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Filtration, evaporation, chromatography, recrystallisation
Typology: Lab Reports
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Glaxo comp the s a lea infect nervo
The comm qualit to live
World manu Curra the a facilit in de chem
The C site w autom with P
We a GSK’ Type Canc
Glaxo Dung Dubli
tapped sharply against the desk causing the crystals to fall to the sealed end. When about 3 mm of crystals are in the base of the tube it is placed in the oil bath. The temperature at which the sample begins to melt and the temperature at which it is completely melted are recorded.
To double check your result, mix a sample of benzoic acid with some pure benzoic acid. If both are pure benzoic acid the melting point will remain the same but if the sample is not pure benzoic acid then the melting point will be lowered.
The melting point of a substance is not the exact point at which it melts but rather the range of temperatures from when the samples starts to melt until it has completely melted. The greater the range the more impurities present. A range of less than 1 °C indicates a pure substance.
The use of crystallisation in the pharmaceutical industry is an important process for controlling the physical properties, yield and purity of an Active Pharmaceutical Ingredient (API). Many production processes use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape, to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs of the same substance, but only one will be suitable for drug development and manufacture.
In industry, the way an API is filtered and dried can have a very significant impact on the physical properties of the material.
After the crystallisation process the amount of sample will have been reduced as impurities have been removed. To calculate how much of the pure substance was present in the initial impure sample, the percentage yield is calculated.
Mass of pure sample (after recrystallisation) Mass of impure sample (before recrystallisation)
The percentage yield is a good indicator of the purity of the initial sample. A high percentage yield implies a low concentration of impurities, whereas a low percentage yield indicates a sample with a lot of impurities.
Recrystallisation is a very important purification technique, purifying substances by removing unwanted by-products. It is also used to manufacture the correct crystal size and shape of a material. These factors can have a very significant impact on how a medicine acts when taken by a patient. The same principles and techniques of recrystallisation can be applied both on a laboratory and industry scale.
The process depends on two principles; the fact that substances tend to be more soluble in a hot solvent than in cold solvent, and that each solute tends to behave as though it were alone in the solvent.
Using the correct solvent is a very important part of the process. The solute must be insoluble in the solvent at room temperature, and as the temperature of the solvent increases, the solubility of the solute also increases. It is also important that the impurities present are soluble in the solvent at room temperature and insoluble at higher temperatures.
An excellent substance for showing this process is benzoic acid (C 6 H 5 COOH). A molecular crystal rather than an ionic crystal, shown by its low melting point of 122 °C, benzoic acid is used as an anti- microbial agent and is found in toothpastes, mouthwashes, cosmetics and deodorants.
Impure benzoic acid contains the impurities phthalic acid and benzylbenzoate. If the impure sample is dissolved in a minimal volume of hot solvent – in this case boiling water – and filtered to remove insoluble impurities, the resulting solution will contain dissolved benzoic acid as well as dissolved impurities.
Upon cooling, the benzoic acid crystals comes out of solution as its solubiluty in the solvent decreases. The impurities will remain in solution and can be filtered off.
It is very important when carrying out this experiment that rubber gloves are worn, because organic substances can be absorbed through the skin, and as well, goggles should be worn to protect your eyes from hot liquids which may spray out from the flask.
to be created. It is possible to produce crystals of varying particle size, polymorphs suitable for drug development and manufacture.
to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs suitable for drug development and manufacture.
targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape,
use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
A pure substance has a fixed melting point while an impure substance melts over a wide range of temperatures and at a lower temperature than the pure substance. The melting points of almost all substances are available in tables.
To check the melting point place a few crystals of the sample on an aluminium block which has a thermometer inserted. Use a hot plate to heat the block slowly. Watch the crystals carefully and note the temperature at which they begin to melt and the temperature at which they have all melted. Compare this value with the value found on the bottle of pure substance. Another method of checking the melting point of crystals is to use a narrow capillary tube in an oil bath. The capillary tube has one end open and the other end sealed. The open end is pressed into fine crystals of the substance and the turned upside down and
Beaker containing benzoic acid dissolved in minimum amount of boiling water
Filter funnel with fluted filter paper to speed up the filtrarion process. Insoluble impurities left behind as residue
Conical flask with hot concentrated benzoic acid solution which still contains soluble impurities
Fig.1 Filtration to remove insoluble impurities
Pure benzoic acid cystals
Büchner funnel
Büchner flask
Water containing soluble impurities
Fig.2 After cooling, the remaining solution is filtered off
Thermometer
Benzoic acid crystals
Aluminium block
Bunsen burner
Fig.1 Finding the melting point of benzoic acid
Percentage yield = x 100
6
5
Fig.1 Filtration to remove insoluble impurities
Pure benzoic acid cystals
Büchner funnel
Büchner flask
Water containing soluble impurities
Fig.2 After cooling, the remaining solution is filtered off
Glaxo comp the s a lea infect nervo The comm qualit to live World manu Curra the a facilit in de chem The C site w autom with P We a GSK’ Type Canc Glaxo Dung Dubli
of its
tapped sharply against the desk causing the crystals to fall to the sealed end. When about 3 mm of crystals are in the base of the tube it is placed in the oil bath. The temperature at which the sample begins to melt and the temperature at which it is completely melted are recorded. To double check your result, mix a sample of benzoic acid with some pure benzoic acid. If both are pure benzoic acid the melting point will remain the same but if the sample is not pure benzoic acid then the melting point will be lowered.
The melting point of a substance is not the exact point at which it melts but rather the range of temperatures from when the samples starts to melt until it has completely melted. The greater the range the more impurities present. A range of less than 1 °C indicates a pure substance.
The use of crystallisation in the pharmaceutical industry is an important process for controlling the physical properties, yield and purity of an Active Pharmaceutical Ingredient (API). Many production processes use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape, to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs of the same substance, but only one will be suitable for drug development and manufacture. In industry, the way an API is filtered and dried can have a very significant impact on the physical properties of the material.
After the crystallisation process the amount of sample will have been reduced as impurities have been removed. To calculate how much of the pure substance was present in the initial impure sample, the percentage yield is calculated. Mass of pure sample (after recrystallisation) Mass of impure sample (before recrystallisation) The percentage yield is a good indicator of the purity of the initial sample. A high percentage yield implies a low concentration of impurities, whereas a low percentage yield indicates a sample with a lot of impurities.
especially in the pharmaceutical industry. Separating insoluble solids from solvents is easily achieved using a simple technique called filtration. Soluble solids again are easily separated from solvents by evaporation , and chromatography is used to separate a mixture of liquids. But what happens when we have two soluble solids that we want to separate? In this lesson we will look at recrystallisation , a commonly-used process in the pharmaceutical industry.
Recrystallisation is a very important purification technique, purifying substances by removing unwanted by-products. It is also used to manufacture the correct crystal size and shape of a material. These factors can have a very significant impact on how a medicine acts when taken by a patient. The same principles and techniques of recrystallisation can be applied both on a laboratory and industry scale.
recrystallisation?
The process depends on two principles; the fact that substances tend to be more soluble in a hot solvent than in cold solvent, and that each solute tends to behave as though it were alone in the solvent.
Using the correct solvent is a very important part of the process. The solute must be insoluble in the solvent at room temperature, and as the temperature of the solvent increases, the solubility of the solute also increases. It is also important that the impurities present are soluble in the solvent at room temperature and insoluble at higher temperatures. An excellent substance for showing this process is benzoic acid (C 6 H 5 COOH). A molecular crystal rather than an ionic crystal, shown by its low melting point of 122 °C, benzoic acid is used as an anti- microbial agent and is found in toothpastes, mouthwashes, cosmetics and deodorants. Impure benzoic acid contains the impurities phthalic acid and benzylbenzoate. If the impure sample is dissolved in a minimal volume of hot solvent – in this case boiling water – and filtered to remove insoluble impurities, the resulting solution will contain dissolved benzoic acid as well as dissolved impurities. Upon cooling, the benzoic acid crystals comes out of solution as its solubiluty in the solvent decreases. The impurities will remain in solution and can be filtered off. It is very important when carrying out this experiment that rubber gloves are worn, because organic substances can be absorbed through the skin, and as well, goggles should be worn to protect your eyes from hot liquids which may spray out from the flask. to be created. It is possible to produce crystals of varying particle size, polymorphs suitable for drug development and manufacture. to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs suitable for drug development and manufacture. targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape, use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
our substance?
A pure substance has a fixed melting point while an impure substance melts over a wide range of temperatures and at a lower temperature than the pure substance. The melting points of almost all substances are available in tables. To check the melting point place a few crystals of the sample on an aluminium block which has a thermometer inserted. Use a hot plate to heat the block slowly. Watch the crystals carefully and note the temperature at which they begin to melt and the temperature at which they have all melted. Compare this value with the value found on the bottle of pure substance. Another method of checking the melting point of crystals is to use a narrow capillary tube in an oil bath. The capillary tube has one end open and the other end sealed. The open end is pressed into fine crystals of the substance and the turned upside down and Beaker containing benzoic acid dissolved in minimum amount of boiling water Filter funnel with fluted filter paper to speed up the filtrarion process. Insoluble impurities left behind as residue Conical flask with hot concentrated benzoic acid solution which still contains soluble impurities Fig.1 Filtration to remove insoluble impurities Pure benzoic acid cystals Büchner funnel Büchner flask Water containing soluble impurities Fig.2 After cooling, the remaining solution is filtered off Thermometer Benzoic acid crystals Aluminium block Bunsen burner Fig.1 Finding the melting point of benzoic acid Percentage yield = x 100
Glax www
company committed to excellence and innovation. We are the second largest life science company in the world and have a leadership position in four major therapeutic areas – anti- infectives, gastrointestinal/metabolic, respiratory and central nervous system. The source of our competitive advantage is the energy and commitment of our employees. Our mission is to improve the quality of human life to enable people to do more, feel better and to live longer. World-wide we employ over 110,000 people and have 80 manufacturing sites in 37 countries. At our Cork Site in Currabinny, which was established in 1975, we manufacture the active ingredients of medical compounds. Our Currabinny facility employs over 500 people, many of whom are engaged in development chemistry, analytical and quality chemistry and chemical and process engineering. The Cork facility is a strategic global new product introduction site within GSK’s manufacturing network. We have a highly automated manufacturing facility, as well as an R&D Pilot Plant with Pilot Plant Laboratories on site. We are currently the primary production site for a number of GSK’s top selling drugs which treat illnesses such as depression, Type 2 Diabetes, Congestive Heart Failure, Ulcers, HIV, Ovarian Cancer, Breast Cancer, Parkinson’s Disease and Arthritis. GlaxoSmithKline also has a manufacturing and R&D facility in Dungarvan, Co. Waterford and sales and marketing functions in Dublin. GSK currently employs over 1,400 in Ireland. � �
of its tapped sharply against the desk causing the crystals to fall to the sealed end. When about 3 mm of crystals are in the base of the tube it is placed in the oil bath. The temperature at which the sample begins to melt and the temperature at which it is completely melted are recorded. To double check your result, mix a sample of benzoic acid with some pure benzoic acid. If both are pure benzoic acid the melting point will remain the same but if the sample is not pure benzoic acid then the melting point will be lowered. How do I know I have a pure substance? The melting point of a substance is not the exact point at which it melts but rather the range of temperatures from when the samples starts to melt until it has completely melted. The greater the range the more impurities present. A range of less than 1 °C indicates a pure substance. How is crystallisation used in industry? The use of crystallisation in the pharmaceutical industry is an important process for controlling the physical properties, yield and purity of an Active Pharmaceutical Ingredient (API). Many production processes use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape, to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs of the same substance, but only one will be suitable for drug development and manufacture. In industry, the way an API is filtered and dried can have a very significant impact on the physical properties of the material. Calculating the percentage yield After the crystallisation process the amount of sample will have been reduced as impurities have been removed. To calculate how much of the pure substance was present in the initial impure sample, the percentage yield is calculated.
Mass of pure sample (after recrystallisation) Mass of impure sample (before recrystallisation)
sample. A high percentage yield implies a low concentration of impurities, whereas a low percentage yield indicates a sample with a lot of impurities. to be created. It is possible to produce crystals of varying particle size, polymorphs suitable for drug development and manufacture. to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs suitable for drug development and manufacture. targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape, use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
Thermometer Benzoic acid crystals Aluminium block Bunsen burner Fig.1 Finding the melting point of benzoic acid Percentage yield = x 100
GlaxoSmithKline at www.gsk.com, www.gsk.com/worldwide/ie.htm or at www.sta.ie
Glaxo comp the s a lea infect nervo
The comm qualit to live
World manu Curra the a facilit in de chem
The C site w autom with P
We a GSK’ Type Canc
Glaxo Dung Dubli
tapped sharply against the desk causing the crystals to fall to the sealed end. When about 3 mm of crystals are in the base of the tube it is placed in the oil bath. The temperature at which the sample begins to melt and the temperature at which it is completely melted are recorded.
To double check your result, mix a sample of benzoic acid with some pure benzoic acid. If both are pure benzoic acid the melting point will remain the same but if the sample is not pure benzoic acid then the melting point will be lowered.
The melting point of a substance is not the exact point at which it melts but rather the range of temperatures from when the samples starts to melt until it has completely melted. The greater the range the more impurities present. A range of less than 1 °C indicates a pure substance.
The use of crystallisation in the pharmaceutical industry is an important process for controlling the physical properties, yield and purity of an Active Pharmaceutical Ingredient (API). Many production processes use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape, to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs of the same substance, but only one will be suitable for drug development and manufacture.
In industry, the way an API is filtered and dried can have a very significant impact on the physical properties of the material.
After the crystallisation process the amount of sample will have been reduced as impurities have been removed. To calculate how much of the pure substance was present in the initial impure sample, the percentage yield is calculated.
Mass of pure sample (after recrystallisation) Mass of impure sample (before recrystallisation)
The percentage yield is a good indicator of the purity of the initial sample. A high percentage yield implies a low concentration of impurities, whereas a low percentage yield indicates a sample with a lot of impurities.
Recrystallisation is a very important purification technique, purifying substances by removing unwanted by-products. It is also used to manufacture the correct crystal size and shape of a material. These factors can have a very significant impact on how a medicine acts when taken by a patient. The same principles and techniques of recrystallisation can be applied both on a laboratory and industry scale.
The process depends on two principles; the fact that substances tend to be more soluble in a hot solvent than in cold solvent, and that each solute tends to behave as though it were alone in the solvent.
Using the correct solvent is a very important part of the process. The solute must be insoluble in the solvent at room temperature, and as the temperature of the solvent increases, the solubility of the solute also increases. It is also important that the impurities present are soluble in the solvent at room temperature and insoluble at higher temperatures.
An excellent substance for showing this process is benzoic acid (C 6 H 5 COOH). A molecular crystal rather than an ionic crystal, shown by its low melting point of 122 °C, benzoic acid is used as an anti- microbial agent and is found in toothpastes, mouthwashes, cosmetics and deodorants.
Impure benzoic acid contains the impurities phthalic acid and benzylbenzoate. If the impure sample is dissolved in a minimal volume of hot solvent – in this case boiling water – and filtered to remove insoluble impurities, the resulting solution will contain dissolved benzoic acid as well as dissolved impurities.
Upon cooling, the benzoic acid crystals comes out of solution as its solubiluty in the solvent decreases. The impurities will remain in solution and can be filtered off.
It is very important when carrying out this experiment that rubber gloves are worn, because organic substances can be absorbed through the skin, and as well, goggles should be worn to protect your eyes from hot liquids which may spray out from the flask.
to be created. It is possible to produce crystals of varying particle size, polymorphs suitable for drug development and manufacture.
to be created. It is possible to produce crystals of varying particle size, shape and form polymorphs suitable for drug development and manufacture.
targets. Recent advances in crystallisation process monitoring allow for a better understanding of the process. These advances allow crystals with specific physical properties, for example particle size and shape,
use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
use crystallisation in the final stage of manufacture to achieve these targets. Recent advances in crystallisation process monitoring allow for
A pure substance has a fixed melting point while an impure substance melts over a wide range of temperatures and at a lower temperature than the pure substance. The melting points of almost all substances are available in tables.
To check the melting point place a few crystals of the sample on an aluminium block which has a thermometer inserted. Use a hot plate to heat the block slowly. Watch the crystals carefully and note the temperature at which they begin to melt and the temperature at which they have all melted. Compare this value with the value found on the bottle of pure substance. Another method of checking the melting point of crystals is to use a narrow capillary tube in an oil bath. The capillary tube has one end open and the other end sealed. The open end is pressed into fine crystals of the substance and the turned upside down and
Beaker containing benzoic acid dissolved in minimum amount of boiling water
Filter funnel with fluted filter paper to speed up the filtrarion process. Insoluble impurities left behind as residue
Conical flask with hot concentrated benzoic acid solution which still contains soluble impurities
Fig.1 Filtration to remove insoluble impurities
Pure benzoic acid cystals
Büchner funnel
Büchner flask
Water containing soluble impurities
Fig.2 After cooling, the remaining solution is filtered off
Thermometer
Benzoic acid crystals
Aluminium block
Bunsen burner
Fig.1 Finding the melting point of benzoic acid
Percentage yield = x 100