solid liquid extraction experiment

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Applications and Summary

Solid-liquid extraction.

Source: Laboratory of Dr. Jay Deiner — City University of New York

Extraction is a crucial step in most chemical analyses. It entails removing the analyte from its sample matrix and passing it into the phase required for spectroscopic or chromatographic identification and quantification. When the sample is a solid and the required phase for analysis is a liquid, the process is called solid-liquid extraction. A simple and broadly applicable form of solid-liquid extraction entails combining the solid with a solvent in which the analyte is soluble. Through agitation, the analyte partitions into the liquid phase, which may then be separated from the solid through filtration. The choice of solvent must be made based on the solubility of the target analyte, and on the balance of cost, safety, and environmental concerns.

Extraction uses the property of solubility to transfer a solute from one phase to another phase. In order to perform an extraction, the solute must have a higher solubility in the second phase than in the original phase. In liquid-liquid extraction, a solute is separated between two liquid phases, typically an aqueous and an organic phase. In the simplest case, three components are involved: the solute, the carrier liquid, and the solvent. The initial mixture, containing the solute dissolved in the carrier liquid, is mixed with the solvent. Upon mixing, the solute is transferred from the carrier liquid to the solvent. The denser solution settles to the bottom. The location of the solute will depend on the properties of both liquids and the solute.

Solid-liquid extraction is similar to liquid-liquid extraction, except that the solute is dispersed in a solid matrix, rather than in a carrier liquid. The solid phase, containing the solute, is dispersed in the solvent and mixed. The solute is extracted from the solid phase to the solvent, and the solid phase is then removed by filtration.

In this video, an example of the solid-liquid extraction technique will be illustrated by showing the extraction of organochlorine residue from soil. The illustrated solid-liquid extraction entails combination of the sample with n -hexanes followed by ultrasonic agitation, filtration, removal of residual water by drying over CaCl 2 , and pre-concentration under flowing nitrogen. The as-prepared sample is then ready for analysis by a range of spectroscopic and chromatographic methods.

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1. Extraction of Adsorbed Organics from Soil

• Place 20 g of soil in a clean, dry wide-mouth Pyrex dish in a 50 °C oven and dry for a minimum of 12 h. After drying, remove the soil from the Pyrex dish and grind to a uniform powder using a mortar and pestle. Weigh 5.00 g of the soil and place it into a clean, dry round-bottom flask (100 mL in size). To the flask, add 15 mL of n -hexane. Place flask in an ultrasonic bath, and sonicate for 60 min.

2. Separation of Extract and Soil

• Prepare a Büchner funnel with analytical filter paper. Wet the filter paper with 1 mL of n -hexanes and begin vacuum filtration. Slowly pour the contents of the round-bottom flask over the filter paper. The Büchner flask now contains the n -hexanes with the organics extracted from the soil. The filter retains the stripped soil solids.

3. Clean up and Pre-concentration

• If the n -hexane solution is cloudy, there is residual water. To dry the n -hexane solution, add one small spatula of CaCl 2 . Swirl the solution and observe for a minimum of 15 min. If the solution is still cloudy and/or all of the CaCl 2 is clumped, there is still water remaining, and step 3.1 should be repeated. If the solution is translucent and the CaCl 2 is free flowing, then do not repeat step 3.1. Once a clear solution has been achieved, separate the hexanes from CaCl 2 using gravity filtration. If the extract concentration is sufficient for detection, the filtered hexanes may be transferred to a clean, dry flask for storage and later analysis. If extract concentration is low relative to the limit of detection, transfer the filtered hexanes into a clean, dry three-necked round-bottom flask, 100 mL in size. Place a rubber stopper into the center neck of the flask, and a rubber septum over one of the other necks. Leave the third neck open. Pierce the rubber septum and introduce a nitrogen flow through the flask. The nitrogen should be flowing in the space above the solution, not bubbling through the solution. The extract can now be pre-concentrated by flowing nitrogen to evaporate excess solvent. The sample is now ready for analysis.

Extraction is a crucial separation technique in organic chemistry, used to separate components of a mixture based on their solubilities in two different phases that do not mix.

Extractions are performed between two phases. In the case of a liquid-liquid extraction, the dissolved solute is transferred from one liquid phase to another. Extractions are also performed with a liquid and solid phase, called solid-liquid extraction, where the solute is transferred from a solid phase to a liquid phase. A simple example of solid-liquid extraction is coffee brewing, which involves the mixing of solid coffee grounds with water. The coffee flavor compounds are extracted from the grounds into the water to form coffee. This video will illustrate the principles of extraction, and demonstrate solid-liquid extraction in the lab through the removal of organochloride residues from soil.

Extraction uses the property of solubility to transfer a solute from one phase to another. In order to perform an extraction, the solute must have a higher solubility in the second phase than in the original. In general, very nonpolar solutes will partition into an organic phase, while very polar solutes will partition into an aqueous phase. The choice of phases will depend on the solute of interest.

The two phases also must be immiscible. Immiscible solutions never mix and remain as separate phases, like oil and water. Miscible solutions are completely homogeneous after mixing.

In liquid-liquid extraction, a solute is separated between two liquid phases, typically aqueous and organic. This is often performed in a separatory funnel fitted with a stopcock at the bottom and stopper at the top.

In the simplest case, three components are involved: The solute, the carrier liquid, and the solvent. The initial mixture, containing the solute dissolved in the carrier liquid, is mixed with the solvent. Upon mixing, the solute is transferred from the carrier liquid to the solvent, as long as the solute is more soluble in the solvent than in the carrier liquid, and as long as the carrier liquid and solvent are immiscible. The denser solution settles to the bottom.

There are two resulting phases: the raffinate, containing the carrier liquid, and the extract, which contains the solute and the solvent. In reality, there is likely to be residue of each component in both phases. Solid-liquid extraction is similar to liquid-liquid extraction, except that the solute is dispersed in a solid matrix rather than in a carrier liquid. The solid phase, containing the solute, is dispersed in the solvent and mixed. The solute is extracted from the solid phase to the solvent, and the solid phase is then removed by filtration. Now that the principles of extraction have been outlined, the solid-liquid extraction technique will be demonstrated by performing the extraction in the laboratory.

In this experiment, soil samples were collected from a brownfield site, similar to this one in Sewickley, Pennsylvania. Brownfields, as defined by the U.S. EPA, are real property, where the expansion, redevelopment, or reuse may be complicated due to the potential presence of hazardous contaminants. The pollutant of interest in this case is an organochloride: the herbicide atrazine . Once a soil sample has been collected from the site of interest, transfer it into the laboratory.

Weigh out 10 g of the soil in a clean, dry, wide-mouth Pyrex dish. Put the dish into an oven to dry for at least 12 h. Once dry, grind the soil to a uniform powder with a mortar and pestle. Place 5 g of the ground soil into a clean, dry 100-mL round-bottom flask. Add 15 mL of hexane and loosely stopper the flask. Place it into an ultrasonic bath and sonicate for 60 min.

Prepare a Büchner funnel with analytical filter paper. Once sonication is complete, wet the paper with hexane and begin vacuum filtration. Slowly pour the sample over the filter paper. Rinse the residual solids from the flask with hexane and add it to the filter. The stripped soil remains on the filter, while the hexane and extracted organics collect in the flask.

If the hexane solution is cloudy, residual water is present. To dry the solution, add a small spatula of desiccant, such as calcium chloride. Stir the solution until the desiccant is dissolved, and observe the solution.

If the solution is still turbid or if the calcium chloride has aggregated, there is still water in the solution. Repeat the process until the solution is clear and the desiccant is free flowing.

Next, remove the calcium chloride by gravity filtration.

If the concentration of the compound of interest is below the limit of quantification, it must be concentrated. Transfer the filtered extract to a clean, dry 3-necked round-bottom flask. Stopper the center neck, and place a rubber septum over one of the other necks. The third is left open.

Pierce the septum and attach tubing to a nitrogen line. Begin flowing nitrogen through the flask. The gas should be flowing in the headspace above the solution, and not bubbling through it. The flowing gas evaporates the excess solvent. Allow the gas to flow until there is about 50% volume reduction.

Once the organic components of the soil are extracted and concentrated, they can be analyzed by gas chromatography .

The atrazine concentration can be calculated using atrazine standard concentrations. In this case, the approximate atrazine concentration in the brownfield site studied was 2 mg of atrazine per 1 kg of soil.

Solid-liquid extraction is used in a wide range of fields.

This technique can be used to understand the transfer of polychlorinated biphenyls, or PCBs, from fish. PCBs are man-made chlorinated hydrocarbons that have been banned by the EPA. PCBs do not readily decompose in the environment and tend to accumulate in fish.

In this experiment, prey fish containing PCBs were fed to predator fish. The predator fish were then collected and sacrificed. The fish tissue was ground in preparation for extraction.

The PCB in the fish tissue was extracted to an organic phase using a Soxhlet extractor. The Soxhlet extractor setup, composed of a round-bottom flask, condenser, and the Soxhlet apparatus, is frequently used to extract solutes that are poorly soluble in solvents. The Soxhlet extraction enables a small amount of solvent to be used with a large solid sample. The extract was then tested for PCB content using mass spectrometry.

Dry plant matter, called lignocellulose, is the most abundant raw material being researched for bio-derived fuels. However, the carbohydrates used as the fuel are trapped within the rigid plant matrix, called lignin.

When the carbohydrates are removed, the lignin matrix is typically disposed of as waste. However, in this experiment, waste lignin was examined as a fuel source. Solid-liquid extraction was utilized to separate the carbohydrate components from lignocellulose, leaving lignin behind. The lignin was then used for further fermentation experiments.

Solid-liquid extraction can also be used to measure the wax content in fruit skins. In this experiment, the wax content of tomato skins was analyzed.

Exhaustive dewaxing of dried tomato skins was completed using a Sohxlet apparatus, in order to fully remove the wax content in the skins. Tomato skins with wax removed were then further analyzed using nuclear magnetic resonance spectroscopy. This helped elucidate the composition and degradation of native and engineered fruits.

You've just watched JoVE's introduction to solid-liquid extraction. You should now have a better understanding of the extraction of solutes between solid and liquid phases.

Thanks for watching!

A soil sample was collected from a Brownfield site similar to one in Sewickley Pennsylvania, as shown in Figure 1. Brownfields, as defined by the United States Environmental Protection Agency (U. S. EPA), are real property, where the expansion, redevelopment, or reuse may be complicated due to the potential presence of hazardous contaminants. The soil was collected from the Brownfield site using a soil sampler, as shown in Figure 2.

The pollutant of interest in this experiment was atrazine ( Figure 3 ); a common organochloride herbicide. Once the organic components of the soil were extracted and concentrated, they were analyzed by gas chromatography with a flame ionization detector (GC-FID). The GC analysis was carried out using a Shimadzu 14A GC (detector: FID) equipped with split/splitless injector and a CBP-10 capillary column (30 m × 0.22 mm i.d.). The column temperature was first set at 150 °C and then programmed from 150 to 230 °C at a rate of 5 °C per min. The injector temperature was 250 °C and the detector temperature was 260 °C. Injections were performed with splitless mode. Helium carrier gas was used at a constant flow rate of 1 mL/min. The atrazine concentration was calculated using atrazine standard concentrations, as shown in Figure 4 . In this case, the approximate atrazine concentration in the Brownfield site studied was 2 mg of atrazine per kg of soil.

The general solid-liquid extraction procedure is applicable to a range of fields from environmental monitoring (shown in this video) to cosmetics and food processing. The critical issue is to pick a solvent that effectively dissolves the analyte. With minimal changes in solvent, the sample preparation method in this video can be used to extract any of a broad range of semivolatile environmental contaminants that partition primarily on soils and sludges.

Examples of such semivolatiles include many harmful pollutants like pesticides, polycyclic aromatic hydrocarbons (PAHs), and polychlorinated biphenyls (PCBs). Because of the potential health effects of these molecules, identification and quantification of these species is of academic interest, and also widely practiced in the environmental consulting industry and in government agencies. The EPA maintains compendia of approved analytical and sampling methods to identify and quantify possible pollutants. The method shown in this video illustrates the basic principles contained in EPA method 3550C, which describes ultrasonic extraction of semivolatiles and nonvolatiles from solids. 1 EPA method 3550C is one of the extraction methods referenced in EPA method 8081B, which describes GC analysis of organochlorine pesticides. 2 Most of the EPA-approved method files are written with the assumption that the analyst has significant prior training. Thus, gaining familiarity with the basic characteristics of sample preparation aids in following the EPA methods.

The use of a Soxhlet apparatus can aid in the extraction of solutes that are poorly soluble in solvents. The setup consists of a round-bottom flask, a Soxhlet extractor, and a reflux condenser. This technique is demonstrated by the removal of PCBs from fish in order to examine the transfer of toxins between predator fish and prey fish. 3 Additionally, this technique can be used to measure the wax content in fruit skins in order to understand the composition and degradation of native and engineered fruits. 4 Finally, the extraction of carbohydrates from lignocellulose, or dry plant matter, can be accomplished using solid liquid extraction. 5 When the carbohydrates are extracted, lignin is left behind. Both components can then be used for biofuel applications.

Disclosures

No conflicts of interest declared.

• US Environmental Protection Agency. Ultrasonic Extraction, Method 3550C. Washington: Government Printing Office (2007).
• US Environmental Protection Agency. Organochlorine pesticides by gas chromatography, Method 8081B. Washington: Government Printing Office (2007).
• Madenjian, C. P., Rediske, R. R., O'Keefe, J. P., David, S. R. Laboratory Estimation of Net Trophic Transfer Efficiencies of PCB Congeners to Lake Trout ( Salvelinus namaycush ) from Its Prey.  J. Vis. Exp.  (90), e51496, (2014).
• Chatterjee, S., Sarkar, S., Oktawiec, J., Mao, Z., Niitsoo, O., Stark, R. E. Isolation and Biophysical Study of Fruit Cuticles.  J. Vis. Exp.  (61), e3529, (2012).
• Mathews, S. L., Ayoub, A. S., Pawlak, J., Grunden, A. M. Methods for Facilitating Microbial Growth on Pulp Mill Waste Streams and Characterization of the Biodegradation Potential of Cultured Microbes.  J. Vis. Exp.  (82), e51373, (2013).

The two phases also must be immiscible. Immiscible solutions never mix and remain as separate phases, like oil and water. Miscible solutions are completely homogeneous after mixing.

In liquid-liquid extraction, a solute is separated between two liquid phases, typically aqueous and organic. This is often performed in a separatory funnel fitted with a stopcock at the bottom and stopper at the top.

There are two resulting phases: the raffinate, containing the carrier liquid, and the extract, which contains the solute and the solvent. In reality, there is likely to be residue of each component in both phases. Solid-liquid extraction is similar to liquid-liquid extraction, except that the solute is dispersed in a solid matrix rather than in a carrier liquid. The solid phase, containing the solute, is dispersed in the solvent and mixed. The solute is extracted from the solid phase to the solvent, and the solid phase is then removed by filtration. Now that the principles of extraction have been outlined, the solid-liquid extraction technique will be demonstrated by performing the extraction in the laboratory.

In this experiment, soil samples were collected from a brownfield site, similar to this one in Sewickley, Pennsylvania. Brownfields, as defined by the U.S. EPA, are real property, where the expansion, redevelopment, or reuse may be complicated due to the potential presence of hazardous contaminants. The pollutant of interest in this case is an organochloride: the herbicide atrazine. Once a soil sample has been collected from the site of interest, transfer it into the laboratory.

Weigh out 10 g of the soil in a clean, dry, wide-mouth Pyrex dish. Put the dish into an oven to dry for at least 12 h. Once dry, grind the soil to a uniform powder with a mortar and pestle. Place 5 g of the ground soil into a clean, dry 100-mL round-bottom flask. Add 15 mL of hexane and loosely stopper the flask. Place it into an ultrasonic bath and sonicate for 60 min.

Prepare a Büchner funnel with analytical filter paper. Once sonication is complete, wet the paper with hexane and begin vacuum filtration. Slowly pour the sample over the filter paper. Rinse the residual solids from the flask with hexane and add it to the filter. The stripped soil remains on the filter, while the hexane and extracted organics collect in the flask.

Once the organic components of the soil are extracted and concentrated, they can be analyzed by gas chromatography.

This technique can be used to understand the transfer of polychlorinated biphenyls, or PCBs, from fish. PCBs are man-made chlorinated hydrocarbons that have been banned by the EPA. PCBs do not readily decompose in the environment and tend to accumulate in fish.

You've just watched JoVE's introduction to solid-liquid extraction. You should now have a better understanding of the extraction of solutes between solid and liquid phases.

JoVE Science Education Database. Organic Chemistry. Solid-Liquid Extraction. JoVE, Cambridge, MA, (2024).

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Principles of Extraction

Extraction and Separation of Organics from Soil

Pre-concentration and Analysis

Applications

Solid-Liquid Extraction

Source: Laboratory of Dr. Jay Deiner — City University of New York

Extraction is a crucial step in most chemical analyses. It entails removing the analyte from its sample matrix and passing it into the phase required for spectroscopic or chromatographic identification and quantification. When the sample is a solid and the required phase for analysis is a liquid, the process is called solid-liquid extraction. A simple and broadly applicable form of solid-liquid extraction entails combining the solid with a solvent in which the analyte is soluble. Through agitation, the analyte partitions into the liquid phase, which may then be separated from the solid through filtration. The choice of solvent must be made based on the solubility of the target analyte, and on the balance of cost, safety, and environmental concerns.

1. Extraction of Adsorbed Organics from Soil

• Place 20 g of soil in a clean, dry wide-mouth Pyrex dish in a 50 °C oven and dry for a minimum of 12 h. After drying, remove the soil from the Pyrex dish and grind to a uniform powder using a mortar and pestle. Weigh 5.00 g of the soil and place it into a clean, dry round-bottom flask (100 mL in size). To the flask, add 15 mL of n -hexane. Place flask in an ultrasonic bath, and sonicate for 60 min.

A soil sample was collected from a Brownfield site similar to one in Sewickley Pennsylvania, as shown in Figure 1. Brownfields, as defined by the United States Environmental Protection Agency (U. S. EPA), are real property, where the expansion, redevelopment, or reuse may be complicated due to the potential presence of hazardous contaminants. The soil was collected from the Brownfield site using a soil sampler, as shown in Figure 2.

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The general solid-liquid extraction procedure is applicable to a range of fields from environmental monitoring (shown in this video) to cosmetics and food processing. The critical issue is to pick a solvent that effectively dissolves the analyte. With minimal changes in solvent, the sample preparation method in this video can be used to extract any of a broad range of semivolatile environmental contaminants that partition primarily on soils and sludges.

• US Environmental Protection Agency. Ultrasonic Extraction, Method 3550C. Washington: Government Printing Office (2007).
• US Environmental Protection Agency. Organochlorine pesticides by gas chromatography, Method 8081B. Washington: Government Printing Office (2007).
• Madenjian, C. P., Rediske, R. R., O'Keefe, J. P., David, S. R. Laboratory Estimation of Net Trophic Transfer Efficiencies of PCB Congeners to Lake Trout ( Salvelinus namaycush ) from Its Prey.  J. Vis. Exp.  (90), e51496, (2014).
• Chatterjee, S., Sarkar, S., Oktawiec, J., Mao, Z., Niitsoo, O., Stark, R. E. Isolation and Biophysical Study of Fruit Cuticles.  J. Vis. Exp.  (61), e3529, (2012).
• Mathews, S. L., Ayoub, A. S., Pawlak, J., Grunden, A. M. Methods for Facilitating Microbial Growth on Pulp Mill Waste Streams and Characterization of the Biodegradation Potential of Cultured Microbes.  J. Vis. Exp.  (82), e51373, (2013).

Extraction is a crucial separation technique in organic chemistry, used to separate components of a mixture based on their solubilities in two different phases that do not mix.

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Solid-liquid extraction (Soxhlet)

What is solid-liquid extraction, functioning, references and notes, copy short link.

Solid Liquid Extraction (Leaching)

Ola Akinsunmade

Chemical Engineer

• June 3, 2022
• One Comment

Table of Contents

What is solid-liquid extraction.

Solid-Liquid Extraction (SLE), otherwise known as Leaching, is a solvent extraction separation technique which involves the  dissolution of a solute attached to an insoluble solid phase via an extraction solvent.

Leaching operations typically occur in the following three stages [1] :

• Dissolution of solute (soluble constituents)
• Separation of solution from solid residue
• Washing of solid residue

Just as is the case in Liquid-Liquid Extraction (LLE) , separation is driven mainly by solute solubility differences between the carrier and solvent phases whilst extraction is driven by phase immiscibility. It is commonly used in the extraction of oils from seeds and leaching of metal ores.

Factors Affecting Leaching Extraction Rate

Factors that impact the efficiency of a leaching process include:

• Particle size
• Temperature
• Particle size: Smaller particle size increases interfacial area resulting in a higher rate of mass transfer. Mass transfer is impeded in the leaching of very fine particles if some form of liquid agitation is not introduced due to high settling velocities. 
• Solvent: An ideal solvent will have a high saturation limit, high selectivity for the desired solute and a low viscosity to allow for free circulation.
• Temperature: In most cases, a higher extraction temperature increases the solute solubility in the solvent. 
• Agitation: As is in the case of LLE, agitation increases eddy diffusion and mass transfer across phases. Agitation is also vital in the leaching of fine particles, preventing sedimentation and creating an effective use of the interfacial area [1] . 

Solid-Liquid Extraction Equipment

Below are a few examples of equipment used industrially for solid-liquid extraction:

• Bollman-type Extractor
• Dorr Classifier
• Kennedy Extractor
• Bonotto Extractor
• De Smet Belt Extractor
• Rotocel Extractor
• Pachuca Tanks
• Continuously Stirred Tank Reactors (CSTR)

Equipment used in solid-liquid extraction is primarily dependent on the nature (granular or cellular) and texture (coarse or fine) of the solid phase in the process. The texture of the solid phase becomes a particularly important design consideration when selecting the ideal solvent contacting method.

Finer solid particles offer a higher resistance to solvent percolation due to their higher settling velocities. As a result, solid-liquid extraction is performed in a dispersed solids leaching system often requiring some form of agitation to prevent sedimentation.

In general, industrial leaching systems are distinguished and classified by the following operating design choices [2] :

• Operating Cycle (batch, continuous, multi batch)
• Direction of Streams (concurrent, countercurrent, hybrid)
• Staging (single-stage, multistage, differential stage)
• Contacting Method (sprayed percolation, immersed percolation, solids dispersion)

Here’s a video of rake classifier in operation:

Classifications of Common Leaching Equipment and Applications

Equilibrium in a Solid-Liquid Extraction

In a typical continuous single or multistage leaching process, the stream containing the solid phase is called the underflow whilst the solute-rich stream is referred to as the overflow stream . 

Equilibrium in a solid-liquid stream is established when the concentration of solute in the underflow and overflow streams leaving a stage are equal. 

This is with the assumption that the solute is not adsorbed to the leached solid and is completely dissolved and distributed in both streams.

V 1 = Overflow Solution Flow 

V 2 = Solvent Feed Flow

L 0 = Feed Solid/Slurry Flow

L 1 = Underflow Solution Flow

x A,1 = Solute Composition in Overflow

x A,0 = Solute Composition in Solvent Feed

y A,0 = Solute Composition in Feed Slurry

y A,1 = Solute Composition in Underflow

The equilibrium concentration of the solute in the overflow and underflow stream is represented on the x-y plot as a 45 degree line.

The equilibrium plot is typically represented by plotting the ratio of the entrained solids in a stream/solution (N) with respect to the solute and solvent mass versus the solute equilibrium concentration (x, y).

• D. G. Peacock and J. F. Richardson, “Leaching,” in Coulson & Richardson Chemical Engineering , Oxfors: Butterworth-Heinemann, 2012. 
• J. M. Coulson and J. F. Richardson, “Liquid Liquid Extraction,” in Particle Technology and separation processes , Oxford: Pergamon Press, 1998. 
• D. Michaud, “Rake classifier,” Mineral Processing & Metallurgy , 13-May-2021. [Online]. Available: https://www.911metallurgist.com/blog/rake-classifier. [Accessed: 04-May-2022]. 

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• • Aqueous extraction
• • Acidic extraction
• • Basic extraction
• 1. Weigh about 3 g of the unknown mixture and transfer to a clean, dry 125 mL Erlenmeyer flask. Dissolve in approximately 50 mL dichloromethane. Dichloromethane may be harmful if ingested, inhaled, or absorbed through the skin. Minimize contact with the liquid and handle it under the fume hood.
• 2. Prepare at least 100 mL of a saturated sodium bicarbonate solution (about 10% w/v). Add your solution from step 1 to a seperatory funnel and extract the aspirin in two 25 mL portions of NaHCO 3 . Your mentor will demonstrate the proper use of a seperatory funnel.  Collect the organic and aqueous layers in separate Erlenmeyer flasks. Why will aspirin be extracted into the aqueous layer?
• 3. Set your organic layer aside. Slowly add 6 M HCl to your aqueous layer while stirring until the pH is about 2. Cool the solution and filter off the solid by vacuum filtration. Wash your solid with cold distilled water and dry to constant mass. Take the melting point.
• 4. Dry your organic layer with sodium sulfate and gravity filter into a pre-weighed round-bottom flask. Evaporate the solvent using a rotovap and determine the mass of solid you obtain. Determine the melting point of your crude solid.
• 5. Dissolve your solid in a minimal amount of boiling water in an Erlenmeyer flask. Why is an Erlenmeyer flask ideal for recrystallizations?
• 6. If the solution is colored, add a small amount of activated carbon and gravity filter the hot solution into a second flask. Add additional hot solvent to your solution before filtering and use a funnel pre-heated with vapors from your boiling solvent to prevent recrystallization and loss of product.
• 7. Heat your solution until the solute is completely dissolved and then allow it to cool to room temperature. Cool for 10-15 minutes on an ice bath to complete the recrystallization and collect the crystals by vacuum filtration.
• 8. While your solution cools, convince yourself that water is an appropriate solvent for recrystallization by performing three solubility tests. Take about 10 mg of your crude unknown (the tip of a spatula) and place in a test tube with about 0.3 mL of either distilled water, hexanes, ethyl acetate, acetone, or ethanol. Observe the degree to which the solid dissolves at room temperature, at 0°C, and at the solvent’s boiling point.
• 9. After your recrystallized unknown is sufficiently dry, determine its melting point and identify it as either acetanilide or phenacetin. Confirm your results by grinding a 50/50 mixture of your unknown and a pure sample of the compound you suspect, and determine the melting point. How does this technique work to confirm your result?

Exploring Solid-Liquid Extraction: Examples and Applications

• Nuovæstrazione
• Ottobre 25, 2023

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Solid-liquid extraction is a widely used process in various industries, including food, pharmaceutical, and chemical manufacturing. It involves the separation of a solid compound or solute from a liquid solvent through the application of physical and chemical principles. This article delves into the basics of solid-liquid extraction, its role in different industries, the extraction process itself, challenges faced, and future advancements. Let’s dive in!

Understanding the Basics of Solid-Liquid Extraction

Solid-liquid extraction is a fundamental separation technique that relies on the differences in solubility between a solid and a liquid. The process involves bringing the solid material into contact with the liquid solvent, allowing the solute to dissolve and form a solution. The subsequent separation of the solute from the solvent is accomplished through various techniques, such as filtration or evaporation.

The Science Behind Solid-Liquid Extraction

At the core of solid-liquid extraction is the principle of dissolution. The solute particles are surrounded by the solvent molecules, which disrupt the attractive forces holding the solute particles together. This allows the solute to break down and disperse evenly throughout the solvent, resulting in a homogeneous solution.

The rate of dissolution depends on factors like temperature, agitation, and the size of the solid particles. Increasing the temperature or agitation speeds up the dissolution process by increasing the collision between the solid and liquid particles. The smaller the particle size, the larger the surface area available for contact, leading to faster dissolution.

Moreover, the solubility of a solute in a particular solvent is influenced by various factors, including the nature of the solute and solvent, as well as the presence of other substances. For example, the polarity of the solute and solvent can significantly affect their solubility. Polar solvents tend to dissolve polar solutes more readily, while nonpolar solvents favor nonpolar solutes.

Key Components of Solid-Liquid Extraction

In a typical solid-liquid extraction setup, several components play a crucial role. First and foremost is the solvent, which selectively dissolves the desired solute while leaving impurities behind. The choice of solvent depends on factors such as the solute’s solubility, toxicity, and environmental impact.

The solid material, often referred to as the feedstock, can be in the form of a powder, granules, or chunks. The physical characteristics of the solid, such as particle size and surface area, can significantly influence the extraction efficiency. Smaller particle sizes provide a larger surface area for contact with the solvent, promoting faster and more efficient extraction.

The extraction vessel, equipped with agitation mechanisms, facilitates the interaction between the solid and liquid phases. Agitation helps to maximize the contact between the solid and liquid, ensuring efficient mass transfer and enhancing the extraction process. Various agitation methods can be employed, including stirring, shaking, or using specialized equipment like ultrasonic baths.

Additionally, depending on the nature of the solute or desired product, auxiliary components such as pH adjusters, surfactants, or complexing agents may be added to enhance the extraction process or improve the selectivity. pH adjusters can be used to optimize the solubility of the solute, while surfactants can aid in the removal of impurities or enhance the solute’s solubility. Complexing agents are often employed to selectively extract specific components from the solid material.

Furthermore, the choice of extraction technique depends on the specific requirements of the process. Filtration is commonly used to separate the solid particles from the liquid after extraction. This can be achieved through various filtration methods, such as gravity filtration, vacuum filtration, or centrifugation. Evaporation is another technique employed to separate the solvent from the solute, typically by heating the solution to evaporate the solvent and leaving behind the solid residue.

In conclusion, solid-liquid extraction is a versatile separation technique that finds applications in various industries, including pharmaceuticals, food processing, and environmental analysis. Understanding the science behind this process and the key components involved is essential for optimizing extraction efficiency and obtaining high-quality products.

The Role of Solid-Liquid Extraction in Various Industries

Solid-liquid extraction finds wide applications in diverse industries, exploiting its ability to selectively extract valuable compounds from complex mixtures. Let’s explore the role of solid-liquid extraction in the food industry and pharmaceutical manufacturing.

Solid-Liquid Extraction in the Food Industry

The food industry extensively employs solid-liquid extraction to extract desired flavors, colors, and bioactive compounds from natural sources. Coffee production, for example, utilizes solid-liquid extraction to extract the flavorful compounds from roasted coffee beans. The process involves soaking the ground coffee beans in water, allowing the soluble compounds to dissolve and form a liquid extract. This extract is then concentrated and used to create various coffee products, such as instant coffee or coffee syrups.

Similarly, the extraction of vanilla from vanilla pods relies on solid-liquid extraction techniques. The pods are first crushed and mixed with a solvent, such as ethanol, which helps dissolve the aromatic compounds present in the pods. The mixture is then filtered to separate the liquid extract from the solid residue. The extract is further processed to obtain pure vanilla extract or vanilla flavoring used in a wide range of food products, including ice creams, cakes, and beverages.

Additionally, solid-liquid extraction is also employed in the production of essential oils, where aromatic compounds are extracted from plant materials using solvents. This process allows the food industry to incorporate natural flavors and aromas into various food products. For example, the extraction of citrus essential oils involves the use of solvents to separate the aromatic compounds from the citrus peels. The resulting essential oils are used to enhance the flavor of beverages, confectioneries, and baked goods.

Solid-Liquid Extraction in Pharmaceutical Manufacturing

In the pharmaceutical industry, solid-liquid extraction plays a vital role in the extraction of active pharmaceutical ingredients (APIs) from natural sources. Medicinal plants contain various bioactive compounds, and solid-liquid extraction helps isolate these compounds in high purity. The process begins with the selection and preparation of plant materials, which are then subjected to extraction using suitable solvents. The solvent selectively dissolves the desired compounds, leaving behind impurities and unwanted components. The resulting extract is then further processed to obtain the pure API, which serves as the basis for the development of drugs and nutritional supplements.

Furthermore, solid-liquid extraction is also used in pharmaceutical manufacturing for the purification of intermediates and the removal of impurities. After the initial synthesis of a drug molecule, there may be impurities or by-products present that need to be removed to ensure the production of safe and effective medications. Solid-liquid extraction techniques are employed to selectively extract the desired compound from the mixture, leaving behind the impurities. This purification process helps meet the stringent quality standards required in the pharmaceutical industry.

In conclusion, solid-liquid extraction plays a crucial role in both the food industry and pharmaceutical manufacturing. Its ability to selectively extract valuable compounds from complex mixtures enables the production of high-quality food products and pharmaceuticals. Whether it’s extracting flavors from coffee beans or isolating active pharmaceutical ingredients from medicinal plants, solid-liquid extraction continues to be a valuable technique in various industries.

The Process of Solid-Liquid Extraction

The process of solid-liquid extraction involves several stages, including preparation, extraction, and post-extraction processes. Let’s explore each step in detail.

Preparing for Extraction

Prior to extraction, it is crucial to prepare the solid material by grinding, sieving, or drying it to achieve a desired particle size and enhance the surface area for contact with the solvent. Additionally, certain pre-treatment steps like washing or leaching may be employed to remove unwanted impurities.

Performing the Extraction

During the extraction step, the solid material is introduced into an extraction vessel containing the liquid solvent. Agitation mechanisms, such as stirring or ultrasonication, are employed to ensure efficient contact between the solid and liquid phases. The extraction time and temperature are optimized to achieve maximum solute recovery and selectivity.

Once the desired extraction is complete, the mixture is typically subjected to a separation process, such as filtration or centrifugation, to separate the solid residue from the liquid solution.

Post-Extraction Processes

After the extraction, it is often necessary to further process the extracted solution to concentrate the desired solute or remove impurities. Techniques like evaporation, crystallization, or phase separation are employed for this purpose. The final product may undergo purification steps to meet the required specifications for its intended use.

Challenges and Solutions in Solid-Liquid Extraction

While solid-liquid extraction is a versatile technique, it is not without challenges. Let’s explore some common difficulties faced during the process and innovative solutions to overcome them.

Common Difficulties in Solid-Liquid Extraction

One of the primary challenges in solid-liquid extraction is achieving high extraction yields and minimizing solvent consumption. Factors like solute solubility, diffusion limitations, and mass transfer resistances can affect the extraction efficiency. In some cases, the presence of competing solutes or impurities may interfere with the extraction process, necessitating further purification steps.

Innovative Solutions for Solid-Liquid Extraction

To address these challenges, researchers are continually exploring innovative techniques and technologies. These include the use of novel solvents, such as supercritical fluids or deep eutectic solvents, which offer enhanced extraction efficiency and reduced environmental impact. Additionally, the development of advanced equipment, like continuous-flow extraction systems or membrane-based extraction, improves process control and scalability.

The Future of Solid-Liquid Extraction

The field of solid-liquid extraction is witnessing exciting advancements that hold promise for the future. Let’s explore two key aspects influencing the future of this technique.

Technological Advancements in Solid-Liquid Extraction

Ongoing advancements in extraction technology aim to enhance process efficiency, selectivity, and sustainability. The integration of automation and artificial intelligence enables real-time monitoring and optimization of extraction parameters. This leads to improved process control and reduced energy consumption, making the extraction process more economical and environmentally friendly.

Sustainability and Solid-Liquid Extraction

As the global focus on sustainability grows, solid-liquid extraction offers opportunities for resource recovery and waste valorization. By extracting valuable compounds from waste streams or industrial by-products, solid-liquid extraction can contribute to a circular economy and minimize environmental impact. Furthermore, the development of green solvents and eco-friendly extraction techniques helps reduce the ecological footprint of the extraction process.

In conclusion, solid-liquid extraction is a versatile separation technique with various applications across industries. Whether it’s extracting flavors from coffee or isolating active pharmaceutical ingredients from plants, solid-liquid extraction plays a crucial role in achieving desired products. With ongoing advancements and a focus on sustainability, the future of solid-liquid extraction looks promising, paving the way for innovative solutions and resource-efficient processes.

More To Explore

Naviglio extractor: applications in various industries.

Key Takeaways Information Details Topic Applications of Naviglio Extractor in Various Industries Industries Pharmaceutical, Food and Beverage, Cosmetics, and Environment Advantages Speed, Efficiency, Versatility Plant

Naviglio’s Principle: The Secret Behind Naviglio Extractor

Key Takeaways Information Summary What is Naviglio’s Principle? The foundation behind the Naviglio Extractor’s fast, dynamic solid-liquid extraction. How Does It Differ? Uses pressure changes

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Observing flows at a liquid-liquid-solid intersection

by Rachel Berkowitz, SciencePOD

Most of us are familiar with the classic example of a liquid-gas moving contact line on a solid surface: a raindrop, sheared by the wind, creeps along a glass windscreen. The contact line's movements depend on the interplay between viscous and surface tension forces—a relationship that has been thoroughly investigated in experimental fluid mechanics.

In a study published in The European Physical Journal Special Topics , Harish Dixit, of the Indian Institute of Technology Hyderabad, and his colleagues now examine the movements of a contact line formed at the interface between two immiscible liquids and a solid. The experiments fill a gap in fluid dynamics and suggest a mechanism for an imposed boundary condition that eludes mathematical description.

According to theory, the movement of a liquid-liquid contact line should be governed entirely by the liquids' viscosity ratio and the angle at which the liquid interface meets the solid. To examine this in a real-world system, Dixit and his colleagues filled a rectangular tank with two liquid layers—silicone oil atop sugar water—with similar densities but significantly different viscosities. The researchers placed a glass slide at the edge of the tank, which they could slide vertically to create a moving contact line.

Using a technique that tracks tiny particles introduced to the liquids and illuminated with laser light , the researchers simultaneously mapped the flow field on both sides of the liquid-liquid interface while they moved the glass slide. They found that the flow velocities rapidly decreased close to the contact line. Additionally, the liquid interface appeared to slip along the moving glass slide, rather than staying pinned to it—resolving the apparent "singularity" in models that impose a no-slip boundary condition on the moving wall.

The findings lend support to theoretical models of contact line dynamics, and offer parameters that could improve numerical simulations which are based on similar-viscosity liquids.

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Experimental study and analysis on wear characteristics of mining pumps transporting solid-liquid two-phase flows, share and cite.

Hong, S.; Hu, X. Experimental Study and Analysis on Wear Characteristics of Mining Pumps Transporting Solid-Liquid Two-Phase Flows. Appl. Sci. 2024 , 14 , 5634. https://doi.org/10.3390/app14135634

Hong S, Hu X. Experimental Study and Analysis on Wear Characteristics of Mining Pumps Transporting Solid-Liquid Two-Phase Flows. Applied Sciences . 2024; 14(13):5634. https://doi.org/10.3390/app14135634

Hong, Shunjun, and Xiaozhou Hu. 2024. "Experimental Study and Analysis on Wear Characteristics of Mining Pumps Transporting Solid-Liquid Two-Phase Flows" Applied Sciences 14, no. 13: 5634. https://doi.org/10.3390/app14135634

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