서울여자대학교 유기화학실험 Recrystallization & melting point 결과 레포트

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1. Melting point

순수한 물질의 melting point 와 freezing point 는 통상 1 atm 에서 액상과 고체상이 equilibrium 에 있게 되는 온도를 말한다. 녹는 물질이 순수한 물질이라면 그 물질이 녹는 동안 가열해도 온도가 일정하게 유지되는 일정 온도 구간이 나타난다. 녹는점의 범위는 sample 이 녹기 시작할 때부터 완전히 녹았을 때까지 이고 melting point 는 이 범위 중 최고의 온도이다. Melting point 는 물질 마다 다르기 때문에 그 물질만이 가지는 고유한 물질의 특성이 된다.
2. Solubility

용해도란 특정 온도에서 용매에 녹을 수 있는 용질의 최대량이다.(용해열은 용질이 용매에 녹을 때 방출 혹은 흡수하는 열량) 고체의 경우 온도가 올라갈수록 용해도도 커진다. 이때, 포화 용액은 주어진 온도에서 주어진 용매 내에 최대의 용질이 포함되어 있는 용액이며, 포화 용액에 존재하는 용질보다 더 많은 양의 용질이 있으면 과포화 용액이고, 이 불안정한 과포화 용액이 시간이 지나 일부 용질이 용액으로부터 빠져나와 결정을 형성하는 과정을 crystallization이라고 한다.
3. Recrystallization

재결정이란 solid product는 crystal을 형성하고 impurity는 재결정 solvent에 녹는 성질을 이용하여 고체 compound를 purification하기 위해 사용하는 방법이다. 이는 고체를 용해시키는 경우에는 solvent가 cold할 때보다 hot한 상태일 때, 즉 온도가 더 높을 때에 용해를 더 잘하는 경향을 가진다는 용해의 원리를 따른다.
4. Solvent selection

Solvent를 선택할 때에는 Solute의 impurity에 대한 temperature coefficient가 맞는 것, Solvent의 boiling point가 100℃ 이하인 것, Solute의 melting point보다 solvent의 boiling point가 낮은 것, Solvent와 정제하고자 하는 물질이 chemically inert한 것, 경제성과 handling이 간편한 것 등을 고려해야 한다.
5. Drying

순수한 유기물을 얻어 characterization하려면 건조하여 수분을 제거해야 한다. 과거에는 vacuum oven에서 beaker와 watchglass를 사용하여 건조시켰으나 이제는 round bottom flask에서 vacuum line을 연결해서 heating하여 수분을 제거한다.
6. Single crystal

Single crystal은 일정 격자 구조가 반복되어 잘 packing이 되므로 impurity가 끼어들 수 없다. 이때 결정은 bp에서 포화되었다 하더라도 실온에서 역시 일정량의 용해도가 있기 때문에 50~60%가 석출되게 되므로 2차, 3차 재결정으로 수득률(yield)을 높일 수 있다.
7. Crystal formation

결정 형성속도가 매우 느리다면 용기 벽면에 scratching을 해준다. Crystal의 생성속도는 final product의 purity를 결정짓는데 중요한 역할을 가진다. 너무 빨리 solvent를 식혀주거나 너무 많은 양의 nonpolar solvent를 polar solvent에 넣어주게 되면 소량의 impurity가 섞여서 나올 수가 있다.
8. Filtration

유기 용매에 있는 불순물을 제거하거나 유기 solid를 따로 분리해내고 싶을 때, 여과를 이용한다. 천천히 대기압 하에서 여과하는 gravity filtration과 vacuum filtration이 있다.
9. Yield

시약의 양은 반응이 완료된 후 얻을 수 있는 생성물의 양, 즉 이론적 수득량을 결정한다. 그러나 실제 반응을 통해서 얻은 생성물의 양, 즉 실제 수득량은 가역적인 반응이어서, 혹은 실험 오차에 의해, 혹은 부반응에 의해 이론적 수득량보다 작을 수밖에 없다.
10. Melting point measurement

Melting point 측정기의 전원을 켜고 plateau를 100 ℃까지 설정하고 slope를 5.0 ℃/min으로 맞춘다. 한 쪽이 막혀 있는 Capillary tube에 시료를 5 mm 높이까지 채워준 후 측정기에 넣어 온도를 올리면서 녹기 시작하는 시초점과 완전히 녹는 종말점을 확인한다.

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1. Melting point

The melting point is a crucial physical property that provides valuable information about the nature and composition of a substance. It represents the temperature at which the solid and liquid phases of a material coexist in equilibrium. Understanding and accurately determining the melting point is essential in various fields, such as chemistry, materials science, and pharmaceutical development. Accurate melting point measurements can help identify and characterize unknown compounds, monitor the purity of substances, and optimize processing conditions. Additionally, the melting point can provide insights into the intermolecular forces and crystal structure of a material, which are fundamental to understanding its behavior and potential applications. Precise melting point determination is particularly important in the pharmaceutical industry, where it is used to assess the quality and stability of drug substances and formulations. Overall, the melting point is a versatile and indispensable property that plays a vital role in the characterization, identification, and optimization of a wide range of materials and compounds.
2. Solubility

Solubility is a fundamental property that describes the ability of a substance to dissolve in a given solvent, forming a homogeneous solution. Understanding and controlling solubility is crucial in numerous scientific and industrial applications, ranging from chemical synthesis and purification to drug formulation and environmental remediation. The solubility of a compound is influenced by various factors, such as temperature, pressure, and the nature of the solvent and solute. Accurately determining the solubility of a substance is essential for optimizing reaction conditions, improving separation and purification processes, and developing effective drug delivery systems. In the pharmaceutical industry, solubility plays a critical role in the development of new drug candidates, as poor solubility can significantly limit their bioavailability and therapeutic efficacy. Solubility data also informs the selection of appropriate solvents and excipients for formulations, ensuring the stability and efficacy of the final product. Beyond pharmaceuticals, solubility principles are applied in fields like materials science, environmental chemistry, and food processing, where they guide the design of novel materials, the remediation of pollutants, and the development of functional food ingredients. Overall, the understanding and control of solubility is a fundamental aspect of chemistry and engineering, with far-reaching implications across diverse scientific and technological domains.
3. Recrystallization

Recrystallization is a powerful purification technique that is widely used in various fields, including organic chemistry, pharmaceutical sciences, and materials science. This process involves the controlled dissolution and subsequent crystallization of a solid substance, often with the aim of improving its purity, particle size, and morphology. By carefully manipulating the recrystallization conditions, such as solvent selection, temperature, and cooling rate, it is possible to selectively remove impurities and obtain a more homogeneous and well-defined crystalline product. Recrystallization is particularly valuable in the pharmaceutical industry, where it is employed to purify active pharmaceutical ingredients (APIs) and ensure their quality, stability, and bioavailability. In materials science, recrystallization is used to tailor the microstructure and properties of metals, ceramics, and other functional materials, enabling the optimization of their performance for specific applications. Additionally, recrystallization principles are applied in the synthesis and purification of organic compounds, inorganic salts, and other chemical substances, where the ability to control crystal size, shape, and purity is crucial. Overall, recrystallization is a versatile and indispensable tool in the arsenal of chemists, materials scientists, and engineers, allowing them to refine and enhance the properties of a wide range of materials and compounds.
4. Solvent selection

Solvent selection is a critical aspect of many chemical and pharmaceutical processes, as the choice of solvent can have a profound impact on the efficiency, safety, and environmental impact of these operations. Selecting the appropriate solvent involves carefully considering a range of factors, including the solubility of the target compound, the polarity and reactivity of the solvent, its boiling point and ease of removal, as well as its toxicity and environmental impact. In organic synthesis, the choice of solvent can influence the reaction kinetics, the selectivity of the transformation, and the ease of product isolation and purification. In the pharmaceutical industry, solvent selection is particularly important in the development of drug formulations, where the solvent must not only solubilize the active pharmaceutical ingredient (API) but also ensure the stability, bioavailability, and safety of the final product. Beyond these applications, solvent selection is also crucial in areas such as materials science, where the choice of solvent can affect the morphology and properties of the synthesized materials, and in environmental remediation, where the selection of appropriate solvents is essential for the effective extraction and separation of contaminants. As sustainability and environmental concerns become increasingly important, the development of greener, more environmentally friendly solvents and solvent selection strategies has become a growing area of research and innovation. Overall, the careful and informed selection of solvents is a fundamental aspect of many scientific and industrial processes, with far-reaching implications for efficiency, safety, and environmental stewardship.
5. Drying

Drying is a crucial process in various scientific and industrial applications, ranging from the production of pharmaceuticals and chemicals to the processing of food and materials. The primary goal of drying is to remove unwanted moisture or solvents from a substance, thereby improving its stability, purity, and handling characteristics. Effective drying techniques are essential in the pharmaceutical industry, where they are used to dry active pharmaceutical ingredients (APIs), excipients, and final drug formulations, ensuring their quality, stability, and bioavailability. In materials science, drying plays a vital role in the synthesis and processing of a wide range of materials, such as ceramics, polymers, and composites, where it can influence their microstructure, mechanical properties, and performance. In the food industry, drying is employed to preserve and extend the shelf life of various food products, while in environmental remediation, it is used to remove contaminants and prepare samples for further analysis. The selection of the appropriate drying method, whether it be evaporation, lyophilization, spray drying, or other techniques, depends on the specific properties of the material, the desired final product characteristics, and the overall process requirements. Advances in drying technologies, such as the development of energy-efficient and environmentally friendly drying systems, have further expanded the applications and importance of this fundamental process in the scientific and industrial realms. Overall, drying is a versatile and indispensable tool that enables the effective processing, preservation, and transformation of a wide range of materials and substances.
6. Single crystal

Single crystals are highly ordered, defect-free crystalline materials that possess unique and valuable properties, making them essential in a wide range of scientific and technological applications. The growth and characterization of single crystals is a critical area of research and development, as these materials exhibit superior physical, chemical, and optical properties compared to their polycrystalline or amorphous counterparts. In the field of materials science, single crystals are used in the fabrication of high-performance electronic and optoelectronic devices, such as semiconductors, lasers, and sensors, where their exceptional structural and electronic properties are crucial. In the pharmaceutical industry, the growth and analysis of single crystals of active pharmaceutical ingredients (APIs) and their polymorphs is essential for understanding and controlling the stability, solubility, and bioavailability of drug substances. Single crystals also play a vital role in the field of structural biology, where they are used to determine the three-dimensional structures of proteins, enzymes, and other biomolecules, providing invaluable insights into their function and potential therapeutic applications. Furthermore, single crystals are employed in the development of advanced materials for energy storage, catalysis, and other emerging technologies, where their unique properties can be leveraged to enhance performance and efficiency. The growth and characterization of high-quality single crystals remains a challenging and active area of research, as scientists and engineers continue to push the boundaries of materials science and engineering to develop innovative solutions to complex problems.
7. Crystal formation

Crystal formation is a fundamental process that underpins a wide range of scientific and technological applications, from the development of new materials to the production of pharmaceuticals and the understanding of natural phenomena. The formation of crystals, whether in a laboratory setting or in the natural world, is a complex and fascinating process that involves the ordered arrangement of atoms, molecules, or ions into a highly structured, three-dimensional lattice. Understanding the factors that govern crystal formation, such as supersaturation, temperature, pressure, and the presence of impurities or additives, is crucial for controlling and optimizing the properties of the resulting crystals. In the field of materials science, the ability to precisely control crystal formation is essential for the development of advanced functional materials, such as semiconductors, superconductors, and optical materials, whose performance is heavily dependent on their crystalline structure. In the pharmaceutical industry, the formation and characterization of drug crystals is a critical aspect of drug development, as the crystal form can significantly impact the solubility, stability, and bioavailability of the active pharmaceutical ingredient. Beyond these applications, the study of crystal formation has also provided valuable insights into the formation of minerals, the growth of biological structures, and the behavior of complex fluids and gels. As our understanding of the underlying principles of crystal formation continues to evolve, researchers and engineers are poised to unlock new possibilities in materials design, drug development, and the exploration of natural phenomena, ultimately driving innovation and progress across a wide range of scientific and technological domains.
8. Filtration

Filtration is a fundamental separation technique that is widely used in various scientific and industrial applications, from the purification of pharmaceuticals and chemicals to the treatment of water and wastewater. The process of filtration involves the selective removal of solid particles, suspended matter, or other unwanted components from a fluid stream, allowing the desired components to pass through a porous medium or membrane. Effective filtration is crucial in ensuring the quality, purity, and safety of a wide range of products and processes. In the pharmaceutical industry, filtration is employed at multiple stages of drug development and manufacturing, from the purification of active pharmaceutical ingredients (APIs) to the sterilization of final drug formulations. In the chemical industry, filtration is used to separate reaction products, remove catalysts, and purify intermediates and final products. In the environmental sector, filtration plays a vital role in water treatment, wastewater management, and the removal of contaminants from air and soil. The selection of the appropriate filtration technology, such as membrane filtration, centrifugal separation, or adsorption-based methods, depends on the specific characteristics of the feed stream, the target contaminants, and the desired level of purity or separation efficiency. Advances in filtration materials, membrane technologies, and process optimization have continuously expanded the capabilities and applications of this essential separation technique. As sustainability and environmental concerns become increasingly important, the development of more efficient, energy-saving, and environmentally friendly filtration technologies has become a growing area of research and innovation.
9. Yield

Yield is a critical metric in various scientific and industrial processes, as it directly reflects the efficiency and productivity of these operations. In the context of chemical reactions, yield refers to the amount of the desired product obtained relative to the theoretical maximum amount that could be produced. In other applications, such as pharmaceutical manufacturing or materials processing, yield may be defined as the ratio of the usable or marketable product to the total input or raw materials. Maximizing yield is a fundamental goal in many scientific and industrial endeavors, as it directly impacts the economic viability, resource utilization, and environmental impact of these processes. In the chemical and pharmaceutical industries, optimizing yield is essential for ensuring the cost-effectiveness and scalability of production processes. High yields translate to more efficient use of raw materials, reduced waste, and lower energy consumption, all of which contribute to the overall sustainability and profitability of the operation. In materials science and engineering, yield considerations are crucial in the development and manufacturing of advanced materials, where the efficient utilization of scarce or expensive precursors is paramount. Beyond the economic and environmental benefits, high yields also contribute to the quality and consistency of the final products. In the pharmaceutical industry, for example, maintaining a consistent and reliable yield of active pharmaceutical ingredients (APIs) is crucial for ensuring the safety, efficacy, and regulatory compliance of drug formulations. Achieving high yields often requires a deep understanding of the underlying chemical, physical, and biological processes involved, as well as the ability to optimize process parameters, control impurities, and implement effective purification and recovery strategies. Advances in analytical techniques, process modeling, and automation have enabled researchers and engineers to continuously improve yield and enhance the overall efficiency and sustainability of a wide range of scientific and industrial operations.
10. Melting point measurement

Accurate melting point measurement is a critical analytical technique that provides valuable information about the purity, identity, and physical properties of a wide range of materials, from organic compounds and pharmaceuticals to inorganic salts and polymers. The melting point, defined as the temperature at which the solid and liquid phases of a substance coexist in equilibrium, is a fundamental characteristic that can reveal insights into the molecular structure, intermolecular interactions, and thermal stability of a material. Precise melting point determination is particularly important in the pharmaceutical industry, where it is used to assess the quality and stability of active pharmaceutical ingredients (APIs) and drug formulations. Deviations from the expected melting point can indicate the presence of impurities, polymorphic changes, or other issues that may affect the drug's efficacy and safety. In organic synthesis, melting point measurements are routinely used to monitor the progress of reactions, identify the purity of products, and characterize unknown compounds. Beyond pharmaceuticals and organic chemistry, melting point determination is also crucial in materials science, where it provides insights into the thermal behavior and phase transitions of a wide range of materials, including metals, ceramics, and polymers. This information is essential for understanding and optimizing the processing, performance, and applications of these materials. Advances in melting point measurement techniques, such as the development of automated and high-throughput instrumentation, have significantly improved the accuracy, precision, and efficiency of this analytical method. Furthermore, the integration of melting point data with other analytical techniques, such as spectroscopy, X-ray diffraction, and thermal analysis, has enabled researchers and engineers to gain a more comprehensive understanding of the physical and chemical properties of materials, ultimately driving innovation and progress across diverse scientific and technological domains.
11. Yield

Yield is a critical metric in various scientific and industrial processes, as it directly reflects the efficiency and productivity of these operations. In the context of chemical reactions, yield refers to the amount of the desired product obtained relative to the theoretical maximum amount that could be produced. In other applications, such as pharmaceutical manufacturing or materials processing, yield may be defined as the ratio of the usable or marketable product to the total input or raw materials. Maximizing yield is a fundamental goal in many scientific and industrial endeavors, as it directly impacts the economic viability, resource utilization, and environmental impact of these processes. In the chemical and pharmaceutical industries, optimizing yield is essential for ensuring the cost-effectiveness and scalability of production processes. High yields translate to more efficient use of raw materials, reduced waste, and lower energy consumption, all of which contribute to the overall sustainability and profitability of the operation. In materials science and engineering, yield considerations are crucial in the development and manufacturing of advanced materials, where the efficient utilization of scarce or expensive precursors is paramount. Beyond the economic and environmental benefits, high yields also contribute to the quality and consistency of the final products. In the pharmaceutical industry, for example, maintaining a consistent and reliable yield of active pharmaceutical ingredients (APIs) is crucial for ensuring the safety, efficacy, and regulatory compliance of drug formulations. Achieving high yields often requires a deep understanding of the underlying chemical, physical, and biological processes involved, as well as the ability to optimize process parameters, control impurities, and implement effective purification and recovery strategies. Advances in analytical techniques, process modeling, and automation have enabled researchers and engineers to continuously improve yield and enhance the overall efficiency and sustainability of a wide range of scientific and industrial operations.

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서울여자대학교 유기화학실험 결과 레포트 3. recrystallization and melting point 재결정과 녹는점 14페이지

1. Subject : Recrystallization and Melting Point Analysis 2. Principle Recrystallization은 고체 유기 화합물을 purifying하는 technique 중 하나로, solubility 차이를 이용한다. Impurity(불순물)가 포함된 solid compound를 적절한 solvent에 녹인 후, 용액의 온도를 변화시켜 pure crystal compound를 얻는 과정이다. 뜨거워진 saturated solution을 cooling시키면 차가워진 solvent...

2025.07.05· 14페이지