in columns packed with homemade molecularly imprinted polymers. Purified extracts were determined by liquid chromatography (LC) coupled with different detection systems (diode array detection--DAD and mass spectrometry--MS) involving the Ascentis RP-Amide as a stationary phase and gradient elution. The combination of UE-MISPE-LC (ultrasonic extraction--molecularly imprinted solid-phase extraction--liquid chromatography) produced high (R≈95-98%) and repeatable (RSD<3%) recovery values for ZON and α-ZOL. © The Author(s) 2011. This article is published with open access at Springerlink.com

  4. Dynamic microwave assisted extraction coupled with dispersive micro-solid-phase extraction of herbicides in soybeans.

    PubMed

    Li, Na; Wu, Lijie; Nian, Li; Song, Ying; Lei, Lei; Yang, Xiao; Wang, Kun; Wang, Zhibing; Zhang, Liyuan; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei

    2015-09-01

    Non-polar solvent dynamic microwave assisted extraction was firstly applied to the treatment of high-fat soybean samples. In the dispersive micro-solid-phase extraction (D-µ-SPE), the herbicides in the high-fat extract were directly adsorbed on metal-organic frameworks MIL-101(Cr). The effects of several experimental parameters, including extraction solvent, microwave absorption medium, microwave power, volume and flow rate of extraction solvent, amount of MIL-101(Cr), and D-µ-SPE time, were investigated. At the optimal conditions, the limits of detection for the herbicides ranged from 1.56 to 2.00 μg kg(-1). The relative recoveries of the herbicides were in the range of 91.1-106.7%, and relative standard deviations were equal to or lower than 6.7%. The present method was simple, rapid and effective. A large amount of fat was also removed. This method was demonstrated to be suitable for treatment of high-fat samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Extractant composition including crown ether and calixarene extractants

    DOEpatents

    Meikrantz, David H.; Todd, Terry A.; Riddle, Catherine L.; Law, Jack D.; Peterman, Dean R.; Mincher, Bruce J.; McGrath, Christopher A.; Baker, John D.

    2009-04-28

    An extractant composition comprising a mixed extractant solvent consisting of calix[4] arene-bis-(tert-octylbenzo)-crown-6 ("BOBCalixC6"), 4',4',(5')-di-(t-butyldicyclo-hexano)-18-crown-6 ("DtBu18C6"), and at least one modifier dissolved in a diluent. The DtBu18C6 may be present at from approximately 0.01M to approximately 0.4M, such as at from approximately 0.086 M to approximately 0.108 M. The modifier may be 1-(2,2,3,3-tetrafluoropropoxy)-3-(4-sec-butylphenoxy)-2-propanol ("Cs-7SB") and may be present at from approximately 0.01M to approximately 0.8M. In one embodiment, the mixed extractant solvent includes approximately 0.15M DtBu18C6, approximately 0.007M BOBCalixC6, and approximately 0.75M Cs-7SB modifier dissolved in an isoparaffinic hydrocarbon diluent. The extractant composition further comprises an aqueous phase. The mixed extractant solvent may be used to remove cesium and strontium from the aqueous phase.

  6. DOE Office of Scientific and Technical Information (OSTI.GOV)

    Harman-Ware, Anne E.; Sykes, Robert; Peter, Gary F.

    Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts frommore » the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. In conclusion, diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.« less

  7. "Solvent-free" ultrasound-assisted extraction of lipids from fresh microalgae cells: a green, clean and scalable process.

    PubMed

    Adam, Fanny; Abert-Vian, Maryline; Peltier, Gilles; Chemat, Farid

    2012-06-01

    In order to comply with criteria of green chemistry concepts and sustainability, a new procedure has been performed for solvent-free ultrasound-assisted extraction (UAE) to extract lipids from fresh Nannochloropsis oculata biomass. Through response surface methodology (RSM) parameters affecting the oil recovery were optimized. Optimum conditions for oil extraction were estimated as follows: (i) 1000 W ultrasonic power, (ii) 30 min extraction time and (iii) biomass dry weight content at 5%. Yields were calculated by the total fatty acids methyl esters amounts analyzed by GC-FID-MS. The maximum oil recovery was around 0.21%. This value was compared with the one obtained with the conventional extraction method (Bligh and Dyer). Furthermore, effect of temperature on the yield was also investigated. The overall results show an innovative and effective extraction method adapted for microalgae oil recovery, without using solvent and with an enable scaling up. Copyright © 2012 Elsevier Ltd. All rights reserved.

  8. Dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by high-performance liquid chromatography with ultraviolet detection and liquid chromatography-tandem mass spectrometry for the determination of triclosan and 2,4-dichlorophenol in water samples.

    PubMed

    Zheng, Cao; Zhao, Jing; Bao, Peng; Gao, Jin; He, Jin

    2011-06-24

    A novel, simple and efficient dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) technique coupled with high-performance liquid chromatography with ultraviolet detection (HPLC-UV) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of triclosan and its degradation product 2,4-dichlorophenol in real water samples. The extraction solvent used in this work is of low density, low volatility, low toxicity and proper melting point around room temperature. The extractant droplets can be collected easily by solidifying it at a lower temperature. Parameters that affect the extraction efficiency, including type and volume of extraction solvent and dispersive solvent, salt effect, pH and extraction time, were investigated and optimized in a 5 mL sample system by HPLC-UV. Under the optimum conditions (extraction solvent: 12 μL of 1-dodecanol; dispersive solvent: 300 of μL acetonitrile; sample pH: 6.0; extraction time: 1 min), the limits of detection (LODs) of the pretreatment method combined with LC-MS/MS were in the range of 0.002-0.02 μg L(-1) which are lower than or comparable with other reported approaches applied to the determination of the same compounds. Wide linearities, good precisions and satisfactory relative recoveries were also obtained. The proposed technique was successfully applied to determine triclosan and 2,4-dichlorophenol in real water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Assessment of critical-fluid extractions in the process industries

    NASA Technical Reports Server (NTRS)

    1982-01-01

    The potential for critical-fluid extraction as a separation process for improving the productive use of energy in the process industries is assessed. Critical-fluid extraction involves the use of fluids, normally gaseous at ambient conditions, as extraction solvents at temperatures and pressures around the critical point. Equilibrium and kinetic properties in this regime are very favorable for solvent applications, and generally allow major reductions in the energy requirements for separating and purifying chemical component of a mixture.

  10. Determination of Parameters for the Supercritical Extraction of Antioxidant Compounds from Green Propolis Using Carbon Dioxide and Ethanol as Co-Solvent

    PubMed Central

    Barreto, Gabriele de Abreu; Costa, Samantha Serra; Silva, Rejane Pina Dantas; da Silva, Danielle Figuerêdo; Brandão, Hugo Neves; da Rocha, José Luiz Carneiro; Nunes, Silmar Baptista; Umsza-Guez, Marcelo Andres

    2015-01-01

    The aim of this study was to determine the best processing conditions to extract Brazilian green propolis using a supercritical extraction technology. For this purpose, the influence of different parameters was evaluated such as S/F (solvent mass in relation to solute mass), percentage of co-solvent (1 and 2% ethanol), temperature (40 and 50°C) and pressure (250, 350 and 400 bar) using supercritical carbon dioxide. The Global Yield Isotherms (GYIs) were obtained through the evaluation of the yield, and the chemical composition of the extracts was also obtained in relation to the total phenolic compounds, flavonoids, antioxidant activity and 3,5-diprenyl-4-hydroxicinnamic acid (Artepillin C) and acid 4-hydroxycinnamic (p-coumaric acid). The best results were identified at 50°C, 350 bar, 1% ethanol (co-solvent) and S/F of 110. These conditions, a content of 8.93±0.01 and 0.40±0.05 g/100 g of Artepillin C and p-coumaric acid, respectively, were identified indicating the efficiency of the extraction process. Despite of low yield of the process, the extracts obtained had high contents of relevant compounds, proving the viability of the process to obtain green propolis extracts with important biological applications due to the extracts composition. PMID:26252491

  11. Determination of phthalate esters in soil using a quick, easy, cheap, effective, rugged, and safe method followed by GC-MS.

    PubMed

    Liu, Qianjun; Chen, Di; Wu, Jiyuan; Yin, Guangcai; Lin, Qintie; Zhang, Min; Hu, Huawen

    2018-04-01

    A quick, easy, cheap, effective, rugged, and safe procedure was designed to extract pesticide residues from fruits and vegetables with a high percentage of water. It has not been used extensively for the extraction of phthalate esters from sediments, soils, and sludges. In this work, this procedure was combined with gas chromatography with mass spectrometry to determine 16 selected phthalate esters in soil. The extraction efficiency of the samples was improved by ultrasonic extraction and dissolution of the soil samples in ultra-pure water, which promoted the dispersion of the samples. Furthermore, we have simplified the extraction step and reduced the risk of organic solvent contamination by minimizing the use of organic solvents. Different extraction solvents and clean-up adsorbents were compared to optimize the procedure. Dichloromethane/n-hexane (1:1, v/v) and n-hexane/acetone (1:1, v/v) were selected as the extractants from the six extraction solvents tested. C18/primary secondary amine (1:1, m/m) was selected as the sorbent from the five clean-up adsorbents tested. The recoveries from the spiked soils ranged from 70.00 to 117.90% with relative standard deviation values of 0.67-4.62%. The proposed approach was satisfactorily applied for the determination of phthalate esters in 12 contaminated soil samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. The Chemistry of Separations Ligand Degradation by Organic Radical Cations

    DOE PAGES

    Mezyk, Stephen P.; Horne, Gregory P.; Mincher, Bruce J.; ...

    2016-12-01

    Solvent based extractions of used nuclear fuel use designer ligands in an organic phase extracting ligand complexed metal ions from an acidic aqueous phase. These extractions will be performed in highly radioactive environments, and the radiation chemistry of all these complexants and their diluents will play a major role in determining extraction efficiency, separation factors, and solvent-recycle longevity. Although there has been considerable effort in investigating ligand damage occurring in acidic water radiolysis conditions, only minimal fundamental kinetic and mechanistic data has been reported for the degradation of extraction ligands in the organic phase. Extraction solvent phases typically use normalmore » alkanes such as dodecane, TPH, and kerosene as diluents. The radiolysis of such diluents produce a mixture of radical cations (R •+), carbon-centered radicals (R •), solvated electrons, and molecular products such as hydrogen. Typically, the radical species will preferentially react with the dissolved oxygen present to produce relatively inert peroxyl radicals. This isolates the alkane radical cation species, R •+ as the major radiolytically-induced organic species that can react with, and degrade, extraction agents in this phase. Here we report on our recent studies of organic radical cation reactions with various ligands. Elucidating these parameters, and combining them with the known acidic aqueous phase chemistry, will allow a full, fundamental, understanding of the impact of radiation on solvent extraction based separation processes to be achieved.« less

  13. The Chemistry of Separations Ligand Degradation by Organic Radical Cations

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Mezyk, Stephen P.; Horne, Gregory P.; Mincher, Bruce J.

    Solvent based extractions of used nuclear fuel use designer ligands in an organic phase extracting ligand complexed metal ions from an acidic aqueous phase. These extractions will be performed in highly radioactive environments, and the radiation chemistry of all these complexants and their diluents will play a major role in determining extraction efficiency, separation factors, and solvent-recycle longevity. Although there has been considerable effort in investigating ligand damage occurring in acidic water radiolysis conditions, only minimal fundamental kinetic and mechanistic data has been reported for the degradation of extraction ligands in the organic phase. Extraction solvent phases typically use normalmore » alkanes such as dodecane, TPH, and kerosene as diluents. The radiolysis of such diluents produce a mixture of radical cations (R •+), carbon-centered radicals (R •), solvated electrons, and molecular products such as hydrogen. Typically, the radical species will preferentially react with the dissolved oxygen present to produce relatively inert peroxyl radicals. This isolates the alkane radical cation species, R •+ as the major radiolytically-induced organic species that can react with, and degrade, extraction agents in this phase. Here we report on our recent studies of organic radical cation reactions with various ligands. Elucidating these parameters, and combining them with the known acidic aqueous phase chemistry, will allow a full, fundamental, understanding of the impact of radiation on solvent extraction based separation processes to be achieved.« less

  14. Simultaneous cell disruption and lipid extraction of wet aurantiochytrium sp. KRS101 using a high shear mixer.

    PubMed

    Kwak, Minsoo; Kang, Seul Gi; Hong, Won-Kyung; Han, Jong-In; Chang, Yong Keun

    2018-05-01

    Microalgae are regarded as a promising source of biofuels, and the concept of a microalgae-based biorefinery has attracted increasing attention in recent years. From an economic perspective, however, the process remains far from competitive with fossil fuels. This is particularly true of lipid extraction, due in part to the energy-intensive drying step. As a result, wet extraction methods have been studied as an economic alternative. In the present study, a novel extraction approach which utilizes high shear stress mixing was adopted and demonstrated for simultaneous lipid extraction and cell disruption to enable the retrieval of lipids directly from concentrated wet biomass. When a high shear mixer (HSM) was used to extract lipid from a dense biomass (> 350 g/L) of the oleaginous algae Aurantiochytrium sp., it exhibited a yield of esterifiable lipids which exceeded 80% in 10 min at 15,000 rpm with various solvent types. The HSM was found to improve the lipid yields substantially with solvents less miscible with either lipids or water, such that the range of Hansen solubility parameters for the usable solvents became 3.3 times wider (14.9-26.5 MPa 1/2 ). The HSM, which appeared effectively to loosen the water barrier that prevents solvent molecules from penetrating through the cell envelope, was found to be more efficient with hexane, hexane/isopropanol, and ethanol, all of which showed nearly identical lipid yields compared to the dry extraction process. The HSM can, indeed, offer a powerful mechanical means of lipid extraction with non-polar and less toxic solvents from wet biomass.

  15. SITE TECHNOLOGY CAPSULE: TERRA-KLEEN SOLVENT EXTRACTION TECHNOLOGY

    EPA Science Inventory

    Remediation of PCBs in soils has been difficult to implement on a full-scale, cost-effective basis. The Terra-Kleen solvent extraction system has overcome many of the soil handling, contaminant removal, and regulatory restrictions that have made it difficult to implement a cost-e...

  16. TERRA-KLEEN RESPONSE GROUP, INC. SOLVENT EXTRACTION TECHNOLOGY: INNOVATIVE TECHNOLOGY EVALUATION REPORT

    EPA Science Inventory

    This report summarizes the results of a field demonstration conducted under the SITE program. The technology which was demonstrated was a solvent extraction technology developed by Terra-Kleen Response Group. Inc. to remove organic contaminants from soil. The technology employs...

  17. Synergism and antagonism in extracting local anesthetics from aqueous media with mixtures of solvents

    NASA Astrophysics Data System (ADS)

    Sukhanov, P. T.; Chibisova, T. V.; Korenman, Ya. I.

    2014-12-01

    The extraction of local anesthetics from aqueous media with mixtures of solvent is examined and its synergistic and antagonistic effects are determined. Synergism parameters, separation factors, constants for the formation of anesthetic complexes, and solvate numbers are calculated.

  18. Extraction-Scrub-Strip test results from the interim Salt Disposition Program Macrobatch 9 Tank 21H qualification samples

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Peters, T.

    2016-02-23

    Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 9 for the Interim Salt Disposition Program (ISDP). The Salt Batch 9 characterization results were previously reported. An Extraction-Scrub-Strip (ESS) test was performed to determine cesium distribution ratios (D (Cs)) and cesium concentration in the strip effluent and decontaminated salt solution (DSS) streams; this data will be used by Tank Farm Engineering to project a cesium decontamination factor (DF). This test used actual Tank 21H material, and a blend solvent prepared by SRNL that mimics the solvent composition currently being used atmore » the Modular Caustic-Side Solvent Extraction Unit (MCU). The ESS test showed acceptable performance with an extraction D (Cs) value of 52.4. This value is consistent with results from previous salt batch ESS tests using similar solvent formulations. This compares well against the predicted value of 56.5 from a recently created D (Cs) model« less

  19. Field-portable supercritical CO{sub 2} extractor

    DOEpatents

    Wright, B.W.; Zemanian, T.S.; Robins, W.H.; Woodcock, L.J.

    1997-06-10

    The present invention is an apparatus for extracting organic compounds from solid materials. A generator vessel has a removable closure for receiving a solid or liquid solvent which is heated with a resistive heating element to a gaseous or supercritical phase. The removable closure is unencumbered because the side wall is penetrated with an outlet for the gaseous or supercritical solvent. The generator vessel further has a pressure transducer that provides an electronic signal related to pressure of the gaseous or supercritical solvent. The apparatus of the present invention further includes at least one extraction cell having a top and a bottom and a wall extending there between, wherein the bottom is sealably penetrated by an inlet for gaseous or supercritical solvent received through a manifold connected to the outlet, the top having an easy-open removable closure cap, and the wall having an outlet port. Finally, a permeable sample cartridge is included for holding the solid materials and to provide radial-flow of the extraction fluid, which is placed within the extraction cell. 10 figs.

  20. Field-portable supercritical CO.sub.2 extractor

    DOEpatents

    Wright, Bob W.; Zemanian, Thomas S.; Robins, William H.; Woodcock, Leslie J.

    1997-01-01

    The present invention is an apparatus for extracting organic compounds from solid materials. A generator vessel has a removable closure for receiving a solid or liquid solvent which is heated with a resistive heating element to a gaseous or supercritical phase. The removable closure is unencumbered because the side wall is penetrated with an outlet for the gaseous or supercritical solvent. The generator vessel further has a pressure transducer that provides an electronic signal related to pressure of the gaseous or supercritical solvent. The apparatus of the present invention further includes at least one extraction cell having a top and a bottom and a wall extending therebetween, wherein the bottom is sealably penetrated by an inlet for gaseous or supercritical solvent received through a manifold connected to the outlet, the top having an easy-open removable closure cap, and the wall having an outlet port. Finally, a permeable sample cartridge is included for holding the solid materials and to provide radial-flow of the extraction fluid, which is placed within the extraction cell.

  1. Predictive model for ionic liquid extraction solvents for rare earth elements

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Grabda, Mariusz; Oleszek, Sylwia; Institute of Environmental Engineering of the Polish Academy of Sciences, ul. M. Sklodowskiej-Curie 34, 41-819, Zabrze

    2015-12-31

    The purpose of our study was to select the most effective ionic liquid extraction solvents for dysprosium (III) fluoride using a theoretical approach. Conductor-like Screening Model for Real Solvents (COSMO-RS), based on quantum chemistry and the statistical thermodynamics of predefined DyF{sub 3}-ionic liquid systems, was applied to reach the target. Chemical potentials of the salt were predicted in 4,400 different ionic liquids. On the base of these predictions set of ionic liquids’ ions, manifesting significant decrease of the chemical potentials, were selected. Considering the calculated physicochemical properties (hydrophobicity, viscosity) of the ionic liquids containing these specific ions, the most effectivemore » extraction solvents for liquid-liquid extraction of DyF{sub 3} were proposed. The obtained results indicate that the COSMO-RS approach can be applied to quickly screen the affinity of any rare earth element for a large number of ionic liquid systems, before extensive experimental tests.« less

  2. Microencapsulation by solvent extraction/evaporation: reviewing the state of the art of microsphere preparation process technology.

    PubMed

    Freitas, Sergio; Merkle, Hans P; Gander, Bruno

    2005-02-02

    The therapeutic benefit of microencapsulated drugs and vaccines brought forth the need to prepare such particles in larger quantities and in sufficient quality suitable for clinical trials and commercialisation. Very commonly, microencapsulation processes are based on the principle of so-called "solvent extraction/evaporation". While initial lab-scale experiments are frequently performed in simple beaker/stirrer setups, clinical trials and market introduction require more sophisticated technologies, allowing for economic, robust, well-controllable and aseptic production of microspheres. To this aim, various technologies have been examined for microsphere preparation, among them are static mixing, extrusion through needles, membranes and microfabricated microchannel devices, dripping using electrostatic forces and ultrasonic jet excitation. This article reviews the current state of the art in solvent extraction/evaporation-based microencapsulation technologies. Its focus is on process-related aspects, as described in the scientific and patent literature. Our findings will be outlined according to the four major substeps of microsphere preparation by solvent extraction/evaporation, namely, (i) incorporation of the bioactive compound, (ii) formation of the microdroplets, (iii) solvent removal and (iv) harvesting and drying the particles. Both, well-established and more advanced technologies will be reviewed.

  3. Tetrahydrofuran-water extraction, in-line clean-up and selective liquid chromatography/tandem mass spectrometry for the quantitation of perfluorinated compounds in food at the low picogram per gram level.

    PubMed

    Ballesteros-Gómez, Ana; Rubio, Soledad; van Leeuwen, Stefan

    2010-09-17

    A new solvent extraction system was developed for extraction of PFCs from food. The extraction is carried out with 75:25 (v/v) tetrahydrofuran:water, a solvent mixture that provides an appropriate balance of hydrogen bonding, dispersion and dipole-dipole interactions to efficiently extract PFCs with chains containing 4-14 carbon atoms from foods. This mixture provided recoveries above 85% from foods including vegetables, fruits, fish, meat and bread; and above 75% from cheese. Clean-up with a weak anion exchange resin and Envi-carb SPE, which were coupled in line for simplicity, was found to minimize matrix effects (viz. enhancement or suppression of electrospray ionization). The target analytes (PFCs) were resolved on a perfluorooctyl phase column that proved effective in separating mass interferences for perfluorooctane sulfonate (PFOS) in fish and meat samples. The mass spectrometer was operated in the negative electrospray ionization mode and used to record two transitions per analyte and one per mass-labeled method internal standard. The target PFCs were quantified from solvent based calibration curves. The limits of detection (LODs) were as low as 1-5 pg analyte g(-1) food; by exception, those for C(4) and C(5) PFCs were somewhat higher (25-30 pg g(-1)) owing to their less favourable mass response. To the best of our knowledge these are among the best LODs for PFCs in foods reported to date. The analysis of a variety of foods revealed contamination with PFCs at levels from 4.5 to 75 pg g(-1) in 25% of samples (fish and packaged spinach). C(10)-C(14) PFCs were found in fish, which testifies to the need to control long-chain PFCs in this type of food. The proposed method is a useful tool for the development of a large-scale database for the presence of PFCs in foods. 2010 Elsevier B.V. All rights reserved.

  4. Separation of thorium from lanthanides by solvent extraction with ionizable crown ethers.

    PubMed

    Du, H S; Wood, D J; Elshani, S; Wai, C M

    1993-02-01

    Thorium and the lanthanides are extracted by alpha-(sym-dibenzo-16-crown-5-oxy)acetic acid and its analogues in different pH ranges. At pH 4.5, Th is quantitatively extracted by the crown ether carboxylic acids into chloroform whereas the extraction of the lanthanides is negligible. Separation of Th from the lanthanides can be achieved by solvent extraction under this condition. The extraction does not require specific counteranions and is reversible with respect to pH. Trace amounts of Th in water can be quantitatively recovered using this extraction system for neutron activation analysis. The nature of the extracted Th complex and the mechanism of extraction are discussed.

  5. Comparison of solvent/derivatization agent systems for determination of extractable toluene diisocyanate from flexible polyurethane foam.

    PubMed

    Vangronsveld, Erik; Berckmans, Steven; Spence, Mark

    2013-06-01

    Flexible polyurethane foam (FPF) is produced from the reaction of toluene diisocyanate (TDI) and polyols. Limited and conflicting results exist in the literature concerning the presence of unreacted TDI remaining in FPF as determined by various solvent extraction and analysis techniques. This study reports investigations into the effect of several solvent/derivatization agent combinations on extractable TDI results and suggests a preferred method. The suggested preferred method employs a syringe-based multiple extraction of foam samples with a toluene solution of 1-(2-methoxyphenyl)-piperazine. Extracts are analyzed by liquid chromatography using an ion trap mass spectrometry detection technique. Detection limits of the method are ~10ng TDI g(-1) foam (10 ppb, w/w) for each TDI isomer (i.e. 2,4-TDI and 2,6-TDI). The method was evaluated by a three-laboratory interlaboratory comparison using two representative foam samples. The total extractable TDI results found by the three labs for the two foams were in good agreement (relative standard deviation of the mean of 30-40%). The method has utility as a basis for comparing FPFs, but the interpretation of extractable TDI results using any solvent as the true value for 'free' or 'unreacted' TDI in the foam is problematic, as demonstrated by the difference in the extracted TDI results from the different extraction systems studied. Further, a consideration of polyurethane foam chemistry raises the possibility that extractable TDI may result from decomposition of parts of the foam structure (e.g. dimers, biurets, and allophanates) by the extraction system.

  6. SOLVENT EXTRACTION PROCESS FOR SEPARATING URANIUM AND PLUTONIUM FROM AQUEOUS ACIDIC SOLUTIONS OF NEUTRON IRRADIATED URANIUM

    DOEpatents

    Bruce, F.R.

    1962-07-24

    A solvent extraction process was developed for separating actinide elements including plutonium and uranium from fission products. By this method the ion content of the acidic aqueous solution is adjusted so that it contains more equivalents of total metal ions than equivalents of nitrate ions. Under these conditions the extractability of fission products is greatly decreased. (AEC)

  7. Chemical model for the solvent extraction of GdCl3 from a chloride solution with saponified PC88A

    NASA Astrophysics Data System (ADS)

    Lee, Man-Seung; Lee, Jin-Young; Kim, Joon-Soo

    2005-12-01

    Solvent extraction experiments of Gd with 40% saponified PC88A have been conducted from a chloride solution under different extraction conditions. The effect of saponification of an acidic extractant on the extraction of Gd was investigated. To analyze the ionic equilibria of a GdCl3 solution, we estimated the necessary thermodynamic properties from reported values. Moreover, when applying the chemical model developed in this study, we used experimental data to estimate the equilibrium constant for the extraction of Gd with partially saponified PC88A.

  8. Micro-solid phase extraction of benzene, toluene, ethylbenzene and xylenes from aqueous solutions using water-insoluble β-cyclodextrin polymer as sorbent.

    PubMed

    Nojavan, Saeed; Yazdanpanah, Mina

    2017-11-24

    Water-insoluble β-cyclodextrin polymer was synthesized by chemical cross-linking using epichlorohydrin (EPI) as a cross-linker agent. The produced water-insoluble polymer was used as a sorbent for the micro-solid phase extraction (μ-SPE) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water samples. The μ-SPE device consisted of a sealed tea bag envelope containing 15mg of sorbent. For the evaluation of the extraction efficiency, parameters such as extraction and desorption time, desorption solvent and salt concentration were investigated. At an extraction time of 30min in the course of the extraction process, analytes were extracted from a 10mL aqueous sample solution. The analytes were desorbed by ultrasonication in 200μL of acetonitrile for 20min. Analysis of the analytes was done by a gas chromatography-flame ionization detector (GC-FID) system. The enrichment factor (EF) was found to be in the range 23.0-45.4 (EF max =50.0). The method provided linearity ranges of between 0.5 and 500.0ng/mL (depending on the analytes), with good coefficients of determination (r 2 ) ranging between 0.997 and 0.999 under optimized conditions. Detection limits for BTEX were in the range of between 0.15 and 0.60ng/mL, while corresponding recoveries were in the range of 46.0-90.0%. The relative standard deviation of the method for the analytes at 100.0ng/mL concentration level ranged from 5.5 to 11.2% (n=5). The proposed method was concluded to be a cost effective and environmentally-friendly extraction technique with ease of operation and minimal usage of organic solvent. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Accelerated solvent extraction combined with solid phase extraction for the determination of organophosphate esters from sewage sludge compost by UHPLC-MS/MS.

    PubMed

    Pang, Long; Yang, Peijie; Ge, Liming; Du, Jingjing; Zhang, Hongzhong

    2017-02-01

    Organophosphate esters (OPEs), widely used as flame retardants and plasticizers, are regarded as emerging pollutants. OPEs are prone to concentrate into residual activated sludge, which might cause secondary pollution if not suitably treated. Composting is an economical and effective approach to make sewage sludge stable and harmless. Therefore, it is essential to develop a novel method for analyzing OPEs in sewage sludge compost samples. However, in the composting process, large amounts of amendments are doped into the sludge to adjust the carbon-nitrogen ratio. Amendment has a strong capacity for adsorption and thus induces a decrease of extraction efficiency. This study developed a novel procedure for determining OPEs in compost samples. Accelerated solvent extraction (ASE) and solid phase extraction (SPE) were used for extracting and concentrating the OPEs from sewage sludge compost samples, and then analyzed by UHPLC-MS/MS. Some parameters were optimized in this study, mainly including the extraction solvent type, extraction temperature, static extraction time, extraction cycles, and flush volume. Under the optimal conditions, the proposed method showed good linearity between 0.50 and 100 μg kg -1 with regression coefficients in the range of 0.9984-0.9998. Detection limits were in the range of 0.02-3 μg kg -1 with standard deviations ranging from 2 to 6%. Acceptable recoveries between 56 and 119% for samples spiked at different concentration levels were achieved. In contrast, the recoveries merely ranged from 24 to 58% by using ultrasonic-assisted extraction. Graphical abstract A comparison of recoveries between ultrasonic-assisted extraction (UAS) and accelerated solvent extraction (ASE) for organophosphate esters from sewage sludge compost samples.

  10. Extraction of organic compounds from representative shales and the effect on porosity

    DOE PAGES

    DiStefano, Victoria H.; McFarlane, Joanna; Anovitz, Lawrence M.; ...

    2016-09-01

    This study is an attempt to understand how native organics are distributed with respect to pore size to determine the relationship between hydrocarbon chemistry and pore structure in shales, as the location and accessibility of hydrocarbons is key to understanding and improving the extractability of hydrocarbons in hydraulic fracturing. Selected shale cores from the Eagle Ford and Marcellus formations were subjected to pyrolysis gas chromatography (GC), thermogravimetric analysis, and organic solvent extraction with the resulting effluent analyzed by GC-mass spectrometry (MS). Organics representing the oil and gas fraction (0.1 to 1 wt. %) were observed by GC-MS. For most ofmore » the samples, the amount of native organic extracted directly related to the percentage of clay in the shale. The porosity and pore size distribution (0.95 nm to 1.35 m) in the Eagle Ford and Marcellus shales was measured before and after solvent extraction using small angle neutron scattering (SANS). An unconventional method was used to quantify the background from incoherent scattering as the Porod transformation obscures the Bragg peak from the clay minerals. Furthermore, the change in porosity from SANS is indicative of the extraction or breakdown of higher molecular weight bitumen with high C/H ratios (asphaltenes and resins). This is mostly likely attributed to complete dissolution or migration of asphaltenes and resins. These longer carbon chain lengths, C30-C40, were observed by pyrolysis GC, but either were too heavy to be analyzed in the extracts by GC-MS or were not effectively leached into the organic solvents. Thus, experimental limitations meant that the amount of extractable material could not be directly correlated to the changes in porosity measured by SANS. But, the observable porosity generally increased with solvent extraction. A decrease in porosity after extraction as observed in a shale with high clay content and low maturity was attributed to swelling of pores with solvent uptake or migration of resins and asphaltenes.« less

  11. Effect of extraction solvents on the biomolecules and antioxidant properties of Scorzonera undulata (Asteraceae): Application of factorial design optimization phenolic extraction.

    PubMed

    Athmouni, Khaled; Belghith, Taheni; Bellassouad, Khaled; Feki, Abdelfattah El; Ayadi, Habib

    2015-01-01

    Phenolic compounds were extracted and isolated from S. undulata roots. Sample of roots from E. hirta was tested for phenolic compounds, and in vitro antioxidant activity by diphenyl-1-picrylhydrazyl (DPPH) assay, ABTS, FRAP and reducing power was measured using cyano- ferrate method. The methanolic fraction exhibited the highest total phenol content (6.12 ±0.11 mg AGE/g DW). On the other hand, the highest flavonoids concentration was observed in ethyl acetate fraction (2.90 ±0.05 mg CE/g DW) in addition to anthocyanins (28.56 ±3.96 mg/l). Besides, the highest level of tannins content was measured in the polar aprotic solvent ethyl acetate extract (3.25 ±0.06 mg CE/g DW). The different extracts of S. undulata were evaluated for their radical scavenging activities by means of the DPPH assay. The strongest scavenging activity was observed in methanolic fraction scavenged radicals effectively with IC   values of 0.14 ±0.02 mg/ml. Similarly, the potassium ferricyanide reduction (FRAP) and ABTS•+ of methanol extract. On the other hand, the total reducing power of ethyl acetate extract was found higher than of other extracts. This paper presents the application of the design-of experiment method for optimizing the extraction of phenolic content using methanol solvent. The resulting regression model has shown that the effect of temperature is not statistically significant (with >95% certainty), while that of agitation speed is. The two main effects are contributed by the solvent concentration and the maceration period. Our results clearly showed that the extraction of phenolic compounds and their antioxidant capacity is significantly affected by solvent combinations. S. undulata presented the highest total phenolic content, total flavonoids content and antioxidant capacity values. The resulting regression model has shown that the effect of temperature is not statistically significant (with >95% certainty), while that of agitation speed is.

  12. Characterization of Chemical Compounds with Antioxidant and Cytotoxic Activities in Bougainvillea x buttiana Holttum and Standl, (var. Rose) Extracts

    PubMed Central

    Abarca-Vargas, Rodolfo; Peña Malacara, Carlos F.; Petricevich, Vera L.

    2016-01-01

    Bougainvillea is widely used in traditional Mexican medicine to treat several diseases. This study was designed to characterize the chemical constituents of B. x buttiana extracts with antioxidant and cytotoxic activities using different solvents. The extraction solvents used were as follows: distilled water (dH2O), methanol (MeOH), acetone (DMK), ethanol (EtOH), ethyl acetate (EtOAc), dichloromethane (DCM), and hexane (Hex) (100%) at an extraction temperature of 26 °C. Analysis of bioactive compounds present in the B. x buttiana extracts included the application of common phytochemical screening assays, GC-MS analysis, and cytotoxicity and antioxidant assays. The results show that the highest extraction yield was observed with water and methanol. The maximum total phenolic content amount and highest antioxidant potential were obtained when extraction with methanol was used. With the exceptions of water and ethanol extractions, all other extracts showed cytotoxicity ranging between 31% and 50%. The prevailing compounds in water, methanol, ethanol, and acetone solvents were as follows: 4H-pyran-4-one, 2,3-dihydro-3, 5-dihydroxy-6-methyl (2), 2-propenoic acid, 3-(2-hydrophenyl)-(E)- (3), and 3-O-methyl-d-glucose (6). By contrast, the major components in the experiments using solvents such as EtOH, DMK, EtOAc, DCM, and Hex were n-hexadecanoic acid (8), 9,12-octadecadienoic acid (Z,Z) (12); 9-octadecenoic acid (E)- (13), and stigmasta-5,22-dien-3-ol (28). PMID:27918436

  13. Extraction and preconcentration of residual solvents in pharmaceuticals using dynamic headspace-liquid phase microextraction and their determination by gas chromatography-flame ionization detection.

    PubMed

    Farajzadeh, Mir Ali; Dehghani, Hamideh; Yadeghari, Adeleh; Khoshmaram, Leila

    2017-02-01

    The present study describes a microextraction and determination method for analyzing residual solvents in pharmaceutical products using dynamic headspace-liquid phase microextraction technique followed by gas chromatography-flame ionization detection. In this method dimethyl sulfoxide (μL level) placed into a GC liner-shaped extraction vessel is used as a collection/extraction solvent. Then the liner is exposed to the headspace of a vial containing the sample solution. The effect of different parameters influencing the microextraction procedure including collection/extraction solvent type and its volume, ionic strength, extraction time, extraction temperature and concentration of NaOH solution used in dissolving the studied pharmaceuticals are investigated and optimized. Under the optimum extraction conditions, the method showed wide linear ranges between 0.5 and 5000 mg L -1 . The other analytical parameters were obtained in the following ranges: enrichment factors 240-327, extraction recoveries 72-98% and limits of detection 0.1-0.8 mg L -1 in solution and 0.6-3.2 μg g -1 in solid. Relative standard deviations for the extraction of 100 mg L -1 of each analyte were obtained in the ranges of 4-7 and 5-8% for intra-day (n = 6) and inter-day (n = 4) respectively. Finally the target analytes were determined in different samples such as erythromycin, azithromycin, cefalexin, amoxicillin and co-amoxiclav by the proposed method. Copyright © 2016 John Wiley & Sons, Ltd.

  14. Supercritical fluid extraction

    DOEpatents

    Wai, Chien M.; Laintz, Kenneth

    1994-01-01

    A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated or lipophilic crown ether or fluorinated dithiocarbamate. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

  15. Solvent Hold Tank Sample Results for MCU-15-661-662-663: April 2015 Monthly Sample

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F.; Taylor-Pashow, K.

    2015-07-08

    The Savannah River National Lab (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-661, MCU-15-662, and MCU-15-663 pulled on April 2, 2015) for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-661-662-663 indicated a low concentration (~ 63% of nominal) of the suppressor (TiDG) and a slightly below the nominal concentration (~ 10% below nominal) of the extractant (MaxCalix). The modifier (CS-7SB) level was also 10% below its nominal value while the Isopar™ L level was slightly above its nominal value. This analysis confirms the addition of Isopar™L to the solvent onmore » March 6, 2015. Despite that the values are below target component levels, the current levels of TiDG, CS-7SB and MaxCalix are sufficient for continuing operation without adding a trim at this time until the next monthly sample. No impurities above the 1000 ppm level were found in this solvent. However, the sample was found to contain approximately 18.4 ug/g solvent mercury. The gamma level increased to 8 E5 dpm/mL solvent and it represents an order of magnitude increase relative to previous solvent samples. The increase means less cesium is being stripped from the solvent. Further analysis is needed to determine if the recent spike in the gamma measurement is due to external factors such as algae or other material that may impede stripping. The laboratory will continue to monitor the quality of the solvent in particular for any new impurity or degradation of the solvent components.« less

  16. Ultrasound assisted extraction of food and natural products. Mechanisms, techniques, combinations, protocols and applications. A review.

    PubMed

    Chemat, Farid; Rombaut, Natacha; Sicaire, Anne-Gaëlle; Meullemiestre, Alice; Fabiano-Tixier, Anne-Sylvie; Abert-Vian, Maryline

    2017-01-01

    This review presents a complete picture of current knowledge on ultrasound-assisted extraction (UAE) in food ingredients and products, nutraceutics, cosmetic, pharmaceutical and bioenergy applications. It provides the necessary theoretical background and some details about extraction by ultrasound, the techniques and their combinations, the mechanisms (fragmentation, erosion, capillarity, detexturation, and sonoporation), applications from laboratory to industry, security, and environmental impacts. In addition, the ultrasound extraction procedures and the important parameters influencing its performance are also included, together with the advantages and the drawbacks of each UAE techniques. Ultrasound-assisted extraction is a research topic, which affects several fields of modern plant-based chemistry. All the reported applications have shown that ultrasound-assisted extraction is a green and economically viable alternative to conventional techniques for food and natural products. The main benefits are decrease of extraction and processing time, the amount of energy and solvents used, unit operations, and CO 2 emissions. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Development of continuous dispersive liquid-liquid microextraction performed in home-made device for extraction and preconcentration of aryloxyphenoxy-propionate herbicides from aqueous samples followed by gas chromatography-flame ionization detection.

    PubMed

    Farajzadeh, Mir Ali; Mohebbi, Ali; Feriduni, Behruz

    2016-05-12

    In this study, a rapid, simple, and efficient sample preparation method based on continuous dispersive liquid-liquid microextraction has been developed for the extraction and preconcentration of aryloxyphenoxy-propionate herbicides from aqueous samples prior to their analysis by gas chromatography-flame ionization detection. In this method, two parallel glass tubes with different diameters are connected with a teflon stopcock and used as an extraction device. A mixture of disperser and extraction solvents is transferred into one side (narrow tube) of the extraction device and an aqueous phase containing the analytes is filled into the other side (wide tube). Then the stopcock is opened and the mixture of disperser and extraction solvents mixes with the aqueous phase. By this action, the extraction solvent is dispersed continuously as fine droplets into the aqueous sample and the target analytes are extracted into the fine droplets of the extraction solvent. The fine droplets move up through the aqueous phase due to its low density compared to aqueous phase and collect on the surface of the aqueous phase as an organic layer. Finally an aliquot of the organic phase is removed and injected into the separation system for analysis. Several parameters that can affect extraction efficiency including type and volume of extraction and disperser solvents, sample pH, and ionic strength were investigated and optimized. Under the optimum extraction conditions, the extraction recoveries and enrichment factors ranged from 49 to 74% and 1633 to 2466, respectively. Relative standard deviations were in the ranges of 3-6% (n = 6, C = 30 μg L(-1)) for intra-day and 4-7% (n = 4, C = 30 μg L(-1)) for inter-day precisions. The limits of detection were in the range of 0.20-0.86 μg L(-1). Finally the proposed method was successfully applied to determine the target herbicides in fruit juice and vegetable samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Solvent hold tank sample results for MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017): Quarterly Report

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Fondeur, F. F.; Jones, D. H.

    A trend summary of three Solvent Hold Tank (SHT) monthly samples; MCU-16-1488-1493 (December 2016), MCU-17-86-88 (January 2017), and MCU-17-119-121 (February 2017) are reported. Analyses indicate that the modifier (CS-7SB) and the extractant (MaxCalix) concentrations are at their nominal recommended levels (169,000 mg/L and 46,300 mg/L respectively). The suppressor (TiDG) level has decreased to a steady state level of 673 mg/L well above the minimum recommended level (479 mg/L). This analysis confirms the Isopar™ addition to the solvent in January 18, 2017. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levelsmore » of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). Another impurity observed in the samples was mercury. Up to 38 ± 8 micrograms of mercury per mL of solvent was detected in these samples (the average of the CV-AA and XRF methods). The higher mercury concentration in the solvent (as determined in the last three monthly samples) is possibly due to the higher mercury concentration in Salt Batches 8 and 9 (Tank 49H) or mixing of previously undisturbed areas of high mercury concentration in Tank 49H. The gamma level (0.21E5 dpm/mL) measured in the February SHT sample was one order of magnitude lower than the gamma levels observed in the December and January SHT samples. The February gamma level is consistent with the solvent being idle (since January 10, 2017). The gamma levels observed in the December and January SHT samples were consistent with previous monthly measurements where the process operated normally. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

  19. Fourier Transform Infrared Spectroscopy and Multivariate Analysis for Online Monitoring of Dibutyl Phosphate Degradation Product in Tributyl Phosphate/n-Dodecane/Nitric Acid Solvent

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Tatiana G. Levitskaia; James M. Peterson; Emily L. Campbell

    2013-12-01

    In liquid–liquid extraction separation processes, accumulation of organic solvent degradation products is detrimental to the process robustness, and frequent solvent analysis is warranted. Our research explores the feasibility of online monitoring of the organic solvents relevant to used nuclear fuel reprocessing. This paper describes the first phase of developing a system for monitoring the tributyl phosphate (TBP)/n-dodecane solvent commonly used to separate used nuclear fuel. In this investigation, the effect of extraction of nitric acid from aqueous solutions of variable concentrations on the quantification of TBP and its major degradation product dibutylphosphoric acid (HDBP) was assessed. Fourier transform infrared (FTIR)more » spectroscopy was used to discriminate between HDBP and TBP in the nitric acid-containing TBP/n-dodecane solvent. Multivariate analysis of the spectral data facilitated the development of regression models for HDBP and TBP quantification in real time, enabling online implementation of the monitoring system. The predictive regression models were validated using TBP/n-dodecane solvent samples subjected to high-dose external ?-irradiation. The predictive models were translated to flow conditions using a hollow fiber FTIR probe installed in a centrifugal contactor extraction apparatus, demonstrating the applicability of the FTIR technique coupled with multivariate analysis for the online monitoring of the organic solvent degradation products.« less

  20. Fourier Transform Infrared Spectroscopy and Multivariate Analysis for Online Monitoring of Dibutyl Phosphate Degradation Product in Tributyl Phosphate /n-Dodecane/Nitric Acid Solvent

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Levitskaia, Tatiana G.; Peterson, James M.; Campbell, Emily L.

    2013-11-05

    In liquid-liquid extraction separation processes, accumulation of organic solvent degradation products is detrimental to the process robustness and frequent solvent analysis is warranted. Our research explores feasibility of online monitoring of the organic solvents relevant to used nuclear fuel reprocessing. This paper describes the first phase of developing a system for monitoring the tributyl phosphate (TBP)/n-dodecane solvent commonly used to separate used nuclear fuel. In this investigation, the effect of extraction of nitric acid from aqueous solutions of variable concentrations on the quantification of TBP and its major degradation product dibutyl phosphoric acid (HDBP) was assessed. Fourier Transform Infrared Spectroscopymore » (FTIR) spectroscopy was used to discriminate between HDBP and TBP in the nitric acid-containing TBP/n-dodecane solvent. Multivariate analysis of the spectral data facilitated the development of regression models for HDBP and TBP quantification in real time, enabling online implementation of the monitoring system. The predictive regression models were validated using TBP/n-dodecane solvent samples subjected to the high dose external gamma irradiation. The predictive models were translated to flow conditions using a hollow fiber FTIR probe installed in a centrifugal contactor extraction apparatus demonstrating the applicability of the FTIR technique coupled with multivariate analysis for the online monitoring of the organic solvent degradation products.« less

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