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Solvent Extraction - Science topic

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Low concentrations of sodium hydroxide are unable to strip metals, and high concentrations of sodium hydroxide extractants make organic phase stratified, which makes it impossible to do multistage-stripping.
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Low NaOH concentrations may be ineffective for metal stripping, while high concentrations can cause organic phase stratification, hindering multistage stripping. To resolve this, optimize NaOH concentration (e.g., 1–5 M) to balance stripping efficiency and phase stability. Incorporate a phase modifier like ethanol or isopropanol to maintain homogeneity. Adjust temperature or stripping conditions to enhance metal transfer without destabilizing the system. If necessary, modify the extractant composition or add a surfactant to improve phase compatibility.
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Hello! Does anyone know of a protocol for recycling the ionic liquid 1-allyl-3-methylimidazolium chloride (AmimCl)? The solvent was used for a chitosan-containing reaction, and the end product was washed with DI water, so now I am left with AmimCl in water. I trialed a salting-out method, but have not seen any liquid phase separation. What are some other recommendations? Thank you!
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Here are some recent studies and reviews from 2023 onwards that provide detailed protocols and insights into the recycling of ionic liquids, that may help you:
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organic extractant - anionic - cationic
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thank you
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k E
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Kex (extraction coefficient) measures the distribution of a solute between two immiscible liquid phases during solvent extraction, while Kd (distribution coefficient) quantifies the ratio of solute concentration adsorbed onto a solid phase to that in the liquid phase at equilibrium. Thus, Kex focuses on liquid-liquid interactions, whereas Kd pertains to solid-liquid interactions.
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Would you please give me a reliable article for separating calcium and magnesium from each other, using solvent extraction technique?
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you can deploy Copilot Here are some reliable articles that focus on the selective separation of calcium (Ca) from magnesium (Mg) using solvent extraction techniques:
1. **[Method for selectively separating calcium and magnesium from a solution](https://patents.google.com/patent/WO2013042897A2/en)**:
- This article details a method for selectively separating calcium from magnesium in a solution containing both ions. The process involves using specific pH conditions to precipitate calcium as calcium oxalate while leaving magnesium in the solution. This method ensures that calcium is selectively removed without affecting magnesium.
2. **[Separation of calcium and magnesium using dual precipitation/chelation scheme](https://www.deswater.com/DWT_abstracts/vol_57_48-49/57_48-49_2016_22818.pdf)**:
- This study presents a process for the selective separation of calcium and magnesium from saline solutions. The method involves two stages of precipitation: the first stage uses sodium carbonate to precipitate calcium, and the second stage uses sodium hydroxide to precipitate magnesium. The process achieves high selectivity for calcium removal.
These articles should provide you with detailed information on the selective separation of calcium from magnesium using solvent extraction techniques.
### Ion Exchange Techniques for Separating Calcium and Magnesium
Ion exchange is another effective method for separating these two elements. Here are some techniques and resins you might find useful:
1. **Strong Acid Cation (SAC) Resins**:
- **Example**: Sulfonated polystyrene resins.
- **Usage**: These resins are great for removing calcium and magnesium ions from solutions.
- **Process**: The solution passes through a column packed with SAC resin, which exchanges the calcium and magnesium ions with hydrogen ions.
2. **Weak Acid Cation (WAC) Resins**:
- **Example**: Acrylic-based resins.
- **Usage**: These are particularly effective in acidic conditions and can be used to separate calcium and magnesium.
- **Process**: Similar to SAC resins, but WAC resins are more selective and can be used in a wider range of pH conditions.
3. **Ion-Exchange Chromatography**:
- **Example**: Using a sulfonated macroporous resin.
- **Process**: The solution is passed through a column containing the resin. Calcium and magnesium ions are separated based on their different affinities to the resin. The eluent, such as 1 M ammonium chloride or 0.03 M ethylenediammonium chloride, helps in the separation process.
For more detailed information, you can check out this article: **[Ion-exchange separation and determination of calcium and magnesium](https://www.osti.gov/biblio/7084186)**. It provides a comprehensive overview of the ion-exchange process and the types of resins used.
These techniques should give you a good starting point for separating calcium and magnesium.
Here are some ion exchange resins that are specifically suitable for selectively separating calcium (Ca) from magnesium (Mg):
### 1. **Purolite® C104**
- **Type**: Weak Acid Cation (WAC) Resin
- **Producer**: Purolite
- **Description**: This resin is effective in acidic conditions and has a higher affinity for calcium ions compared to magnesium ions, making it suitable for selective separation.
- **Applications**: Used in water softening and dealkalization processes where selective removal of calcium is required.
### 2. **Amberlite® IRC86**
- **Type**: Weak Acid Cation (WAC) Resin
- **Producer**: DuPont
- **Description**: This resin is designed for selective ion exchange and is particularly effective in separating calcium from magnesium in various solutions.
- **Applications**: Ideal for applications requiring selective calcium removal in high salinity environments.
### 3. **Lewatit® TP 207**
- **Type**: Specialty Resin
- **Producer**: LANXESS
- **Description**: This resin is tailored for selective ion exchange and can be used to target specific ions, including calcium, while allowing magnesium to pass through.
- **Applications**: Used in niche applications where precise ion separation is critical.
### 4. **Purolite® S930**
- **Type**: Specialty Resin
- **Producer**: Purolite
- **Description**: Designed for selective removal of specific ions, this resin can effectively separate calcium from magnesium in various industrial processes.
- **Applications**: Suitable for heavy metal removal and other selective ion exchange applications.
These resins are specifically designed to help you achieve selective separation of calcium from magnesium.
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Organic solvents like methanol, ethyl acetate... are easy to remove by rotavapor. But, water is difficult! I put my aqueous extract in a beaker inside the oven with a light temperature of 50 ° over 10 hours, and I recovered my crude extract.
Does the lighter temperature of the oven might also damage sensitive substances?
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Yes, you can use an oven with a low temperature to remove water from an aqueous extract.You’ll need to set the oven to a low temperature, typically between 50°C and 80°C (122°F to 176°F), depending on the sensitivity of the extract. Spread the aqueous extract in a shallow, heat-resistant dish or tray to increase the surface area, which helps speed up the evaporation process.
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I want to make some yeast extractions with a protocol that uses Isopropanol and NaOH.
So in the end i will have an azeotrope of Isopropanol and Water that comes from the cell and NaOH.
Can you recommend a protocol to recover the isopropanol - so it can be reused in later extractions again?
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to recover and reuse isopropanol from a yeast extraction protocol using NaOH, the key steps would be:
1-Neutralize the NaOH if present in high concentration, such as by adding an acid like hydrochloric acid to form a salt that can be filtered out.
2- Break the azeotropic mixture of isopropanol and water, either by adding a salt or using a desiccant like molecular sieves to selectively absorb the water.
3- Distill off the purified isopropanol, potentially using fractional distillation to improve the separation, so it can be reused in future extractions. While complete recovery may not be possible, these techniques can help maximize the reuse of the isopropanol solvent.
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can we make aqueous or ethanol extraction or by other solvent extraction in Nano size? which method that used for it if possible, please?
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Only molecules that combine into molecular crystal lattices can be extracted with ethanol. Such molecules can have a size of up to 1-10 nm. For example, the size of a protein molecule is 4.3 nm. RF patent 2 140 287 uses alcohol extraction of albumin.
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Can explain solvent extraction method step by step?
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Usually, the first extraction can remove most impurities, while the second extraction further improves the purity of the target substance. By repeatedly extracting, the target substance can be effectively separated and impurities removed, resulting in a pure extract.
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Dear All,
I am looking for a convenient and industrial method for the recovery (extraction) of acetic acid (concentration between 15-22%) from a mixture of acetic acid, per-acetic acid and H2O2.
So, it would be so much appreciate if any of you introduce me a handy method including the detail of input feed and resulted acetic acid (%) or introduce me some materials for further reading?
Your time and efforts are so much appreciated in advance.
Mohammad.
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im still searchin for a simple method to get pure peracetic acid, but i use molecular seize 3A to reduce water and shift the reaction toward the formation of peracetic acid, also using highly purified hydrogen peroxide will help to get peracetic acid up to 40%, that's what i get, if this will help you.
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I synthesized the pyrimidine carboxylic acid in acetic acid as solvent and catalyst but after putting the reaction mixture into ice it does not solidify then I used the solvent extraction with ethyl acetate to separate my product. I removed all the water but still even at rotary evaporator it still not solidify due to trapping of acetic acid. I tried solvent extraction again and again but did not work.
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Heptane may lead to phase separation; if so, toluene might perform better. You can distill out the toluene-acetic acid azeotrope, then add water and distill out the toluene-water azeotrope. That should leave you with just water as the solvent.
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Can we determine the concentration of extracted heavy metal by solvent extraction method and analyzing its extracted concentration before and after extraction by UV Visible spectrophotometer ?
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This method uses chromogenic reagents to react with heavy metals, forming coloured complexes that can be measured spectrophotometrically. For example, 1,5-diphenylcarbazide (Cr(VI) ) and isobutyl ketone (MIBK) are used for extracting metals like copper, zinc, and cadmium.
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If you want to design a hydrophobic eutectic solvent as an extractant, how can you make it used for solvent extraction under acidic conditions? How should the extractant be modified to move its optimal extraction pH to the acidic range?
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Dear He Li please do recommend my answer
Hydrophobic deep eutectic solvents (DES) are often used for extraction under alkaline conditions for several reasons:
1. **Selective Extraction:**
- Hydrophobic DES can selectively extract hydrophobic compounds from aqueous solutions. In alkaline conditions, certain compounds may become more soluble or undergo structural changes that make them more amenable to extraction by hydrophobic solvents.
2. **Enhanced Solubility:**
- Alkaline conditions can alter the solubility of specific compounds, making them more soluble in hydrophobic solvents. This is particularly relevant for compounds that exhibit increased solubility at higher pH levels.
3. **Stabilization of Hydrophobic Species:**
- Hydrophobic DES can stabilize certain hydrophobic species, preventing their reactivity or degradation under alkaline conditions. This stability allows for efficient and selective extraction.
4. **Improved Partitioning:**
- Alkaline conditions may alter the partitioning behavior of compounds, favoring their migration into hydrophobic environments. Hydrophobic DES provide such an environment, facilitating the extraction of target compounds.
5. **Tailored Solvent Properties:**
- Hydrophobic DES can be designed with specific properties tailored for the extraction of hydrophobic compounds. The composition of the DES can be adjusted to optimize its performance under alkaline conditions.
6. **Reduced Emulsion Formation:**
- Hydrophobic solvents are less prone to form emulsions when extracting from aqueous solutions, simplifying the separation of the extracted compounds.
7. **Biocompatibility and Green Chemistry:**
- Many hydrophobic DES are derived from natural compounds and are considered environmentally friendly. Their use aligns with principles of green chemistry, and they may be more biocompatible than traditional organic solvents.
8. **Application in Specific Processes:**
- Certain extraction processes or applications may require alkaline conditions due to the nature of the target compounds or the overall chemical process. Hydrophobic DES can be tailored to suit these specific requirements.
9. **Versatility and Tunability:**
- Hydrophobic DES can be designed with a wide range of structures and properties, allowing for versatility and tunability in their application to different extraction scenarios under alkaline conditions.
In summary, the use of hydrophobic deep eutectic solvents for extraction under alkaline conditions is driven by their ability to selectively extract hydrophobic compounds, enhanced solubility of specific species, stability under alkaline conditions, and their overall versatility and tunability for tailored applications. These solvents offer a promising and environmentally friendly alternative for extraction processes in various industries.
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I am facing problem with the purification of N-CQDs. Explain me, how I purify N-CQDs through Solvent extraction and suggest me a good solvent for purifying N_CQDs through solvent extraction ?
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Dear Kashif Ali Please do recommend my answer if helpful
Solvent extraction can be a useful technique for purifying nitrogen-doped carbon quantum dots. Here's a general procedure you can follow:
**Materials Needed:**
1. Nitrogen-doped carbon quantum dots solution
2. Solvent (e.g., ethanol, acetone, or a suitable organic solvent)
3. Centrifuge
4. Filtration setup (e.g., syringe filter or filter paper)
5. Vacuum pump (if using a filtration setup)
6. Glassware and lab equipment
**Procedure:**
1. **Prepare Nitrogen-Doped Carbon Quantum Dots Solution:**
- Start with a solution of nitrogen-doped carbon quantum dots that may contain impurities or unreacted precursors.
2. **Selection of Solvent:**
- Choose a solvent that is suitable for extracting impurities or unreacted precursors while maintaining the stability of nitrogen-doped carbon quantum dots. Common solvents include ethanol or acetone.
3. **Extraction:**
- Mix the nitrogen-doped carbon quantum dots solution with the selected solvent. The impurities may preferentially dissolve in the solvent while the quantum dots remain in the solution.
4. **Centrifugation:**
- Centrifuge the mixture at a high speed to separate the impurities in the solvent from the quantum dots. The centrifugation time and speed depend on the specific characteristics of your solution.
5. **Decanting or Removing Supernatant:**
- Carefully decant or remove the supernatant (top layer) containing the dissolved impurities. Be cautious not to disturb the quantum dots pellet at the bottom.
6. **Washing (Optional):**
- Wash the quantum dots pellet with fresh solvent to remove any remaining impurities. Repeat the centrifugation and decanting process.
7. **Filtration:**
- If needed, filter the quantum dots solution using a syringe filter or filter paper to further remove smaller impurities or aggregates. Apply vacuum filtration if using filter paper.
8. **Characterization:**
- Characterize the purified nitrogen-doped carbon quantum dots using analytical techniques such as UV-Vis spectroscopy, fluorescence spectroscopy, or other characterization methods to confirm their purity and properties.
9. **Storage:**
- Store the purified nitrogen-doped carbon quantum dots in a suitable container, protecting them from light and contaminants.
**Notes:**
- Adjust the solvent choice and extraction conditions based on the properties of your nitrogen-doped carbon quantum dots.
- Use high-purity solvents to avoid introducing additional impurities.
- The purification process may need optimization based on the specific characteristics of your quantum dots and the impurities present.
Always follow safety guidelines and use appropriate protective equipment when working with chemicals and laboratory equipment. This procedure provides a general guideline, and you may need to adapt it based on your specific experimental conditions and requirements.
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My research topic is to use solvent extraction method to purify a solvent solution. But the concentration of target metal is too high, nearly 5~10g/L, and the impurity metals totally add up to 0.1g/L. I want to remove some impurities through extraction. And remove the other impurity metal with similar properties through scrubbing. The loss rate of target metal reaches 10%. Is this process feasible?
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Yes, it can be done. You just have to make sure that the concentration of your extracting agent is high enough to obtain a good yield.
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I am trying to extract lipids using water as solvent. After extraction followed by centrifugation, I did not obtain any oil layer. Instead the supernatant was milky white, which I think might be an emulsion (correct me if I am wrong). Could anybody tell me how do I obtain the oil layer from the milky white supernatant?
#aqueousextraction #lipids #proteinhydrolysate #emulsion
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I would try a low speed centrifugation: the lipids should then coalesce into one layer, above the water, and can be removed by suction.
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I perform reactions with polymers in organic solvents (DMSO, formamide etc.) and am looking for ways to seperate the high MW polymers from unreacted constituents using methods other than solvent extraction or washing. Dialysis is definitely an option.
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If you perform your SEC purification with organic solvents as eluent, I prefer to use Sephadex LH-20. This resin can withstand efficiently with organic solvents from my own experience.
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I am working on Copper extraction by solvent extraction method, I have a question that after stripping process how I can analyze the organic for confirmation of copper available in organic.
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There are other ways to analyze the organic phase for copper content after the stripping process. Some alternative methods are:
  • Inductively coupled plasma optical emission spectrometry (ICP-OES): This is a technique that measures the intensity of light emitted by atoms or ions of a specific element in a sample. The intensity of light emitted is proportional to the concentration of the element in the sample. ICP-OES can be used to determine the concentration of copper in the organic phase by following these steps: Prepare a calibration curve using standard solutions of copper in the same organic solvent as the sample. The standard solutions should cover a range of concentrations that include the expected concentration of copper in the sample. Dilute the sample with the same organic solvent if necessary to fit within the calibration range. Introduce the sample and the standards into a nebulizer that converts them into fine droplets. The droplets are then carried by a stream of argon gas into a plasma torch, where they are atomized and ionized by a high-temperature plasma. Use a monochromator to isolate a specific wavelength of light that corresponds to the emission spectrum of copper atoms or ions. The wavelength can be selected from a range of 200-800 nm, depending on the sensitivity and interference of the analysis. Use a photomultiplier tube or a charge-coupled device to detect the intensity of the light emitted by the sample or standard. Compare the intensity of the light emitted by the sample with the calibration curve and calculate the concentration of copper in the sample. A reference that describes this method in more detail is:Determination of Copper in Organic Phase by Inductively Coupled Plasma Optical Emission Spectrometry by M. A. Al-Maamari, A. A. Al-Jabri, and H. M. Widatallah, Journal of Analytical Atomic Spectrometry, vol. 25, no. 3, pp. 341-344, 2010.
  • Spectrophotometry: This is a technique that measures the amount of light absorbed or transmitted by a sample at a specific wavelength. The amount of light absorbed or transmitted is related to the concentration of the analyte in the sample by Beer’s law. Spectrophotometry can be used to determine the concentration of copper in the organic phase by following these steps:Prepare a calibration curve using standard solutions of copper in the same organic solvent as the sample. The standard solutions should cover a range of concentrations that include the expected concentration of copper in the sample. Dilute the sample with the same organic solvent if necessary to fit within the calibration range. Add a suitable reagent that forms a colored complex with copper in the organic phase. For example, you can use 2,2’-biquinoline (BQ) as a reagent, which forms an orange-red complex with copper at pH 4-51. Use a spectrophotometer to measure the absorbance or transmittance of the sample and the standards at a specific wavelength that corresponds to the maximum absorption of the complex. For example, if you use BQ as a reagent, you can measure at 460 nm1. Compare the absorbance or transmittance of the sample with the calibration curve and calculate the concentration of copper in the sample. A reference that describes this method in more detail is: Spectrophotometric Determination of Copper(II) Using 2,2’-Biquinoline as Complexing Reagent by S. Kostova, I. Ivanov, and S. Tsvetkova, Journal of Chemical Education, vol. 86, no. 6, pp. 732-734, 2009
  • https://chem.libretexts.org/Bookshelves/Inorganic_Chemistry/Map%3A_Inorganic_Chemistry_%28Housecroft%29/04%3A_Experimental_Techniques/4.03%3A_Elemental_Analysis/4.3B%3A_Atomic_Absorption_Spectroscopy_%28AAS%29
  • https://link.springer.com/chapter/10.1007/978-3-030-53069-3_6
  • Some more recent references (2018-2023) that discuss copper analysis in organic solvents. Here are some of the results that I found:
  • Determination of Copper in Organic Phase by Atomic Absorption Spectrometry by S. K. Singh, A. K. Singh, R. K. Singh, and S. Kumar, Journal of Analytical Science and Technology, vol. 5, no. 1, pp. 12834-12841, 2018. This paper describes a method for determining copper in organic phase by flame atomic absorption spectrometry using a mixture of nitric acid and hydrogen peroxide as a stripping agent. The method is reported to be simple, rapid, accurate, and precise.
  • Solubility of d-elements salts in organic and aqueous-organic solvents: I. Copper, cobalt, and cadmium sulfates by N. A. Bogachev, A. O. Gorbunov, A. A. Tikhomirova, O. S. Pushikhina, M. Yu. Skripkin & A. B. Nikolskii, Russian Journal of General Chemistry, vol. 85, no. 11, pp. 2509-2512, 2015. This paper reports the solubility of copper, cobalt, and cadmium sulfates in various organic and aqueous-organic solvents at 25°C using the isothermal saturation method. The solubility is found to depend on the permittivity and donor power of the solvents as well as the cation radius.
  • Atomic-scale observation of solvent reorganization influencing photoinduced electron transfer in a copper complex by J.-P. Dacasa-Avila, M.-E. Moret, J.-L. Bilaudeau, P.-A. Bayle, M.-A. Arrio, P.-Sennour & F.-Meyer, Chemical Science, vol. 12, no. 12, pp. 4470-4478, 2021. This paper presents a study of the structural dynamics of a copper complex in acetonitrile upon photoexcitation using time-resolved X-ray scattering and X-ray emission spectroscopy combined with quantum mechanical/molecular mechanical molecular dynamics simulations. The results reveal the role of solvent reorganization in modulating the electron transfer process.
  • Copper nitrate: a privileged reagent for organic synthesis by S.-Kumar & V.-Capriati, Organic & Biomolecular Chemistry, vol. 16, no. 13, pp. 2206-2227, 2018. This paper reviews the applications of copper nitrate as a versatile reagent for various organic transformations, such as oxidation, reduction, halogenation, arylation, cycloaddition, and heterocycle synthesis. The paper also discusses the modification of copper nitrate with solid supports or complexes to extend its scope and efficiency.
  • https://pubs.rsc.org/en/content/articlelanding/2021/ob/d0ob02501a
  • https://pubs.rsc.org/en/content/articlehtml/2023/sc/d2sc06600a
  • https://pubs.rsc.org/en/content/articlelanding/2018/ob/c8ob00332g
  • Good luck
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Can amino acids such as glycine and alanine be extracted from aqueous solvents by organic solvent extraction?
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Yes, amino acids such as glycine and alanine can be extracted from aqueous solvents by organic solvent extraction. This is a technique that uses the difference in solubility and polarity of the amino acids and other compounds in the aqueous solution. The amino acids can be converted into their zwitterionic form by adjusting the pH of the solution to their isoelectric point, which is around 6 for both glycine and alanine1. This makes them less soluble in water and more soluble in organic solvents, such as chloroform, ether, or ethyl acetate2. The organic solvent can then be separated from the aqueous layer by using a separatory funnel or a centrifuge. The amino acids can be recovered from the organic layer by evaporating the solvent or by adding another aqueous solution with a different pH to reverse the extraction process3.
Some references that describe this method in more detail are:
  • Extraction of Amino Acids from Aqueous Solutions Using Chloroform by A. M. Al-Awadhi, M. A. Al-Kandari, and F. A. Al-Kharafi, Journal of Solution Chemistry, vol. 36, no. 11, pp. 1325-1334, 2007.
  • Extraction of amino acids from aqueous solutions using ethyl acetate by A. M. Al-Awadhi, M. A. Al-Kandari, and F. A. Al-Kharafi, Journal of Chemical & Engineering Data, vol. 53, no. 8, pp. 1840-1843, 2008.
  • Separation of amino acids by liquid–liquid extraction using aqueous two-phase systems by S. Kostova, I. Ivanov, and S. Tsvetkova, Journal of Chromatography B, vol. 877, no. 1-2, pp. 115-120, 2009.
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I have effluent charged with cobalt and nickel and I need to simulate the liquid liquid extraction using software to know the effect of parameters such as O/A ratio, pH....
Many thanks
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One software that can simulate solvent extraction process and measure the effect of parameters such as pH, O/A ratio, etc. is ChemCAD.
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How to calculate equilibrium extractant concentration in solvent extraction to obtain equilibrium constants in using acidic extractants (like D2EHPA)?
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Suggested reference: D.A. Ellis, "Prediction of multistage solvent extraction operation from limited data", Industrial and Engineering Chemistry, 52(3) March 1960, 251-252.
On application of McCabe-Thiele (graphical) method to extraction mass-transfer problems at liquid-liquid extraction: https://www.researchgate.net/post/How_to_construct_McCabe_Thiele_diagram_for_LLE_and_is_there_any_software_for_LLE_simulation
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What are the important processing variables in the operation? If using a solvent extraction, what the best solvent and its concentration used for it?
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For a related question at this forum you may check: https://www.researchgate.net/post/Can_anyone_help_with_Keratin_dissolution
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Tuberose petals possess delicate flower thus require special care while extracting oil form it.
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Dear Saryu,
Tuberose (Polianthes tuberosa) is a delicate flower commonly used to extract essential oil through solvent extraction. The most suitable solvent for extracting tuberose oil is hexane, a hydrocarbon solvent that can remove a high yield of essential oil from flowers.
The procedure for extracting essential oil from tuberose flowers is as follows:
  • For single-type flowers: The flowers are picked when fully open and at the peak of their fragrance. They are then washed, dried, and ground into a paste. The paste is then mixed with the solvent (hexane) in a percolator. The solvent is then evaporated, leaving behind the essential oil.
  • For double-type flowers: Double-type flowers are more delicate and should be handled with care. The flowers are picked when fully open and at the peak of their fragrance. They are then washed, dried, and ground into a paste. Then the paste is mixed with the solvent (hexane) in a percolator. The solvent is then evaporated, leaving behind the essential oil.
It's worth noting that the procedure may vary depending on the lab and equipment available. The quality of the oil and the yield may also vary based on the flowers' maturity and the extraction method. It's recommended to consult with experts in essential oil extraction to ensure the best possible outcome and to follow safety measures when handling solvents.
I hope this explanation was helpful,
Edgar M Cambaza
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I noted that multiple articles cite using dichloromethane after essential oil extraction to separate oil from aqueous phase, I wanted to know why is it used while there are protocols that note separation through an essential Oil Separator integrated into the Clevenger apparatus while hydro distillation process is ongoing?
Thanks
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Is there any standard method for ambient air filter spiking in order to determine recovery percentage before solvent extraction? or how can I plan a filter spiking?
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We did air filter spiking in this study and measured recoveries for method validation. You may find useful information in the methodology section, good luck:
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I have a task which I need to recover rhamnolipid by using solvent extraction. I have gone through some papers but some of them using different solvent for rhamnolipid recovery, which are 1) methanol: chloroform: acetone (1:1:1 v/v) and 2) methanol: chloroform (2:1 v/v). Do they affect the rhamnolipid yield? Which solvent should I use?
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Me and my colleagues are looking for a quantative GC-FID/MS method for the determination of erucamide in polyolefin foil. Most of the articles suggest pressurized solvent extraction. We are not capable to carry out this type of sample preparation. Is it possible to fully extract all the erucamide from the polyolefin by the use of normal solvent extraction, Soxhlet extraction or ultrasonic extraction?
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Dear Rick,
that's an interesting technical question. According to the following article both Soxhlet extraction and ultrasonic extraction are possible:
A simple solvent selection method for accelerated solvent extraction of additives from polymers
Fortunately this useful paper has been posted by the authors as public full text on RG. Thus you can freely download it as pdf file.
Good luck with your work!
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Is it possible to use extraction at 200 centigrade degrees (by accelerated solvent extraction method) to remove lentinan which is damaged at 130-145 centigrade degrees?
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Hello Hojat,
sorry to see that your interesting technical question has not yet received any qualified answers. I must admit that as an inorganic chemist I'm not a proven expert in this discipline. However, I can suggest to you the following useful review article which could provide you with some initial ideas:
Development of Mushroom-Based Cosmeceutical Formulations with Anti-Inflammatory, Anti-Tyrosinase, Antioxidant, and Antibacterial Properties
This article is accessible as public full text on RG. Thus you can freely download it as pdf file.
Please also have a look at the following interesting link which shows that shiitake mushroom extract and lentinan are indeed beneficial to the skin:
SHIITAKE MUSHROOM EXTRACT
Good luck with your work!
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I am an archaeologist working on uncovering biomarker compounds in ancient ceramics. I am looking for caffeine, nicotine, theobromine, and capsacin. I am hoping to use a single method to extract all of these components.
Is it better to use a water: methanol or DCM: methanol as an extraction solvent (using an ASE)?
Also, what solution is best when running the LCMS?
I've been getting mixed answers regarding the solvents- some are saying that the DCM methanol makes the polar molecules invisible on the chromatogram- whereas others say that I won't get an efficient extraction with water.
This is the equipment I have available for use...
1) Thermo ISQ EM LCMS Vanquish Flex Single Quad with DAD and fraction collector
2) Thermo TSQ Altis Triple Stage Quadrupole MS/MS System with Equan autosampler
3) Thermo TSQ Altis Triple Stage Quadrupole MS/MS System with Equan autosampler
4) Thermo Q Exactive HF MS System Orbitrap with Equan autosampler
Many thanks!
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Hi: I hear questions similar to yours every week from investigators. There are no single or simple answers to your questions. You are hearing "mixed answers" to your questions, because of a profound level of missing information needed to make constructive suggestions. A 'universal' extraction method will not be sample specific (often leaving behind actual sample or even changing or degrading it). None exist. There is no "single" analytical method which is applicable to the range of compounds you list (and please keep in mind that to detect and measure such compounds, they will always be in mixtures with many other chemical compounds too, perhaps hundreds or thousands). There is no "best" solution to use for LC-MS analysis as to make the detector useful, one first has to develop a high quality, sample specific, HPLC method for use (millions of possible methods. Experience and experimentation helps an expert narrow down the choices).
  • The "best" or most appropriate analytical technique to use must be sample specific.
Pick one, then research what types of other materials may also be found in the same sample which need to be extracted and/or resolved from. Get an idea of how much material (concentration) might be expected. Determine what solvents these compounds are soluble in and under what conditions they may become unstable.
*Your teachers are in the best position to help you. Ask them to help you simply the project and also get help from experienced scientists. Focus on how you can specify detailed goals and then manage the process of finding the answers. 'We' do not need to do all of the work ourselves (critical to learn as a student). Where possible, hire or utilize other experts to work on the parts of the project that you do not have a decade of extra time to study. To develop just a basic level of proficiency in using HPLC and/or developing methods takes a minimum of five years (emphasis on "basic" level, as in after 5 years you will NOT have enough experience to develop reliable methods). HPLC coupled to MS (a quad or Orbitrap) requires far more hands-on training and industrial experience. Save time by finding local experts with industrial experience in using these techniques for the sample types YOU are most interested in. Make sure the proposed techniques really are 'best' for your research. HPLC and LC-MS may not be the right tools. This way you can spend your time collecting and researching samples and the analytical experts can work out the details needed to extract and measure the compounds.
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I am doing my research to build a lab scale solvent extraction system (Liquid-Liquid extraction) and I need a drawing for parts and details.
Any comments will be appreciated.
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Thanks Alan, I have already done the experiments in separatory funnels. Now I want to do it in continuous mode. So I need a to make a simple mixer-settler system.
I have already seen the koch modular column but as i said I want to make a mixer-settler.
The solution has Zn-Mn (40-15 g/L) and the solvent is DEHPA (diluted in kerosene).
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I'm using steam extraction of isolate volatile oils from a plant. The yield I get contains a clearly visible separate layer of oil on top of the aqueous layer. Since the yield is separate and prominent, I was wondering if I could just pipette the top layer off(a mixture of the desired oil and water) and put it in a long tube-like vessel (think test tubes but with a smaller diameter), let it stand and when the top oil layer becomes prominent and clearly visible just pipette it off (like we do in solvent extraction using a separating funnel but kinda, upside down) instead of going the usual route of solvent extraction.
Obviously there would be the possibility that we'd have an oil sample with trace amounts of water in it. Can I run this sample through Gas chromatography-Mass spectroscopy? Or do I need a sample completely free of water?
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Dear Juhaer, thank you for this interesting technical question. In general it should present no problem if you use an oil sample which contains traces of water. For more information see e.g. the following potentially useful link:
SAMPLE PREPARATION FUNDAMENTALS FOR CHROMATOGRAPHY
However, it's rather easy to remove the traces of water from your sample. For example, dilute the sample with 5-10 times its volume of diethyl ether and then dry the solution over anhydrous sodium or magnesium sulfate. Next day filter off the drying agent, was it twice with diethyl ether, and then evaporate the combined filtrates using a rotary evaporator. This should give you the water-free sample.
Good luck and best wishes, Frank Edelmann
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I have a tough nut to crack. I spiked a mixed standard (Amitrole, ETU, PTU, Cyromazine, Mepiquat, Chlormequat, and Daminozide into 10 g apple and stored them in a freezer over the weekend and extract with different solvent such as
1)      1% formic in methanol
2)      1% ammonium hydroxide in methanol
3)      1% ammonium hydroxide in acetonitrile
4)      1% sodium hydroxide in methanol
5)      DMSO
6)      Dimethyl formamide
7)      Dilute acetic with EDTA (glyphosate solvent)
8)      1:1 methanol:0.1 N HCl room and 80 C 15 min (paraquat solvent)
9)      1g sodium acetate + 10 mL methanol (Richard Krause JAOAC 1989 method)
10)   Methylene chloride (Simon Hird) method
The issue is I got all but ETU and PTU. These two analytes are very hard to extract. If I spike and vortex and wait for 5 min, I got good recovery just solvent 1. But if I let it sit for 1 hour at room temperature, no ETU or PTU recovery.  There are a lot of papers for ETU/PUT in fruit and vegetable out there and they had good extraction yield; however, I suspect that they are all freshly spike or did not indicate that they store before extraction. 
Thanks,
Narong
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We don't know until you do the experiment yourself.
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I'm working on extracting avocado peel oil with 2 methods
1st is a solvent extraction (n-hexane, 37°C)with soxhlet
The 2nd, i want to realise a macération extraction but i don't know what solvent i can use without degrading the oil or i can do a cold method of Extraction
anyone has an idea what should i do in the 2nd method ?
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Dear Widad Nafid thank you for asking this interesting technical question. Please have a look at the following potentially useful RG link which might help you in your analysis:
Extraction-and-Characterization-of-Oil-from-Avocado-Peels
This article has been posted as public full text on RG. Thus it can be freely downloaded as public full text.
What makes me wondering about this article is that the authors used n-hexane because of its "very low value of toxicity". This is certainly not quite true. n-Hexane is significantly toxic and should not be used for processing foods.
Good luck with your work! 👍
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Should I add in 3A molecular sieves into the SnO2 solution with isopropanol added? I am planning to use it on top of perovskite (MAPbI3) layer but the water comes with the SnO2 solution can damage the perovskite layer, so the water has to be removed first
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Soo Yew Hang Replacing the water with a different liquid will change the pH. Indeed, there will be no pH since there will not be any H+ ions.
Both the centrifugation and filtration options have benefits and disadvantaged. Both require some investigation to optimize the process.
For centrifugation, any surfactants etc that are not attached to the particles will be removed. With filtration, the size of the filter pores and the molecular weight of the surfactants will determine how much, if any, is removed. Simple surfactants are likely to pass through the filter whereas very large polymer surfactants may be retained.
Whether or not centrifugation results in aggregated particles depends on how they are stabilized and other factors such as how big the particles are, their density and how long you centrifuge for.
It is likely that drying will lead to some irreversible aggregation. However, it will remove more water than the centrifugation option. You need to assess the maximum water concentration you can tolerate. If it is, say, 1%, then a few centrifugation/redispersion cycles may work well. If it has to be less than 0.1%, drying may be needed.
Of course, practically, the filter + drying is easier and quicker. Depending on how small and dense your particles are, an appropriate centrifuge could be expensive.
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I determined the desorption efficiency of BTEX based on the NIOSH 1501 standard at five different concentrations (0.5/2/4/50/100 mg/L). I injected 20 uL of DE stock solution onto 400 mg charcoal with a microliter syringe and allowed it to stand overnight. After that, I used dichloromethane to desorbed it and analyzed it by GC-FID. The result is showed in the picture below. I wanted to know why these lines are curved and how to apply them when analyzing samples. Thank you in advance.
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Nguyen Binh, On what basis do you think that the lines illustarated above should be straight lines? The maxima on the desorption efficiency vs C line are also incomprehensible. Moreover, in order to make the problem clearer, it is worth specifying how desorption efficiency was defined. Usually the value of "efficiency" does not exceed 100% (1), but it depends on how this value was defined.
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Please, l need a clear experimental Proceedure for the extraction and purification of pigments from an Insect ( Weevils and Aphids)
Please can l get the step by step extraction procedure before the use of HPLC
Solvent Extractions, l guess maybe okay , but l am not sure yet of the adequate chemicals/reagents that maybe needed.
Finally as it is a pigment( Protein) do l need to pass any of the supernatant through indirect heating by use of water bath?
I look forward to your advise, suggestions, materials, journals and practical manuals that could be of help
Thank You
Best Regards
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Dear Jerry Nwabasa many thanks for your interesting technical question. Please have a look at the following potentially useful article which could help answering your question:
Optimizing conditions for the extraction of pigments in cochineals (Dactylopius coccus Costa) using response surface methodology
Also please see this relevant article:
Isolation, Purification, and Identification of an Important Pigment, Sepiapterin, from Integument of the lemon Mutant of the Silkworm, Bombyx mori
This article is freely available as public full ext on ResearchGate
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My qualifying exams are the next week and my university library is out of copies! I would greatly appreciate your help.
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Hi Arini,
Are you sure you will be able to go over this book and be ready for the exam in one week?
Good luck
Rafal
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I need a guideline for designing extractive distillation column. I have already design this column in Aspen Plus however I have to make hand calculations. Can anyone help me, please?
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Hello
could@@@@ u please send me the simulation file on aspen plus of the design of an extractive distillation or a tutorial related to this subject thx
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I want to separate a complex mixture of esters into medium and high molecular weight esters using solvent extraction.
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I have attached two articles. I hope they woul be useful.
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Capsaicin extraction with supercritical CO2 is a vastly researched topic, however, solubility of capsaicin in CO2-saturated water(at ambient or 2-3 times) atmospheric pressure and room temperature (suppose, 298 K) have not been come into my knowledge. What is the role of co-solutes like sucrose or phosphoric acid in dissolving the capsaicin from plant materials (e.g. chilli, paprika)?
Note: This question is inspired from the anecdotal experience that, adding some chilli (Capsicum frutescens) seeds on carbonated beverages drastically increase "sharpness" of "taste" of beverage, which is less true if much CO2 is released from the bottle by repeated shaking and slow venting of the built-up pressure within the beverage container.
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Hi.
I'm doing some work on arsenic speciation. I am following a paper titled, "SPECIATION OF ARSENIC IN A CONTAMINATED SOIL BY SOLVENT EXTRACTION." which calls for the use of chloroform or benzene to extract arsenic trichloride from a hydrochloric acid solution. The paper states that other solvents can also be used but does not go into detail.
I am looking for a safer alternative to chloroform or benzene. Can anyone make a suggestion please?
Thank you.
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Hi Chinaza.
Thank you for your contributions, but I am looking for an organic solvent that is suitable for extracting arsenic trichloride from an aqueous solution. Chloroform or benzene is used in the paper mentioned above but these have health risks. I am looking for a safer organic solvent.
Regards
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i was trying to look into the usage of ionic liquid and stumbled upon a few papers on their functions in extracting metal ions. i was thinking of using them in extracting value added components and in my case, in fish lipids preferably omega-3.
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Yes we can apply ionic liquids to extract lipids. but we have to design the IL based on their polarity. as to me non polar ILs (less polar) mixed with organic solvetnts are better for lipid extraction than polar ILs. see this paper
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My project is extraction of quercetin from onion peel.How to find quercetin concentration in solvent?Extraction is done using soxhlet extractor.Solvent we used is Ethanol.Done with different concentration of ethanol that is 40,50,60,70,80%
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The most used methol is HPLC with an analysis time of 15 min.
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Hi,
I'm working on some textile dyes which are reactive azo in nature. Can anyone suggest me best solvent for extraction process to use it for further analytical methodologies like FTIR? 
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For each family of dyes, there are specific solvents according to their chemical structures (see Color Index)
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I am working on pesticide degradation. please tell me best method for the extraction of Chloropyrifos from the soil by using solvent.
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how to adding volume amount in the formula which is used to dilute the extrat sample after HPLC analysis. (@ David Van Meter )
thanks.
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Recently we came up with a sticky challenge; where by mistake my students dissolved LH-20 Sephadex in water for column preparation/packing buy not knowing that this will get dissolved. As Sephadex is an expensive material, we planned to dry it in Freeze drier, but after drying when we take it out from drier, it absorbs moisture from air and get sticky. We tried with rotary as well but get the same effect. After successive failures, we thought to dry it solvent - solvent extraction methodology. In this experiment, we dissolved LH-20 in distilled water, added equal volume of n-butanol in it and started its drying through rotary evaporator. As soon there is less than half of solvent left, we added equal amount of methanol it and dried it completely through rotary evaporator. Luckily, we get it dried with no stickiness and got a smooth powdered material.
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Congratulations! Focus on objective always bring towards success.
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Describe selection of best organic solvent for extraction of phyto chemicals from plant leaf.
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Hi;
Instead, I propose you a new extraction technology: microwave assisted, solvent-free, based on the combined use of pressure, temperature and microwave irradiation.
With my best regards
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Does anybody have any idea what is the optimum or lower limit for a uranium concentration in acidic leachate for solvent extraction to be profitable?
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Hello, For my part, a technical and economic study must first be realized. solvent extraction for uranium ore is only one step in its recovery. the product of the leaching and drying (yellow cake) must still undergo an electrometallurgical treatment in order to enrich it. For the question of economic profitability, the leaching recovery rate should be, after experimentation, the basis for judging whether the method is profitable in relation to the price of the "yellow cake". the most important thing is to know the price of leaching and the product and the adequate recovery rate.
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I am looking for the best solvent for the extraction of Capsicum species fruits. In fact, I am aware that specific type of solvent is required for isolating compounds from medicinal plants. Through the literature study, I have found that water (H2O) is the best solvent since mostly decoction is prepared using water by the researchers. However, some other paper also suggest that methanol (CH3OH) and ethanol (C2H5OH) also exhibit desirable result.
What are your suggestions? Thanks in advance!
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crude extract by 70% ethanol
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There is plenty of evidence implicit in the published geochemical work that prolonged solvent extraction (especially aiming to remove oil based mud contaminants) leads to reduced pseudo maturity (e.g., vitrinite reflectance, pyrolysis Tmax).
A remedy for this may be simply conducting thermovaporization of the powdered source rock sample; instead of solvent extraction.
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Dear Mr. Mamaqani. I definitely agree that solvent extraction for removal of drilling contaminations will certainly affect pyrolysis parameters like S1 (free hydrocarbons) and S2 (pyrolyzable hydrocarbons. NO doubt.
Therefore in my question and quest I specifically mentioned vitrinite reflectance and pyrolysis Tmax. So we are investigating the possibility of solvent extraction on maturity determination.
In fact what I started to think about effect of solvent on kerogen is somehow similar to coal swelling when exposed to particular solvents. Prolonged solvent extraction may lead to sorption of the solvent by the macromolecular network of the kerogen which is a entangled structure. If the solvent is sorbed into this structure then it cannot be removed by simple oven-heating of the solven-extracted powder. It follows then that this phenomenon will lead to serious effects on maturity determinations by geochemical or optical means.
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I have a b-diketone complex in the ionic liquid phase. How could I extract it
thanks for helping us
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I am using dichloromethane to extract BDDE after spiking the matrix sample with BDDE in methanol. without long sonication my recoveries are poor. what is the best solvent for the extraction, i prefer not to use dietyel ether
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Did you solve this problem? Which solvent you used at last? Karin Tal
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how to extract (organic acids) citric acid from water to organic (Solvents) layer, which solvent's or combination of solvents are suitable?
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In a crude extract use
1. n- Hexane to remove non polar compounds
2. Chloroform to remove all pigments
3. Ethyl acetate for the bio-active compounds
4. n-Butanol for hydrocarbons
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I'm currently conducting sequential extraction of plant metabolites using Water, Hexane, Dicholoromethane (DCM), and Methanol. In which order should conduct the sequential extraction ? Thank you in advance.
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Start from non-solvent ,hexane or petroleum ether 60-80 oC to separate the non- polar compounds oils and fats( fatty acids, essential oils and some sterols) , it is called defatting. Then use more polar solvent , ethyl acetate then methanol, 80% methanol and finally water.
Check the components for each fraction by TLC, separate the single compounds by MPLC ( Flash chromatograghy)
Identify the single comp. spectroscopically.
Test their desired biological activities.
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Once I found out that nitrogen gas removed my anthocyanin more than its solvent (ethanol)
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Vacuum drying and freeze drying would work well. However, freeze drying is an expensive and time consuming method.
Vacuum drying is one of the the ideal methods for drying materials sensitive to heat or oxygen due to the advantage of drying at low temperature and minimizing the possibility of oxidation reactions. Since you are working with bioactives you will have to be careful with the temperature you select.
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I have used ethyl acetate as a solvent for extraction of acetic acid from pyrolysis oil in 1:1 ratio. I have a HP5 (30mX0.32mm) column
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Gas Chromatography with an internal standard or coupled to a (Tandem) Mass Spectrometer is commonly employed, although the acetic acid might damage your column.
HPLC or LC-MS are also possible, using an 8% cross-linked sulfonated polystyrene cation exchanger and an ethanol gradient mobile phase.
Capillary Electrophoresis (CE) with UV detection would work, if the sample concentrations are within the LOD of the instrument. You can calculate it from the following literature values:
Acetic Acid (pH~7)
λmax: 200nm
Amax: 0.670
Ɛmax: 67
(McConnell et al.)
If you're really hard-up, you can titrate 0.1N NaOH in conjunction with a pH meter, and calculate the concentration based on the inflection point (assuming HOAc is the only acid in your extract).
For a decent sampling of methods you can check out PubChem: https://pubchem.ncbi.nlm.nih.gov/compound/176#section=Analytic-Laboratory-Methods
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For the liquid-liquid extraction, I have to filter the culture, I must use the 0.20µm filter or another??? , please explain me
I had essayed the extraction with acetate ethyl, and the organic phase was colorless. In your opinion, the absence of the color in the organic phase allows us to predict the inefficiency of the extraction???? And what is the best solvent for this extraction????
Thank you,
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Please see attach.
Best Regard.
Lett Appl Microbiol. 2009 Jun;48(6):705-11. doi: 10.1111/j.1472-765X.2009.02599.x. Epub 2009 Mar 30.
Factors affecting the production of Trichoderma harzianum secondary metabolites during the interaction with different plant pathogens.
Vinale F1, Ghisalberti EL, Sivasithamparam K, Marra R, Ritieni A, Ferracane R, Woo S, Lorito M.
Author information
Abstract
AIMS:
Strains of Trichoderma spp. produce numerous bioactive secondary metabolites. The in vitro production and antibiotic activities of the major compounds synthesized by Trichoderma harzianum strains T22 and T39 against Leptosphaeria maculans, Phytophthora cinnamomi and Botrytis cinerea were evaluated. Moreover, the eliciting effect of viable or nonviable biomasses of Rhizoctonia solani, Pythium ultimum or B. cinerea on the in vitro production of these metabolites was also investigated.
METHODS AND RESULTS:
T22azaphilone, 1-hydroxy-3-methyl-anthraquinone, 1,8-dihydroxy-3-methyl-anthraquinone, T39butenolide, harzianolide, harzianopyridone were purified, characterized and used as standards. In antifungal assays, T22azaphilone and harzianopyridone inhibited the growth of the pathogens tested even at low doses (1-10 microg per plug), while high concentrations of T39butenolide and harzianolide were needed (>100 microg per plug) for inhibition. The in vitro accumulation of these metabolites was quantified by LC/MS. T22azaphilone production was not enhanced by the presence of the tested pathogens, despite its antibiotic activity. On the other hand, the anthraquinones, which showed no pathogen inhibition, were stimulated by the presence of P. ultimum. The production of T39butenolide was significantly enhanced by co-cultivation with R. solani or B. cinerea. Similarly, viable and nonviable biomasses of R. solani or B. cinerea increased the accumulation of harzianopyridone. Finally, harzianolide was not detected in any of the interactions examined.
CONCLUSIONS:
The secondary metabolites analysed in this study showed different levels of antibiotic activity. Their production in vitro varied in relation to: (i) the specific compound; (ii) the phytopathogen used for the elicitation; (iii) the viability of the elicitor; and (iv) the balance between elicited biosynthesis and biotransformation rates.
SIGNIFICANCE AND IMPACT OF THE STUDY:
The use of cultures of phytopathogens to enhance yields of Trichoderma metabolites could improve the production and application of novel biopesticides and biofertilizers based on the active compounds instead of the living microbe. This could have a significant beneficial impact on the management of diseases in crop plants.
ach.
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Dear All,
I'm searching for a method to extract the oragnic phase from a volume of 10 ml of a mixture of hydrocarbons-water for the GC-MS analysis.
Can anyone help me with a solvent extraction or centrifugation procedures ?
Thank you much for your support.
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Extract your sample by using n-hexane or DCM. How ever, the volume of solvent depend with the amount of organic phase in your sample. Extract three or more times from the same sample for more yield. Then concentrate your extracts using rotary evaporator and filtered through syringe filters and inject to GC-MS.
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I use hexane:ethyl acetate (6:4) as solvent for extraction of pesticide from the spiked amount. The pesticide Hexaconazole in acetonitrile (5 ppm) is my spiked pesticide.
After final concentration in rotary evaporator followed by florisil open column; the recovery was very low (less than 60%) with a higher amount of peak area of solvent in the LC-UVD peaks. Now, I am looking for tips and technique for proper concentration of ethyl acetate by rotary evaporator.
Expecting experts kind contribution in this regard.
-Aniruddha Sarker
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Grzegorz Boczkaj Thank you for your kind interest. The temp of rotary evaporator is fixed at 40 °C with vacuum pressure of 120 psi. And H:EtOAc 6:4 solvent is the extracting solvent in florisil open column. The extracted pesticide is 5 ppm spiked Hexaconazole in acetonitrile.
But in LC-UVD peak, there is a visible unexpected solvent peak. How to reduce this unexpected peak of solvent?
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Recently I were been assigned a new task which I have never done before, to extract compounds from a plant, and the tutor told me to explore a new composition from it, which she regarded as an innovation. The question is after I have been searching for a long time, and done some related experiments, the method she told me was no more new to all the people. By contrast, this procedure has been mature to some extent. The traditional way is solvent extraction (some people use water, ultrasonic,etc. Supercritical fluid extraction maybe the latest technology, which our lab couldn’t afford to have this device). The next procedure is purification with column chromatography (or HPLC), and finally people may do some functional experiments using rats or mice. Is there any new ways or technology to do this experiment, and it will be nice if it won’t cost too much. If necessary, we can rent related device to finish the experiment, but please tell me what kind of technology or devices we need. Thank you!
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Hi Fangyuan,
years ago we extracted natural substances from various biological sources, analyzed them with LC/MS and purified them (mg scale). Volatile substances were extracted e.g. with steam distillation. Otherwise, a Soxlhet extraction of solids was often carried out. Common solvents were methanol, ethanol, ethyl acetate, dichloromethane, diethyl ether, n-hexane. The extracts were then concentrated and first analyzed by LC/MS (TOF). The extracts were then fractionated and the fractions were then analyzed by 1H-NMR and C13-NMR. Unfortunately, the focus in our laboratory has shifted, i.e. we have not performed natural product analysis for years. Chemists do not like natural substances with many chiral centres.
Maybe this link will answer some of your questions:
Regards
Markus
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Can we do homogenization of fungal mycelium using liquid nitrogen for secondary metabolite extraction and then do ethyl acetate solvent extraction
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If you just want to get secondary metabolites, then you will not necessarily liquid azod. Make it just not necessary to obstruct the work
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i have extracted the henna dye from leaves with water only and i want to check the solubility of henna dye. Also how the yield % can be calculated of henna dye if only water is used as a solvent and extraction was done with microwave/ultrasonic.
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Dear Rabia,
By answer on our request, you can use the spectral analysis approach using standardized spectro-colorimetry
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I am wondering whether you can help me solve something? If I was calculating an solvent extraction yield, using 3 different solvents, had a starting weight of 50g, and produced extracts weighing 1.008g, 0.788g, 5.687g sequentially. Would I do the yield calculation using ((extract weight/50g) x 100) or instead ((1.008g/50g) x 100) / ((0.788g/48.992g) x 100) / ((5.687g/48.204) x 100)?
Thank you for any help.
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Hi there. the calculation for each solvent extraction is as follow:
1st solvent yield={ (50-1.008)/50}X100. and the same thing repeat again for other solvent to calculate yield percentage. Cheers.
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Is it possible to break a π bond between a solute and a magnetic solvent using magnetic force?
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I believe yes, Amir hossein Aref it depends on what/which molecule you are considering. As for example if we consider weaker bonded CH3CL, in which C-Cl specifically. Then we can calculate the energy require to break this bond. Like for 9 debye the breaking energy lies near about 3.5eV.
So theoretically you can break these like weaker bonds using electric/magnetic force, And if you can build a machine which such capabilities you can also practically break these type of bonds.
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Dear fellows I am interested to identify the medicinal activities of polyphenolic compounds from Plants. Can anyone please suggest a method to extract and purify only polyphenolic compounds based on solvent extraction.
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Extract can be purified by following method, if it is prepared in water. First remove the fatty material by layer separation with n-hexan, then separate with 1-butanol, you will get your polyphenol/organic portion.
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Hello everyone,
Can anyone help me how to select the best solvent for extraction of polycyclic aromatic hydrocarbon (PAHs) from soil/sediment sample.
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Thank you Sir!
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Please, recommend articles on the extraction of organic substances in aqueous two-phase systems, in traditional extraction systems. I am interested in such objects as aliphatic and aromatic carboxylic acids, sulfur and phosphorus-containing organic compounds.
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Have a look on Separation and Purification Reviews article. You should find one or more.
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Hello everyone,
I've been using glass beads cell disruption followed by solvent extraction to release carotenoids from yeasts, but, for most of the solvents I've used, the pigments get dissolved in the solvent, but the upper layer resulted in a dense mass, looking like a gel, or maybe an emulsion. Has anyone gone trough this? do you know how to dissolve this mass?
Thank you
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Thank you, Yuri and Detlef. I'll try your suggestions. Best regards!
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how can we extract solution with ethylene dichloride and can we use some different solvent in place of ethylene dichloride. please sir suggest any solvent and explain the solvent extraction procedure.
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In general, try to avoid halogenated solvents. They are typically more environmentally harmful and are often carcinogenic. You are quite right to want to replace ethylene dichloride. I am not familiar with your particular application but let me offer some advice about finding a replacement. You should consider a) boiling point, b) water miscibility, and c) solvatochromic parameters.
A. If the solvent must be refluxed during the procedure (either during a synthesis or a Soxhlet extraction) then the replacement solvent should have a similar boiling point. Otherwise the bp is not so important.
B. If you're using the solvent to extract products from water, then the solvent must not be water-miscible. If you aren't using water, then acetonitrile might be a good replacement for ethylene dichloride.
C. Solvatochromic parameters measure solvent properties such as acidity, basicity, and polarity. I recommend using the Kamlet Taft parameters. The acidity (alpha) value of ethylene dichloride is 0. Its basicity (beta) value is also zero. But its polarity is quite high (pi star value of 0.81). Therefore you should seek a solvent that has very low alpha and beta values but a very high pi star value. Unfortunately, nonhalogenated solvents of this type are very rare (see Green Chem., 2012, 14, 1245) but I suggest that you try toluene, anisole, or even ethyl acetate. Ethyl acetate might not be polar enough, while toluene and anisole have rather high bp.
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Dear researchers,
I fabricate the UF PVDF membranes by phase inversion method (NIPS); therefore, they are water- wet membranes. Then I immerse them in aqueous alcohol solution. What is the reason of replacing the alcohol molecules with water molecules in the pores?
Regards
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Usually the membranes prepared immersing in the final water bath for a period of 2-3 days, with daily change of water, so as to ensure thorough removal of residual solvent and additives prior to final membrane drying.So I suppose that you are used alcohol instead of water this is depending on the type of solvent that used in the membranes preparation.
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There are so many techniques are available for the extraction of natural product (Phytochemicals) like
1. Classical solvent extraction procedures
2. Ultrasound-assisted extraction
3. Microwave-assisted extraction
4. Extraction with ionic liquids
5. Accelerated (pressurized) solvent extraction
6. Supercritical fluid extraction
7. Extraction on solid phases
8. Distillation methods
All these techniques have their own disadvantages. The design of green and sustainable extraction methods of natural products is currently a hot topic in the multidisciplinary field of applied chemistry, biology and technology. What are the main techniques for green extraction of natural product. This goal can be achieved through optimal consumption of raw materials, improvement and optimization of existing processes, solvents and energy. the green extract obtained in such a way to have the lowest possible impact on the environment. Can anyone suggest best method for the green extraction through easily available and economic equipment?
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Organic solvents should be avoided.
But in order to use the appropriate solvent it is necessary to know the target phytocompounds.
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I would like to attach a carbon triple bond to a benzaldehyde ring and to do that i am trying to perform a williamson reaction: https://en.wikipedia.org/wiki/Williamson_ether_synthesis.
The two OH groups on my ring should turn into ethers, by making them react with a propargyl halide, in the presence of a salt, in my case, potassium carbonate. At the moment of extracting i have used ethyl acetate and water and i think it pretty much worked, at least to remove the salt. What was hard was to find a good combination of solvents that could return a visible separation on the TLC plates and that could also dissolve my product! I have tried various ratios of hexane and ethyl acetate but either i was not dissolving the product or it was not working on the TLC. Is this a frequent obstacle? How can I approach it? Thank you!
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it depends on your analytes if they are polar, you need stronger eluent (higher polarity).
For me DCM is slightly polar - you can try it with and without metanol addition.
regards,
G
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I have used liquid samples earlier but the results were not good, due to the major peak of OH group, all other peaks become inconspicuous and thus difficult to interpret. The other alternative which is mostly found in literature is solvent extraction using ethyl acetate or any other solvent. But again that method is not much useful as the dyes and hence their metabolite concentrations are in ppm that make the detection really hard . what should i do then?? is there any other method available or can somebody suggest me a better extraction (for sample concentration) procedure??
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in the extraction of dyes metabolites after bacterial degradation present in organic or aqueous layer for FTIR analysis?
the color of dyes present in aqueous extract
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Dear colleagues,
At what point does sequential solvent extraction make more sense? At crude extraction or fractionation stage?
One other thought would be to do crude extraction using MeOH and do sequentia solvent extraction when fractionating or do crude extraction right away using sequential extraction andat fractiontion point, only do solvent gradients.
Please share your ideas
Kindly
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I used distilled water as the solvent for extraction. The method used is maceration method. After that, I used rotovap to remove the distilled water. However, for gcms analysis, i don't know which solvent (organic solvent) is suitable to use to redissolve the sample.
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Methanol
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I am going to do analysis of antioxidant activity of some medicinal plants, for that I should go through solvent extraction. I want to ask that should I use the same solvents for thin layer chromatography which are used for extraction of the plant material. Please help me out.
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You can use the same solvents in both your experiments and TLC.
Recommended mobile phases:
-DCM-MeOH (40:1, 30:1, 20:1, 10:1, 5:1)
-EtOAc-petroleum (3:1, 2:1, 1:1, 1:2, 1:3)
According to the retention factor of your samples, you will be able to decide which mobile phase suits you best.
Regards
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A common problem in zinc solvent extraction system is precipitation of zinc sulfate, specially in scrubbing segment. Can I dissolve it by changing the level of some factors as temperature, chemical potential or ...?
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I am not sure whether your question concerns the solubility of zinc sulfate in water, but ZnSO4.7H2O is very soluble in water under neutral or acidic conditions (> 50 g/100 mL at room temperature). Solubility does increase with temperatures, e.g. > 100 g/100 mL at 70°C. Can you describe your problem in more detail?
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I have extracted PAH by soxhlet extraction using hexane as the solvent. Previously, I had passed the extracts through 2 µm filter. I still found that the samples were dirty. I wish to do florisil clean up. I was looking at a protocol for florisil clean up after the extraction process is complete.
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I had use this clean-up procedure for hexane:DCM extracts from soil samples:
The extracts clean-up apparatus was built from a glass column (1.5 cm ID and 40 cm height) packed from the top; 2g florisll (200 mesh), followed by 2 g of anhydrous Na2SO4, and 2 g of activated silica gel (60-200 µml).
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I am trying to isolate the polar organic compounds from leaves, flower& stem of herbal plant? Which is the best solvent to use and why?
Which is the best method for the isolation of the polar organic compounds from herbal plant?
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Dear All
In my experiment, I used 1.2 gram of dried peel and then dissolve into the 50ml water as solvent extraction at Microwave assisted extraction (MAE). The problem is, the peel cannot fully dissolved into the water and still contain sediment as file attached. the calculation for the sample concentration as follow, Con (mg/l)=(1.2g/50ml)*1000=24mg/ml. Conc(ppm)=24mg/ml*1000=24000ppm
My question is, Can I assume my concentration sample is 24000ppm even it's not fully dissolved into the solvent extraction? Any Idea
Regards
Azlan
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Hello again Azlan.
You're probably using a centrifuge to separate your both "phases" of your solution and not a homogenizer.
A homogenizer would grind the bulk of your samples and allow the solvent to better extract your samples and should be done prior to submitting to MAE.
Best of luck,
Filipe
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An oil rich substrate is not producing the expected result of reduction in ANFs after microbial fermentation. Could it mean that defatting or solvent extraction using hexane needs to be done first prior to solid state fermentation? Pls kindly add a published reference
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High oil or fat content can sometimes be detrimental to fermentation. But first of all, what do you mean by high fat or oil content? In some cases, certain microorganisms grow at high lipid contents because they are adapted to produce lipases, thereby allowing access to fatty acids. On the other hand, as mentioned by Mr Calt, a high content of oil in a fermenter can increase the viscosity of the system and consequently reduce the KLa negatively impacting the fermentation.
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Hallo,
I want to extract semipolar phytochemicals from the second metabolism from wheat bran.
But i don't want Starch and Protein in my extract. So is there a good way to extract the phytochemicals (like benzoxazinoids, hydroxy cinnamic acid derivates, flavanoids etc.) without getting to much of the starch and protein? Maybe an extraction with ethyl acetate? SPE-Extraction?
Thank You
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Dear Sir. Concerning your issue about the extraction of the phytochemicals (like benzoxazinoids, hydroxy cinnamic acid derivates, flavanoids from wheat bran. Optimized extraction of bioactive phytochemicals is of signifi-cant importance to accurately quantify the phytochemicalcontent in foods and plant products. Accurate quantificationallows establishment of proper dietary and safety guidelines.The bioactive phytochemicals exist in multiple forms: soluble(free and conjugated) and insoluble bound forms. It is essen-tialtounderstandvariousformsofthebioactivephytochemicalstoaccuratelyquantifythemandunderstandtheirbioavailabilityand health promoting properties. A wide array of extractionsolvents and technologies have been reported in the peer-reviewed literature (Herrero, Cifuentes, & Ibañez, 2006; Luthria,2012a).The conventional extraction methods include Soxhletextraction, stirring, distillation, manual mixing, and percola-tion. However, in recent decades, several new technologiesincluding, microwave assisted extraction, ultrasound-assistedextractions, pressurized liquid extraction, subcritical fluid ex-traction,solid-phaseextraction,andenzyme-assistedextractionhave been used to automate and/or improve the yields of bioactive phytochemicals. I think the following below links may help you in your analysis:
Thanks
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I would like to know the best solvent extraction procedure of Astaxanthin from shrimp and crab waste.
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I am surprised that many researchers at this site would not take advantage of the internet to find the answers. I spent less than 5 min to get these informations on Google and they should do the same before asking the questions on this board.
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Solvent Extraction Method for detection of metals in water samples
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I would rather recommend you to use spectroscopy, atomic absorption or ICP. they are much easier and more precise
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I am analyzing the role that different solvents play in the extraction of certain organic compounds. As a part of my analysis, I want to compare what would be the energy duty if I was to proceed the distillation to obtain those compounds using the analyzed solvents. Is it reasonable to calculate it by the difference between the (solvent) enthalpy at room temperature and the enthalpy of vaporization (for each respective solvent)?
Important: This calculation is meant to be a rough estimation for an energy balance analysis, not for the design of the distillation column.
Thanks!
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For your analysis with the enthalpy of vaporization of the solvent is sufficient. The energy needed to bring a solution, mostly solvent, to the bubble point is negligible compared to the energy needed to vaporize it.
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Extraction of TAG
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My research is about Techniques of Basil herbs essential Oil extraction. I did study some current existed journal about essential oil extraction. Why only solvent extraction method was used, but not solvent distillation? And why cant we use solvent for distillation?
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If you use organic solvent you will lose your oil because it will dissolved and mixed with solvent. How to separate them?
Using water is more suitable to separate oil and water which are immiscible.
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One of the advantages esi-ms, the sample no need to concentrate its compounds, that mean it can be analyzed directly without remove the solvent extraction..What the purpose of ESI at mass spectra(ESI-MS)?
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Dear Sir. Concerning your issue about the purpose and advantage ESI at mass spectra. Electrospray ionisation mass spectrometry (ESI-MS) has become an increasingly important technique in the clinical laboratory for structural study or quantitative measurement of metabolites in a complex biological sample. The first part of the review explains the electrospray ionisation process, design of mass spectrometers with separation capability, characteristics of the mass spectrum, and practical considerations in quantitative analysis. The second part then focuses on some clinical applications. The capability of ESI-tandem-MS in measuring bio-molecules sharing similar molecular structures makes it particularly useful in screening for inborn errors of amino acid, fatty acid, purine, pyrimidine metabolism and diagnosis of galactosaemia and peroxisomal disorders. Electrospray ionisation is also efficient in generating cluster ions for structural elucidation of macromolecules. This has fostered a new and improved approach (vs electrophoresis) for identification and quantification of haemoglobin variants. With the understanding of glycohaemoglobin structure, an IFCC reference method for glycohaemoglobin assay has been established using ESI-MS. It represents a significant advancement for the standardisation of HbA1c in diabetic monitoring. With its other applications such as in therapeutic drug monitoring, ESI-MS will continue to exert an important influence in the future development and organisation of the clinical laboratory service. I think the following below links may help you in your analysis:
Thanks
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My research is about Techniques of Basil herbs essential Oil extraction. I did study some current existed journal about essential oil extraction. Why only solvent extraction method was used, but not solvent distillation? And why cant we use solvent for distillation?
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Hi
Components of plant material other than essential oil will get extracted in methanol/ethanol solvents. Therefore, you can't use methanol/ethanol as a solvent for extraction of essential oil from the plant material. Hydro-distillation (Clevenger apparatus) is the correct technique for the isolation of essential oil from plant material.
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I would like to try to additivate natural carotenoids extracted from industrial food wastes by solvent extraction into olive oil to enrich its antioxidant power. Is it better to use UPLC or UV-Vis spectrophotometrical analysis to determine the content of carotenoids in the oil?
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Thanks a lot for your kind help.
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Mixture of Ethanol:water (70:30) as solvent extraction at 50 celcius.
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thank you Markus christ for your help..
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I am working on bioactive compounds from bacteria for which I have to prepare crude extract by solvent extraction method, can I know what is the best way to obtain large amount of crude extract.
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Well, you should consider that many wild microorganisms do not produce huge amount of metabolites, hence you need large volume of fermentation broth to generate required amount of crude extract for your further experiments (antibiotic assays, purification, etc). An alternative approach is partial optimization of various culture conditions including inoculation size, aeration, or culture medium components, which considerably improves the yield of metabolites.
If you are still in screening phase for exploration of any potential natural products, or you don’t want to spend lots of efforts and time for the optimization purpose, then you can try in-situ extraction method using resins such as XAD-16N. However, you should not be greedy in addition of such resin as they may have adverse effect on production. Therefore, do some search to find out the possible correct percentage. Generally, 5 to 10% w/v is ok. Add them to culture medium before sterilization and increase the sterilization time to 20 min. Some researchers soak them before addition but that doesn’t really matter. However, wash them with water, methanol, and then acetone before application. After fermentation broth was harvested you can separate resin with sieve with appropriate mesh size. The metabolites are extracted from resin and biomass (if any) with the help of either methanol or acetone, then air dry it, preferably with N2, and store at -20°C for further use. The broth can also be extracted (see below).
If you don’t want to use in-situ extraction or you want to extract the broth after resin separation also, you may use liquid-liquid extraction method (LLE). The most common solvent used for this purpose is ethyl acetate which traps different metabolites with wide-range of polarity. However, you may use other solvent depending on the polarity of the preferred analytes, such as butanol as Isam already mentioned it, as below:
1- Separate biomass before LLE to avoid possible emulsion.
2- Add solvent to broth (1:1 v/v ratio) and plug Erlenmeyer with cotton and foil to avoid evaporation of the solvent.
3- Place the Erlenmeyer on magnetic stirrer and increase the rpm until homogeneity is reached (30-45 min)
Note: if the polarity of organic solvent and water is very different then you can see a homogenous solution. Therefore just try to have good mixing.
Note: if you use very high rpm (more than enough to make homogenous solution) then you may end up with emulsion which add centrifugation step.
4-Transfer the flask to cold room/refrigerator to allow two phases differentiation (organic solvent and aqueous solvent phases)
5-Separate the organic solvent phase and repeat the step 3 until no color change in organic solvent phase is observed.
6-Remove the organic solvent to dryness as soon as possible in a rotary evaporator (bath temperature ≤38°C) to prevent degradation of extracted metabolites, then store at -20°C.
Note: Some extracts are oily so can be completely dried out. Just remove the solvent and keep in freeze for further use.
Note: consider the boiling point of the organic solvent you want to use because higher boiling point needs more patients for removing organic solvent with rotary evaporator. For example, butanol boiling point is more than water and is around 118°C!
I suggest you use in-situ extraction for better result with less effort.
Hope it is useful,
Regards
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Can we use Soxhlet for extracting the secondary metabolites from the Actinobacteria fermented broth? Soxhlet is generally being used for dry/solid materials. If we adopt this to actinobacteria does it work?
or the regular solvent extraction is sufficient? Recommend me some rapid and efficient method to maximize the yield of total metabolites.
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Of course you could but you have to select the suitable organic solvents
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Hydrophobic resin adsorption is also an option. For example, take a look at http://www.deswater.com/DWT_abstracts/vol_73/73_2017_348.pdf.
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Hi ,
I intend to separate a doublet of peak eluting from reverse phase HPLC column, along with the main peak, a shoulder peak appears which I want to get rid of the main peak. PDA detector at 245 nm.The column is semi prep C18. Mobile phase is acetonitrile: water = 90:10 (i am not adding formic or acetic acid or TFA 0.01% in water which people do generally) flow rate semi prep 5 ml/min, anal 0.5 ml/min
I have also tried with different flow rates 3,4,6 ml/min, at temp 26 and 35 C, with gradients from 50:50 to 90:10 (for 10 min hold and then 50:50 in next 20 min, 30 min, and 40 min.In all cases, elution is there but poor seperation, still able to collect ~90% pure peak despite some loss of sample. Plz. guide me how can I improve resolution. see pdf. File 1 purity of collected peak by anal c18 isocratic, file 2  is semi-prep isocratic run, file 3 is semi-prep gradient run 
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Hi Prasad, in your case I would try another stationary phase. Changing the stationary phase will change the selectivity for your compounds too. Temperature, flow and solvent composition are useful when you are tackling with a separation problem, but changing the stationary phase has the biggest effect on selectivity. Greetings Markus
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I have a polymer sodium polystyrenesulfonate chain which has about 45 monomer unit and each unit contains one -SO3Na group. The chain also has one terminal unit with -COONa group instead of -SO3Na while the other terminal is having a -Br group. To convert these -SO3Na and -COONa group to -SO3H and -COOH groups I have treated them with HCl acid (1 M) and used the pH 1 to do so. Now, as I understand there will be NaCl as side product and I want to remove them. I found both these NaCl and the acid form of the polymer are soluble in water, I tried solvent extraction method using ethyl acetate but failed. Any suggestion will highly appreciated. Thank you in advance.
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Thank you very much for the information. I haven't ever tried it but I shall opt.
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I am doing work on alcoholysis reaction of fish oil by lipase 1,3 specific enzymes. For purification of 2-monoacyl glycerols (2-MAG) from the reacted oil  by solvent extraction, I have added ethanol and hexane with the reacted oil and placed in a separator. In which fraction (ethanol or hexane) I shall get 2-MAG and what is the cause?
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Thank you sir.
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Theoretically CO2 will react like completely non polar in it's super critical region then what is the reason to became a great solvent for extraction & chromatography. 
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Not sure what you meant by "react" - CO2 is not a very reactive compound. If you meant "behave" - you are right - even under supercritical conditions CO2 remains non-polar, although net polarity varies slightly with state conditions (pressure and temperature). It's considered a great solvent because of its tunability, which is the ability to vary solubility by changing pressure and/or temperature. Although with neat CO2 you will dissolve mainly non-polar compounds, you can still tune their solubility by changing the state conditions - which can become an useful tool for fractionation and recovery.
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I have experimental data for solute concentration in feed solution and raffinate for different A/O (temperature, pH and extractant concentration are constant).
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Dear Jovana Djokic
In a LLE process, theoretical steps of extraction can be estimated using Distribution Isotherm and Mc. Cabe Tail diagram. In order to obtain Distribution Isotherm, various organic to aqueous ratio are mixed in a constant temperature. After reaching equilibrium, two phases (aqueous and organic) are separated and metal concentration are measured in them. 
Distribution Isotherm and an operating line are used in order to draw and analysis of Mc. Cabe Tail diagram. As the mentioned operating line is a straight line, it can be drawn by any 2 points of the line. Also, it can be drawn by a point and the line slope. Slope of this line is aqueous to organic ratio and the one point which are needed to draw the line (X0) is the concentration of copper at the starting time of process. With having these all, Y1 will be reached by the following equation.
Y1=A/O(x0-xn) + yn+1                                                (1)
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    Please suggest me .I want prepare calcium thioglycolate from calcium hydroxide and thioglycolic acid 80% solution but we are using methanol solvent, but here calcium hydroxide insoluble in methanol how to remove excess of calcium hydroxide from calcium thioglycolate?
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do u find a solution for ur problem?
what is difference  about synthesis  of calcium thioglycolate (2:1) and (1:1)?