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Soxhlet Extraction.pptx

Dev Verma
20. Mar 2023
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Soxhlet Extraction.pptx

  1. Soxhlet Apparatus PRESENTED BY: LAXMI BHAGAT ROLL NO. 19HPH036 VIITH SEMESTER B. PHARMA.
  2. Table of Contents  Introduction  Apparatus  Working Principle  Sample Preparation  SOP  Advantages of Soxhlet extraction  Disadvantages of Soxhlet extraction  Automated Soxhlet Extraction  Comparison of different Soxhlet extraction modifications  Modern Day Applications
  3. Introduction  Extraction is a process in which a substance is removed from a solid, a liquid or a gas using an extractant. The extraction material is the material from which the substance is to be removed. At the end of the extraction, we get the desired substance and the raffinate from which the substance was removed.  The extractant cannot be any arbitrary solvent. It should only remove the desired material in significant amount from the extraction material and must not chemically react with other materials contained in the extraction material. So The polarity of the solvent should be similar to that of the target analytes. This condition provides sufficient contact with analytes, which governs extraction recovery.  Extraction is often used as a purification method when distillation or rectification cannot be performed.  Soxhlet extraction process is also an extraction process that can remove sparingly soluble substances from solids by means of a solvent. Originally, this method was introduced by Franz von Soxhlet in 1879 for determining the fat content in foods.
  4. Parts of Apparatus 1. Stirrer bar 2. Still pot 3. Distillation path 4. Thimble 5. Solid 6. Siphon top 7. Siphon exit 8. Expansion adapter 9. Condenser 10. Cooling water in 11. Cooling water out
  5. Working Principle  In this method the solvent is placed in a flask and is heated to boiling point. Then, solvent vapours rise in the entire apparatus and condense at a coil condenser. From here, the solvent drips onto a cellulose extraction thimble that sits in the Soxhlet extractor and which is filled with the extraction material. The extractant thus drips directly onto the extraction material and collects in the Soxhlet extractor.  When a critical liquid level is reached, the Soxhlet extractor abruptly drains into the flask. This process is also called siphoning and is driven by way of a suction lifting effect. In the flask, the solvent has now been distilled from the extract and can thus remove new extract from the extraction material.
  6. Sample Preparation
  7. Standard Operating Procedures (SOP)  The drug to be extracted is packed in a paper cylinder made from a filter paper and it is placed in the body of soxhlet extractor.  The solvent is placed in the flask and the apparatus is fitted.  A condenser unit is attached with the extraction tube.  The flask containing solvent is heated and it starts to evaporate  These vapour enters into the condenser through side tube to get condensed into a hot liquid which falls on the column of the drug.  When extractor gets filled with solvent, the level of syphon tube also raises upto its top. The solvent containing active constituent of the drug in the syphon tube, syphon over flow and run into the flask, thus emptying the body of the extractor.  The soluble active constituent of the drug remain in the flask while the solvent is repeatedly volatilised.This process of filling and emptying of extractor is repeated until the drug is exhausted , almost for 15 times for complete exhaustion of drug.  Discontinue the process and clean the extraction tube and thimble.
  8. Advantages of Soxhlet extraction: Conventional Soxhlet extraction has some very important advantages:  the transfer equilibrium is readily displaced because of the repeated contact between the sample and fresh portions of solvent.  the heating of the distillation flask provides a relatively high temperature during the whole extraction process.  the methodology is simple – very little specialized training is required.  no filtration is required after leaching.  the apparatus is simple and inexpensive.  simultaneous extraction in parallel is possible, sample throughput can be increased.  extraction of analytes can be performed from a larger sample mass in comparison with the other techniques for extraction of solid samples.  a wide range of compounds can be extracted from different solid matrices.  many current official analytical methods are based on this standard technique.
  9. Disadvantages of Soxhlet extraction: However, Soxhlet extraction also has some significant drawbacks:  the extraction time is long (up to 48 hours).  large amounts of solvent are used, so there is the problem of proper waste disposal.  analytes may decompose thermally during the long extraction process.  an evaporation/concentration step is required after extraction.  selectivity of extraction is limited to solvent selectivity. Despite these many disadvantages, however, Soxhlet extraction is still a benchmark technique with which the performance of other leaching techniques is compared. That is why much effort has been expended to overcome these difficulties.
  10. Automated Soxhlet Extraction - the Randall Approach • In the early 1970s, Randall developed an accelerated extraction technique, sometimes called the submersion technique, which was a milestone in this field. Randall’s approach has led to a significant reduction in leaching time. Moreover, it is fully compatible with classical Soxhlet extraction, and precision is much better in comparison with the traditional approach. • Unlike classical Soxhlet extraction, the sample is totally immersed in boiling solvent. This simple modification provided the opportunity to shorten the extraction time, because analytes are more soluble in hot solvent than in the cold-to-warm (not boiling) solvent used in the classical Soxhlet method. • Randall’s procedure consists of three stages: boiling, rinsing and evaporation/solvent recovery Diagram of the Randall extractor (left) compared with the conventional Soxhlet extractor (right).
  11. Stages of Randall’s procedure:
  12. Comparison of different Soxhlet extraction modifications
  13. Comparison of different Soxhlet extraction modifications
  14. Applications: The main applications concerning the extraction of soluble matter from different kinds of samples by means of automated systems are: Food Products: • cereals and cereal products; • milk and dairy products; • meat products; • chocolate and cocoa products; • oil and oilseed products; • fruit; • fat in food; • lipids in eggs and egg products; Chemical Industries: • pesticides, phenols, PCBs, dioxins, PAHs, EOXs; • coating of fertilizers, • explosives; • colorants on textile fibers; • paper pulp; • softeners and additives in plastics and rubbers; • polymers Pharmaceutics:
  15. Thank You
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