0% found this document useful (0 votes)
38 views17 pages

A Beginners Guide Mastering Rotatory Evaporation

Uploaded by

Chila
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
38 views17 pages

A Beginners Guide Mastering Rotatory Evaporation

Uploaded by

Chila
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 17

A Beginner’s Guide

Mastering Rotary Evaporation


Table of Contents

1. Introduction 5

2. What is Rotary Evaporation? 6


2.1 Definition and basic principals 6
2.2 Historical perspective 6
2.3 The components of a rotary evaporator 7
2.4 Laboratory applications 8

3. Theory of Distillation 10
3.1 States of matter 10
3.2 Phase transitions 10
3.3 A closer look at thermodynamics 11
3.4 Transport of gas in the system 14
3.5 Separation by distillation 15
3.6 Drying 16

4. The Distillation Process 17


4.1 Distillation using a rotary evaporator 17
4.2 The drying process 17

5. How to Optimize the Process 18


5.1 Temperature and pressure 18
5.2 Evaporating flask size 20
5.3 Rotation speed 20
5.4 Working with a mixture of solvents 21

6. Environmental Considerations 22
6.1 The importance of minimizing solvent loss 22
6.2 When to immerse the flask into the heating bath 22
6.3 Equipment considerations 22

7. Conclusion 23

8. References 24

9. Appendices 26
9.1 Table of solvents 26
9.2 Working pressures for different vapor temperatures of various solvents (mbar) 28
9.3 Glossary of terms 30

2 3
1. Introduction

The aim of this guide is to provide you with everything you need to know to master rotary evaporation, a fun­
damental technique used in laboratories worldwide, starting with the origins of the distillation process, covering
relevant theory, and continuing with applications and how to optimize the process. It is recommended for
beginners to follow through each section to gain a well-rounded understanding of all aspects of the topic. For more
advanced chemists, feel free to jump straight into sections of interest, as there are always new things to learn,
especially when it comes to optimizing the process. The appendices at the end of the guide provide a valuable
resource for anyone starting a new application.

4 5
2. What is Rotary Evaporation?

2.1 Definition and basic principals Islamic golden age (8th –13th century): During this period, the art of distillation advanced significantly in the
The rotary evaporator is a vacuum distillation apparatus widely used in chemistry laboratories to remove Islamic world. Alchemists such as Jabir Ibn Hayyan and Abu Bakr al-Razi made significant contributions,
solvents efficiently and gently from a chemical product. Other applications include drying and Soxhlet extraction refining and perfecting distillation methods and apparatus.
(see section 1.4).
Medieval Europe (12th –15th century): Knowledge of distillation spread to Europe through translations of
Distillation is a separation method that involves evaporating a liquid from a mixture and then condensing it. Arabic texts. It was primarily used for medicinal purposes and distilled spirits.
This process relies on the principle that the vapor formed from a boiling mixture has a different composition
than the original liquid. The component with a lower boiling point becomes enriched in the vapor. Nowadays, The birth of modern chemistry (16th–17th century): Distillation played a vital role in the transition from alchemy to
various distillation methods exist, each with its own advantages and disadvantages. modern chemistry. Notable figures like Paracelsus and later Robert Boyle used distillation in their experiments.
Focus was placed on improving the technology, such as insulating the equipment and using glass instead of metal.
The rotary evaporation technique involves heating a mixture in a rotating flask. The rotation increases the Boyle performed the first vacuum distillations at the end of the 17th century, further refining the process.
surface area and makes the process more efficient than other distillation methods while reducing the risk of
local overheating and incrustation. Rotary evaporator distillations are typically performed under vacuum to Industrial revolution (18th –19 th century): The development of more efficient stills and the rise of industrial
reduce the boiling points, enabling evaporation at low temperatures, therefore allowing a gentler process and chemistry saw distillation become critical in various industries, from the production of spirits and essential oils
preserving heat-sensitive materials. to the refining of petroleum. The invention of rectifying columns enabled multi-stage distillation, and the
invention of the pressure regulator and improvement of pumps enabled a more directed use of the vacuum.

2.2 Historical perspective 20 th century to present: Modern distillation technologies evolved with advances in materials. Articles by C.C.
Since its introduction in the mid-20 century, rotary evaporation has become a staple in laboratories worldwide
th
Draig (1950) and M.E. Colk (1955) published the operating principles behind the rotary evaporator, which had a
for applications such as solvent removal and solvent purification. The development of the rotary evaporation far better heat transfer rate, which spared the product and increased output. In 1957, Walter Büchi introduced
technique began thousands of years ago when basic distillation processes started to be used. Below is a brief the first rotary evaporator to the market. Today, distillation is vital to many industries, including chemical,
history of key dates and developments. pharmaceutical, environmental, and food and feed.

2.3 The components of a rotary evaporator


A rotary evaporator (see Figure 1) consists of three main parts.

Heating bath
Ancient Greek Islamic Modern Industrial 8 Support frame
Present 5
times alchemy golden age chemistry revolution Lift
Rotary drive
Ancient times (circa 3000–1200 BC): Distillation is believed to have begun with the Babylonians of ancient Interface
4
Mesopotamia. Early evidence describes how the process was used for perfumery, and the technique quickly Evaporating flask
spread across Europe, North Africa, and Asia. Baked clay stills across the Indian subcontinent and China Vapor duct with vacuum seal
7
suggest basic distillation methods. Many uses were found for distillation beyond creating essences, such as 6 Condenser
desalinating seawater and alchemy. Receiving flask

Greek alchemy (circa 1st century AD): Greek alchemist Maria the Prophetess is credited with several
2
important innovations and improvements, such as the water bath (bain-marie), which is used to heat 3
9
substances gently and gradually. It is still used in laboratories today. She is also credited with inventing the
tribikos (three-armed-still) and the kerotakis (used for sublimation and other processes).

Figure 1. A schematic illustration of a rotary evaporator with its main components labeled.

6 7
1. The heating bath supplies the energy required for evaporation. A heating element beneath the bath base Rotary evaporators can also be used to perform chemical synthesis. In some reactions, reactants need to be
heats the liquid. heated to their boiling points to react and form the desired products. However, the yield would be minimal if the
2. The support frame holds together and accommodates the lift, the rotary drive, and the interface. The lift reactants simply evaporated. To counter this, a reflux glass assembly is used whereby the connection to the
enables quick introduction and removal of the flask from the heating bath. The rotary drive is used to rotate receiving flask can be closed so that the condensate flows back into the reaction mixture. By following this
the evaporating flask. The interface differs depending on the model of the rotary evaporator. Basic models method, the yield can be significantly increased. The oxidation of ethanol to ethanal and, later, ethanoic acid is
feature knobs/buttons for adjusting rotation speed and heating bath temperature. It is also possible to have an example of a reaction where distillation and reflux come into play.
an additional vacuum control interface. Advanced rotary evaporator interfaces may incorporate a vacuum
controller providing one place to control both the evaporation parameters and the system pressure, A Soxhlet extraction, with the Soxhlet accessory, enables liquid-solid extraction of poorly soluble compounds
enabling automatic distillations, allowing for more streamlined and efficient operation. from an insoluble solid matrix, as illustrated in Figure 2. This is achieved by several immersion cycles in the
3. The glassware includes an evaporating flask where the sample mixture is heated, a vapor duct with a condensed solvent using a constant-level siphon. It is commonly used to extract fat from seeds, nuts, or
dedicated vacuum seal that directs vapor to the condenser (or a dedicated glass assembly), which cools and chocolate, as well as for valuable bioactive compounds from natural sources. Its applications can be found in
condenses the vapor back into a liquid, and a receiving flask for collecting the distilled solvent. The glassware natural products, forensics, environmental, and pharmaceutical segments, to name a few. The benefit of using a
is designed to withstand thermal shock and ensure durability. rotary evaporator instead of a static glassware apparatus is to have multiple instruments in one. The extraction
process can be performed at a higher distillation rate (greater heat transfer due to rotating evaporating flask and
vacuum), and the solvent can be removed from the extract without having to change the instrument.
2.4 Laboratory applications
Rotary evaporators have found extensive applications across various fields, including chemistry, biology, and
even the food and beverage industry.

The primary application is distillation to remove solvents or solvent mixtures from the final reaction product. 3

The primary interest is in the substance remaining in the evaporating flask after the solvent has been
evaporated. For an effective separation, the boiling point of the product and the solvent at atmospheric
pressure must differ by approximately 80 ºC.
4
Depending on the application, the solvent can either be removed completely or only partially.
2

Powders or granular solid materials containing traces of solvents can be dried in the rotary evaporator. One example
of that is the separation of brine into salt and water. Evaporating part of the solvent can increase the concentration
of a dissolved substance. This is commonly used in analytical chemistry to lower the volume of a sample to a level
appropriate for examination. In addition to traditional chemistry, concentration with the use of rotary evaporators is
1 5
also used in molecular cooking, e.g., to remove water from fruit juice to produce a concentrated flavor.

A special form of concentration is recrystallization. After dissolving a contaminated solid substance in a


suitable solvent, the solvent is slowly evaporated. The substance of interest is concentrated and forms pure
crystals. This process leaves impurities dissolved in the residual solution from which the crystals must be separated.
Figure 2. A schematic illustration of a Soxhlet extraction using a rotary evaporator equipped with a Soxhlet accessory.
The focus can also be on the condensed solvent, such as in the case of solvent recycling. Distillation can be
used to clean a contaminated solvent. In this process, the cleaned solvent condenses into the receiving flask
while less volatile contaminants remain in the evaporating flask. As rotary evaporation often takes place after The solvent in the evaporating flask is heated.
chromatography, one can think of recycling solvents used for chromatographic analyses (note: it does not work The vapor from the solvent rises through a side arm into the condenser.
when the solvents form azeotropic mixtures). In elutes, one can find, for example, ethyl acetate, hexane, and The vapor is cooled by the condenser, condensing back into liquid form, and drips onto the solid material in
acetonitrile. Environmental considerations, as well as the cost of chromatography-grade solvents and the cost the thimble.
of disposing of used solvents, might be a good argument for using distillation for solvent recycling. The solvent extracts the desired compound from the solid material as it fills the extractor chamber.
Once the solvent level reaches a certain height, it siphons down into the round-bottom flask, carrying the
extracted compounds.

8 9
3. Theory of Distillation

Gas
3.1 States of matter
Depending on the temperature and pressure, any material may be present in various states. The three classical
states of matter are solid, liquid, and gas (see Figure 3).

The macroscopic properties of a substance under given conditions relate to the microscopic properties of its

Va
n
io
molecules. The shape and structure of molecules influence the distribution of electrons when molecules are

p
sit

or
po

iz a
close together and, thus, the interactions between the molecules. One such interaction is the attraction

C
n

on
De

io

ti o
at

de
between molecules of a substance, known as cohesion (or adhesion in the case of different particles or

n
im

ns
bl
surfaces). This interaction is responsible for phenomena such as the formation of droplets or the presence of

at
Su

io
n
menisci in liquids. In general, these attractive forces cause particles to cling together.

Melting
Solid Liquid
Freezing
Figure 4. A diagram illustrating phase transitions between three states of matter: solid, liquid, and gas.

When heat is applied to a solid material, its kinetic energy increases steadily until, at the melting point, the kinetic
Figure 3. Particle model of the three states of matter (from left to right): solid, liquid, and gas.
energy becomes strong enough to overcome the forces of attraction. The material liquefies. This process is called
melting. Individual molecules are now able to move almost freely within the substance, but the attraction
For a solid, the matter has a fixed shape that occupies a fixed volume and can only be changed by an external between them is still too strong to let them separate from the other molecules. Additional heating of the substance
force. The particles (atoms, molecules, or ions) are close together, and the interactions between them are removes that energy barrier up to the boiling point at which the molecules have sufficient kinetic energy to move
strong. The particles show only small degrees of motion due to a high binding energy. They swing in a fixed freely within space without being held back by intermolecular forces of attraction. The liquid boils and changes
position in their molecular lattices and usually rotate around their axes. The higher the temperature, the more into a gas with an enormous increase in volume in a process called vaporization. It continues to expand when
violently they swing or rotate, and the distance between the particles usually increases. heated. However, any state of matter is influenced not only by temperature but also by pressure. Especially for
gas, the lower the pressure, the weaker the forces of attraction between the molecules. This means that the
In a liquid state, matter takes on the shape of its container but occupies a (nearly) fixed volume. The inter­ boiling point decreases with decreasing pressure. Therefore, supplementing heat is not the only way to induce the
molecular/interatomic forces are less strong than in a solid, letting particles move almost freely within a relatively transition from liquid to gas. One can also reduce the pressure. When a gas turns into a liquid, it is called
close distance. This results in a mobile structure. In most cases, the liquid occupies a volume slightly larger condensation. This happens when the temperature is lowered, and molecules lose kinetic energy. Gas can also
than the corresponding solid. be liquefied by compression. When a liquid turns into a solid, it freezes or solidifies.

In a gas state, matter takes both the shape and volume of its container, allowing it to occupy a volume For some materials, under the right conditions, a solid can transform directly into the gaseous phase, bypassing
hundreds or thousands of times larger than its corresponding liquid or solid state. The particles in a gas do not the liquid state. This process is called sublimation. The reverse process is called deposition.
have fixed positions and are far apart from each other, with enough energy to move freely. In an ideal gas, these
particles do not interact at all. In practice, the intermolecular forces have very little effect. Usually, matter exists in one or a combination of these states. For example, a block of steel is solid, while a river
with ice in it and water vapor in the air encompasses all three states. However, there are special conditions,
such as the critical point or the triple point, where the boundaries between the phases disappear. The state of a
3.2 Phase transitions compound at a particular pressure and temperature combination can be found in a phase diagram.
As the conditions (pressure, temperature) change, matter may undergo a phase transition, i.e., change from
one state to another. Phase transitions are reversible. Figure 4 illustrates phase transitions between the three
classical states of matter: solid, liquid, and gas. 3.3 A closer look at thermodynamics
3.3.1. Vapor pressure boiling point
Although liquid vaporizes at its boiling point, it can also give off gas before it boils: it evaporates at far lower
temperatures. As the heat is supplied to the liquid, a few of the molecules on its surface can gather enough
energy to overcome the forces of attraction and escape into the environment as a gas. This process cools the
liquid since an amount of energy is withdrawn from it. The higher the temperature, the more likely it is that a
particle will be able to gather enough energy to escape into the gas phase.

10 11
· Vapor pressure In a rotary evaporator, the necessary heat is supplied through the heating bath. The bath is filled with a liquid
The escaping molecules exert a pressure counter to the outside pressure. This pressure is called vapor pressure. that serves as a heating medium. The substance used as a heating medium should have good thermal
The more particles that can free themselves from the liquid, the higher that pressure. Vapor pressure is a measure conductivity and a high heat capacity. Usually, water or oil are used. In practice, most solvents used in
of compound volatility. It depends on temperature and differs from one compound to another. chemistry laboratories can be distilled with the rotary evaporator at a heating bath temperature of 50 °C.
This relatively low temperature contributes to the importance of water as the heating medium of choice as
Since the number of particles able to leave the liquid keeps increasing with the rising temperature, vapor pressure contrasted with oil, whose main advantage over water is that it can be heated to much higher temperatures.
rises with temperature. The Clausius-Clapeyron equation shows how vapor pressure depends on temperature:
Water is a great heating medium for several reasons. It stores heat particularly well due to its high heat capacity
dIn p Lv
= (Eq. 1) and offers excellent thermal conductivity. Water is not only inexpensive and readily available but also keeps the
dT RT2 heating bath clean. Its maximum heating limit of 100 ºC significantly reduces the risk of personal injuries
compared to oil baths, which can reach up to 220 ºC. It is crucial to use a heating medium that is compatible
Where p [Pa] is the vapor pressure, T [K] the temperature, R = 8.3145 J · (mol · K) –1 the universal gas constant, and with the heating bath used since water baths can have a higher heating density than oil baths. As oil has lower
Lv [J · mol–1] is the molar heat of vaporization. Once the vapor pressure becomes equal to the outside pressure, thermal conductivity than water, using it in the water heating bath can cause local overheating and increase the
there is no longer any force present that can hold the gaseous molecules back in the liquid. The liquid starts to boil. risk of retarded boiling of the heating medium, which poses a great danger for the user.

· Boiling point A layer of liquid at the bottom of the heating bath (close to the heat source) typically gets hot first. The upper
Boiling occurs at specific combinations of pressure and temperature. The boiling parameters can be found layers remain colder. Convection causes the warm layers to rise, and the colder layers take their place. This leads
using the following equation, which is an approximation of the Clausius-Clapeyron equation. to a slow equalization of temperature. The heat transfer can be further improved by keeping the liquid in motion
with an agitator. For the same reason, the liquid is evaporated from a rotating flask (as is the case in a rotary
For the boiling temperature at a given pressure, use: evaporator). This continuous mixing or forced convection enables excellent heat transfer, better expulsion of the
gas, and quicker distillation.
Ts
Tp = (Eq. 2)
(3.006 - log p) · b + 1
3.3.2. Boiling
Where Ts [K] is the boiling point at atmospheric pressure, and Tp [K] is the boiling point at operating pressure p [mbar]. When boiling occurs, a phase transition from liquid to gas takes place throughout the entire volume of the
The constant b is solvent-specific and can be found in the Table of Solvents in the Appendix (chapter 7.1). liquid. The boiling point is crucial in distillation because gases formed by boiling are removed much faster from
the liquid than by mere evaporation below the boiling point. As the molar volume of a gas is many times that of
For the system pressure when knowing the temperature value, use the rearranged form: a liquid, the substance typically expands about 800 to 1,000 times during boiling. Care must be taken to ensure
that the distillation equipment can handle this increase in volume.
Ts - Tp
log p = 3.006 - (Eq. 3)
b · Tp · Nucleate boiling
The first stage of boiling during distillation is nucleate boiling. Heat causes bubbles to form at nucleation sites
Chapter 4.1.1 provides a few examples of how to make use of Eq. 2 and Eq. 3. on the walls of the container. These bubbles grow as the heat (and pressure) increases, and the gas formed in
other parts of the liquid penetrates the bubbles. They partially detach when buoyant enough to overcome
· Heat of vaporization and transfer of heat adhesive forces, rising to the surface. As heating continues, more bubbles form, eventually creating a
For the phase transition from liquid to gas, at first, energy is needed to raise the liquid temperature to its boiling continuous film of vapor along the container wall.
point (to raise its vapor pressure to the ambient pressure level). However, when a liquid is heated to its boiling
point, and the source of heat is removed, the boiling stops because the energy needed for vaporization has · Special case: bumping
been withdrawn. The liquid cools to below its boiling point. Thus, heat must be supplied continuously to keep a Bumping, or retarded boiling, occurs when a liquid is heated to a temperature above its boiling point
liquid boiling. The amount of additional energy depends on the heat of vaporization of the substance. The heat (superheating) and, upon nucleation, it erupts or splashes. Without sufficient nucleation sites, the liquid forms
of vaporization is a very important parameter in connection with boiling. It is defined as the amount of heat that unstable bubbles that erupt violently upon reaching the surface. This can lead to eruptive boiling, contaminating
must be supplied to evaporate a defined amount of the liquid. A high boiling point does not necessarily mean a the clean side of the system (vapor duct, condenser, and receiving flask). Preventing bumping is crucial for
high heat of vaporization. Water, with a boiling point of 100 °C, has a heat of vaporization of 2,261 kJ/kg, while safety, process efficiency, and sample integrity and can be achieved through careful control of process
xylol, with a boiling temperature of 144 °C, only requires 345 kJ/kg. parameters or the use of a bump trap.

12 13
3.3.3. Condensation
Condensation is the reversal of the evaporation (or vaporization) process, in which a substance changes from
its gaseous to its liquid state. The heat transferred to the molecules during evaporation must be dissipated to
condense a gas into a liquid.

The vapor moving from the point of evaporation (see section 2.4) reaches the condensation part of the rotary
evaporator, i.e., the condenser. The temperature of the condenser is lower than the temperature of the vapor.
Therefore, the vapor precipitates, and a liquid film forms at the condenser surface. The speed of this process is
governed by the heat transfer rate, which, in turn, depends on the difference between the vapor temperature
and the cooling medium. It was found (see Chapter 4.1.1) that a difference of 20 °C or higher is optimal for
efficient condensation.

As the condensed film hinders heat transfer between incoming gas and the coolant, it must be ensured that
this film can be removed or flow away. Condensers are, therefore, always mounted vertically or diagonally.
The draining off condensate collects in the receiving flask. To ensure effective condensation during the entire
distillation process, the cooling medium must be continually refreshed (e.g., by flowing tap water) or re-cooled
(e.g., by a recirculating chiller).
Figure 5. The thermal pump (P) within the rotary evaporator.
Boiling causes a rise in volume as the liquid transforms into a gas. Condensers usually have a large surface area to
provide for effective heat dissipation from the gas with a volume much larger than that of the liquid. In a closed
system, the rise in volume also causes a rise in pressure. During condensation, a large part of the pressure increase 3.5 Separation by distillation
is dissipated, and in a well-balanced distillation, it can be fully compensated. The condenser acts like a pump. The critical factor enabling separation by distillation is the difference in volatility (vapor pressure) of compounds
or how readily each component of a mixture converts from liquid to vapor. The greater the relative volatility
difference between the components, the more effective the separation. During heating, the more volatile
3.4 Transport of gas in the system components accumulate in the vapor. This enriched vapor travels through the distillation apparatus to the
Evaporation and condensation usually take place at different locations in the apparatus. The vapor created condenser, where it condenses and is collected in a receiving flask. At the same time, the less volatile
during evaporation must be transported to the condensation area. This transportation is straightforward due to component remains in the evaporating flask. The lower the amount of the high-boiling component in the vapor,
a key property of gases: they expand to fill the available space. As a result, the vapor flows naturally from the the better the separation.
area of evaporation to the area of condensation.
If the boiling points of two components differ by more than 80 °C at atmospheric pressure, effective separation
When the vapor turns back into a liquid in the condensation area, the volume decreases, creating a vacuum. can usually be achieved with a single distillation. This method is often used to separate highly volatile solvents
This vacuum continuously draws more vapor from the evaporation area. At the same time, vapor is generated from less volatile materials. However, when the boiling points of the components are close, multiple distillation
in the evaporation area to replace what has been drawn away. This creates a dynamic pressure difference that cycles-known as rectification-may be necessary.
moves the vapor through the system, as shown in Figure 5. The driving force for this movement is the supplied
heat, at least equal to the heat of vaporization. The difference in relative volatility is not the sole factor in separation. The specific properties of the mixture and
the relative amounts of the components also significantly influence separability. The vapor pressure
It is important that the rate of condensation and the rate of evaporation are matched. If more substance is dependence of each component on the mixture’s composition is described by Raoult’s law:
evaporated than condensed, the pressure in the apparatus will increase, and the vacuum pump will have to run
continually, pulling in solvent vapor and blowing it into the environment. See Chapter 4 for tips on how to work p1 = p1* ∙ x1 (Eq. 4)
efficiently with a rotary evaporator and ensure that the process remains in equilibrium.
Where p1 is the partial vapor pressure of solvent 1, p1* is the vapor pressure of pure solvent 1, and x¹ is the mole
fraction of solvent 1 in the mixture.

14 15
4. The Distillation Process

For some solvent mixtures, the vapor and liquid compositions may be identical at certain concentrations, 4.1 Distillation using a rotary evaporator
making separation impossible. This occurs at a molar fraction referred to as the azeotropic point. An azeotrope Here are the steps to conduct a distillation process with a rotary evaporator. Some variations to the procedure
is a mixture that boils at a temperature either lower or higher than that of its individual constituents, limiting are possible.
distillation to the azeotropic point.
· Initial checks: All seals, joints, etc., should be checked, greased if necessary, and locked in position. Note: PTFE
gaskets must never be greased.
3.5.1. Improvement of the separation · Connect hoses: Water hoses should be secured with hose clamps. Vacuum hoses should all be of the same
There are several ways in which the separation can be improved: internal diameter and kept as short as possible.
· Determine the optimal temperature and pressure values: These values must be determined according
· The greatest improvement is attained by means of multistage distillation. to the planned application, usually using the ΔT = 20 ºC rule (see section 4.1.1).
· Optimization of the pressure and temperature (see sections 4.1 and 4.1.1). This includes continual adaptation · Fill and attach the flask: The flask can now be filled with the mixture (up to half its volume) and connected
of the parameters since these parameters change as the composition changes. to the rotary evaporator.
· Working in a vacuum. Since relative volatility is higher at low-temperature values, one can take advantage of · Switch on the coolant flow: If applicable, start the connected recirculating chiller. If in-house water cooling
that by using lower temperatures enabled by working under a vacuum. is used instead of a recirculating chiller, turn on the circulation of the cooling water. The flow rate should be
· Installing fillers, e.g., Raschig rings, causes partial condensation on the evaporation side, producing a between 40 and 50 L/h.
counterflow enriched with the higher-boiling component. This principle is also referred to as countercurrent · Heat up the bath: Set the determined operating temperature and start the heating. Using a low bath
distillation. temperature saves energy compared to a higher temperature, which requires more heat input.
· Keeping the mixture in motion by stirring it or rotating it prevents the depletion of the lighter-boiling substances · Set the pressure on a vacuum interface and start evacuation: This adjustment is not made if the
at the surface. distillation is to be run automatically.
· Set rotation speed: Adjustment of the rotation speed completes the preparations for distillation. It is best to
start the rotation at a reduced speed and increase it to the maximum speed once the flask is immersed in the
3.6 Drying heating bath. This can help reduce splashes of the hot heating medium.
Drying is the process of separating a liquid from a solid. Occasionally, it also involves removing water from · Lower the flask: Lower the evaporating flask into the heating bath. If the mixture tends to foam, lower the
high-boiling liquids. In a rotary evaporator, drying typically occurs under vacuum. During this process, vapor is flask gradually. After a short while, the first condensate will appear in the condenser.
carried away from the material. When the product is sufficiently moist, the drying speed depends on the same · Monitoring the distillation: This should be done at regular intervals. Monitor the bath temperature, the
factors as the distillation speed: vapor pressure, system pressure, and heat supplied. vapor temperature (if available), the system pressure, and the condensate level. Short aeration can suppress
any foaming that occurs. Whenever distilling a mixture, the pressure may require readjustment.
As the liquid evaporates from the surface, the drying rate begins to be influenced significantly by the thermal · Ending distillation: When the distillation is complete, the rotation must be stopped. Next, the evaporating
conductivity of the solid and the movement of moisture from the interior to the surface (considering pore flask must be lifted from the bath, and the system must be aerated. Finally, the heating bath must be switched
structure and hygroscopic behavior). Since the vapor pressure of a solid is much lower than that of the liquid off, and the cooling must be shut off.
being removed, complete separation is theoretically possible.
The distillation is now complete.
However, differences arise when drying solids compared to separating components from a liquid mixture.
The product being dried can be present in various forms: as a moist solid, as a pulp or paste, or as a solution
or suspension. Each form requires different procedures. Rotary evaporators are most effective for separating 4.2 The drying process
liquids from solids in solutions but are also used for drying slurries. The solvent is distilled off until the solid The drying process is essentially the same as that for distillation. Whenever processing powders or granulates,
crystallizes out completely. The remaining solvent can then be drained off, and the crystals can be finish-dried it is recommended to use a drying flask with built-in baffle plates and the dedicated drying mode of the rotary
in a separate laboratory instrument, such as a drying chamber. evaporator (that periodically changes the rotation direction). It is advisable to empty the receiving flask regularly
when boiling down solutions to dryness, particularly in the final stage. When the system pressure is very low,
even solvents collected in the receiving flask can start to re-evaporate. The re-evaporated solvent can enter the
distillation path again, causing the system to work harder and longer to achieve the desired dryness.
Furthermore, the re-evaporated solvent can potentially carry contaminants, affecting the purity of the final
product. Therefore, the receiving flask should be emptied regularly. To attain complete dryness, the system
pressure must be lowered as much as possible.

16 17
5. How to Optimize the Process

Regarding pressure, a practical way to check if the value is not too high or too low is to monitor the pump and the
The selection of the correct equipment and the structural design of the apparatus are important for obtaining condensate level in the condenser, ensuring the top part remains clear. This empty space acts as a safety barrier,
optimum distillation results. Other crucial factors include the process temperature and pressure, evaporating protecting against pressure fluctuations and the effects of any low-boiling solvents that might be carried along. If
flask size, and rotation speed. no condensation level is visible, it may indicate that the pressure is too low, resulting in a very small difference
between the cooling temperature and boiling point. In such a case, the vacuum pump would be overloaded.

5.1 Temperature and pressure To help judge the process, consider the following:
To find optimal process parameters, one needs to consider the energy balance in the rotary evaporator as shown
in Figure 6. · If the pump is constantly active, there is likely a mismatch between the supplied and dissipated energy,
indicating that the distillation may be too fast. In this case, the distillation rate should be decreased.
Heating (thermal energy) · If the condensate level in the condenser is too low (below approximately 75 %), it indicates that the distillation
5
Solvent / Analyte is running too slowly, and the distillation rate can be increased.
Evaporation
Vapor A more formal way of finding the optimal pressure value is to use Eq. 2 and Eq. 3 introduced earlier, which are
Condensation (energy removal) also presented in the following section (4.1.1).
4 Distillate
3
5.1.1. The delta 20 rule
2 Several factors affect the optimal working temperatures, the most important being the properties of the
substance being distilled. The Delta 20 Rule is a useful rule that helps choose the correct temperature settings.
1 It states that there should be a 20 ºC difference between the cooling and the boiling temperature and between
the boiling and bath temperature.
6

Examples:

· The chemical product must not be heated above 24 ºC: Distillation at 24 ºC requires a cooling medium
temperature of 4 ºC or lower and a heating bath temperature of 44 ºC. The optimal parameters are 4/24/44 ºC.
· Distillation of diethyl ether at atmospheric pressure: At atmospheric pressure, diethyl ether has a
Figure 6. A scheme showing energy balance in the distillation process. The energy delivered to the process in the form of heat from the
heating bath is used for the evaporation of the liquid and is subsequently dissipated when the vapor reaches the condenser. boiling point of 35 ºC. To distill this solvent, the cooling medium temperature must be 15 ºC or lower, and the
heating bath temperature should be 55 ºC. So, the optimal parameters are 15/35/55 ºC.
In particular, the temperature values in different parts of the equipment relate to the energy supplied and
dissipated in the process. At a given pressure, one should consider the differences between: Knowing the optimal temperature settings, one can determine the corresponding pressure (see the table in the
Appendix, Chapter 7.1). Alternatively, use Eq. 2 and Eq. 3, introduced earlier, to calculate boiling point or
· The temperature of the heating bath and boiling point. pressure. The Delta 20 rule can then be applied to find the optimal process parameters.
· The boiling point and the temperature of the cooling medium.
Example:
The heating bath provides the energy needed for molecules to transition from liquid to gas. The difference
between the bath temperature and the boiling point determines the heat flux and, therefore, affects the · Evaporation of acetone at 35 ºC: What system pressure should be used? Knowing that Tp = 35 ºC =
distillation rate. Conversely, the condenser must dissipate the energy carried by the gas, which was previously 308.15 K, Ts = 56 ºC = 329.15 K, b = 0.196 (b and Ts can be found in the Table of Solvents in the Appendix,
supplied to the molecules by the heating bath. This means the condenser must be cooler than the vapor. Chapter 7.1), one obtains:
The cooling power of the chiller and the heating power of the bath should match the process requirements.
329.15–308.15
Thus, the temperatures of the cooling medium, the boiling point, and the heating bath must be coordinated. log p = 3.006 – = 2.658 (Eq. 5)
A practical method for this is the Delta 20 Rule, explained in Chapter 4.1.1. Keep in mind that the boiling point 0.196 × 308.15

should be above room temperature.


p = 455 mbar
Monitoring the vapor temperature (corresponding to the boiling point) with a vapor temperature sensor can help
maintain the temperature difference required between the cooling medium and the vapor arriving at the
condenser, ensuring sufficient condensation. A temperature difference of at least 15 °C is recommended.

18 19
The required system pressure is 455 mbar. Therefore, the optimal distillation parameters are 15/35/55 °C. 5.4 Working with a mixture of solvents
One application of rotary evaporators is the evaporation of complete solvent mixtures, which requires special
On the other hand, when knowing the pressure, one could also calculate the boiling point, for example: consideration. Setting the parameters becomes more complicated when working with a mixture of several
solvents. The optimal parameters depend on the chemical composition and ratio of the solvents, with the
· Evaporation of heptane at a pressure of 75 mbar: How high is its boiling point? Knowing that p = 75 mbar, properties of the lower-boiling solvent dominating at the start.
b = 0.200, and Ts = 98 ºC = 371.15 K, one obtains:
The distillation begins using the parameters for the lowest-boiling solvent, which then decreases in amount
371.15 within the mixture. As this happens, the properties of the higher-boiling solvent become dominant. Over time,
Tp = K = 302.69 K = 29.5 ºC (Eq. 6)
(3.600–log75) × 0.200 + 1 the distillation rate will decrease and may eventually reach a standstill. Therefore, the pressure must be carefully
reduced until the lower-boiling solvent has been completely distilled. Afterward, the pressure can be further
The boiling point at 75 mbar is 29.5 ºC. Therefore, the optimal parameters are 10/30/50 ºC. reduced to the optimal level for distilling the higher-boiling solvent. To avoid the need for constant monitoring
and adjustment of the process parameters, an automatic distillation function could be used.
For mixtures with varying solvent concentrations, the distillation parameters need continuous readjustment
throughout the process. A rotary evaporator may require an oil bath to distill higher-boiling solvents, as oil efficiently reaches and
maintains higher temperature values.

5.2 Evaporating flask size When the boiling points of the solvents differ greatly, distillation should stop after the first solvent is distilled, and
The size of the flask used can significantly impact the performance of the process. Using a larger flask the receiving flask should be emptied.
increases the surface area, speeding up the process and reducing the impact of foaming and bumping.
Experiments show that increasing the flask size from 250 mL to 1 L can boost the evaporation speed by a factor
of 2.5–3. Further increasing from 1 L to 4 L can enhance performance by an additional factor of 2. To optimize
performance, immerse the flask deeply and use beaker flasks with a large opening. Beaker flasks save time, are
easy to clean, and simplify product removal at the end of the process.

5.3 Rotation speed


Increasing the rotation speed can optimize the process’s performance and distillation rate. Rotation creates
turbulence within the bath and solvent, significantly enhancing the surface area involved in heat transfer, which
facilitates a more effective evaporation process.

Experimental data indicates that as rotation speed increases, the evaporation rate initially rises but eventually
declines. This occurs because, at high rotation speeds, the contents are pressed against the wall by centrifugal
force and corotate with the flask, reducing turbulence and consequently lowering the evaporation rate.

The optimal turbulence depends on the flask size, the consistency and texture of the solvent/substance, and
the filling quantity. Therefore, the rotation speed should be selected to produce maximum turbulence inside the
flask and the heating bath to achieve maximum evaporation output while ensuring the long life of the rotary
evaporator by limiting spillage, vibration, and mechanical problems. For laboratory evaporators equipped with 1 L
flasks, the optimum rotation speed is typically in the range of 250 to 300 rpm. Smaller flasks perform best at higher
speeds, while larger flasks perform best at lower speeds.

Keep the rotation speed low for drying samples or when working with high-viscosity samples.

20 21
6. Environmental Considerations 7. Conclusion

6.1 The importance of minimizing solvent loss As this guide has shown, distillation has been used for millennia for a wide variety of tasks. Mastering rotary
Solvents may escape into the environment during the distillation process and cause harm. Steps should be evaporation is essential for chemists, as the process is used in so many workflows. You should now have a
taken to limit these emissions and keep them within bounds. good grasp of the basic theory and how to approach and optimize your daily distillations. The following
appendices cover the various solvents used and the working pressures for different vapor temperatures.
One important measure is optimizing the distillation conditions, as discussed in Chapter 4-for example, a They serve as a great starting point for determining the conditions for your daily distillations.
consistent application of the Delta 20 Rule results in a well-balanced distillation.

6.2 When to immerse the flask into the heating bath


In practice, the flask is often immersed before the bath reaches its target temperature. An increase in
temperature at a constant system pressure provides more energy for evaporation, resulting in a higher
distillation output. However, if the distillation parameters are optimized for the lower bath temperature, the
condenser may become overloaded and unable to dissipate the excess heat by the time the bath reaches its
set temperature. Therefore, it is advisable to ensure that the heating bath has reached its final temperature
before immersing the flask. Additionally, immersing the flask only after the apparatus has been evacuated helps
reduce solvent emissions.

Some more advanced rotary evaporators can automatically adjust the pressure as the bath temperature
increases. This feature allows the user to immerse the flask in a cold bath without worrying about overloading
the condenser.

6.3 Equipment considerations


The correct design and equipment selection can help save a lot of solvent. For example, applying the Delta 20
Rule correctly is ineffective if the surface area of the condenser is too small to dissipate the heat. Therefore, it is
important to consider all aspects of the apparatus to ensure an environmentally conscious process.

Some important considerations:

· A well-sealed system: Leakage from the system can cause solvent loss. The pump must compensate for
air penetrating into the apparatus through poorly sealed connectors or seals. Air drawn from the system is
typically saturated with solvent, resulting in a continuous flow of carrier air that transports solvent out of the
system. A well-sealed system with a stable vacuum minimizes such losses.
· Using a secondary condenser: Despite efforts to restrict solvent loss, no system is perfect. Some losses,
particularly with low-boiling solvents, are inevitable. Installing a secondary condenser at the pump output can
condense residual vapors and prevent their release.
· Using an automatic function: The automatic distillation function can help choose optimal conditions for the
given solvent or solvent mixture, minimizing emissions.
· Sufficient surface area of the condenser: The condenser must have enough surface area to dissipate the
heat from the vapor it contacts.
· Correct chiller with sufficient power: The chiller must have adequate power to provide efficient cooling of
the coolant.

22 23
8. References

· Anderegg, G., Nägeli, R., Fässler, T. F.: Praktikum in allgemeiner Chemie I und II. 1995. Laboratorium für
anorganische Chemie der ETH Zürich, Zurich.
· Baehr, H. D.: Thermodynamik. 7th Edition, 1989. Springer Verlag, Heidelberg.
· Bertele, E., Humbel, F. A.: Neukonzeption eines Ofens zur Beheizung kleiner Mengen – insbesondere für die
K-R-Destillation. G-I-T Fachzeitschrift für das Laboratorium, Juni 1973. G-I-T Verlag, Darmstadt.
· Billet, R.: Grundlagen der thermischen Flüssigkeitszerlegung. 1st Edition, 1961. Bibliographisches Institut,
Mannheim.
· BÜCHI Labortechnik: Der automatische Vakuum Kontroller – ein Beitrag zum aktiven Umweltschutz. BÜCHI,
Flawil.
· BÜCHI Labortechnik: Training documents “Grundlagen der Destillation”, “Destillation mit dem
Rotationsverdampfer”, “Umweltschonendes Destillieren”, “Trocknen, Destillieren und Sublimieren im Glasofen
B-580”. Büchi, Flawil.
· BÜCHI Labortechnik: Your Evaporation Guide Operation – Evaporating flask size. BÜCHI, Flawil.
· BÜCHI Labortechnik: Various Operating Instructions. BÜCHI, Flawil.
· E. J. Rothery B.Sc. (1968) Æneas Coffey (1780–1852), Annals of Science, 24:1, 53–71.
· Jian Feng et Guo Li, “Discussions on the History of Technology of Traditional Chinese Alcohol Brewing”,
e-Phaïstos, II-1 | 2013, 87–93.
· Frank Raymond Allchin (1979), “India: the ancient home of distillation?” Man, New Series 14:1:55–63.
· Frank, W., Kutsche, D.: Buchreihe Verfahrenstechnik, (2) Die schonende Destillation. 1st Edition, 1969. Otto
Krausskopf Verlag, Essen.
· Haw, Stephen G. (2012). “Wine, women, and poison.” Marco Polo in China. Routledge. pp. 147–148.
· Kirschbaum, E.: Destillier- und Rektifiziertechnik. 4 th Edition, 1969. Springer Verlag, Heidelberg.
· Krell, E.: Handbuch der Laboratoriumsdestillation. 3rd Edition, 1976. Deutscher Verlag der Wissenschaften,
Berlin.
· Levey, Martin (1959). Chemistry and Chemical Technology in Ancient Mesopotamia. Elsevier. p. 36.
· Matissek, R., Schnepel, F. M., Steiner, G.: Lebensmittelanalytik. 2nd Edition, 1992. Springer Verlag, Heidelberg.
· Moureau, S. (2020). Min al-Kīmiyā’ ad Alchimiam. The Transmission of Alchemy from the Arab-Muslim World
to the Latin West in the Middle Ages. Micrologus: Natura, Scienza E Societa Medievali – Nature, Science and
Medieval Societies, 28.
· Multhauf, Robert P. (1966). The Origins of Chemistry. London: Oldbourne: 204–206.
· Partington, J. R. (January 1947). “History of Alchemy and Early Chemestry*[sic].” Nature. 159 (4029): 81–85.
· Pfalz, A., Keese, R.: Grundoperationen der präparativen organischen Chemie. 5th Edition, 1994. Institut für
Organische Chemie der Universität Bern, Berne.
· www.buchi.com/knowledge/technologies/rotary-evaporation
· Rotary Evaporation | Buchi.com. (n.d.). www.buchi.com.
· Sattler, K.: Thermische Trennverfahren. 1st Edition, 1977. Vogel Verlag, Würzburg.
· Schlünder, E.U., Thurner, F.: Destillation, Absorption, Extraktion. 1st Edition, 1995.
· Friedrich Vieweg & Sohn Verlagsgesellschaft, Braunschweig.
· Society of German Chemists: Sicheres Arbeiten im chemischen Labor. 2nd Edition, 1988. Bundesverband der
Unfallversicherungsträger der öffentlichen Hand eV. (BAGUV), Germany.
· Stapleton, Azo & Hidayat Husain 1927, pp. 338–340.
· Taylor, Frank Sherwood (January 1992). Alchemists, Founders of Modern Chemistry. pp. 38–39.
· Walker, Paul E. (1998). “al-Razi, Abu Bakr Muhammad ibn Zakariyya’ (d. 925)”. In Craig, Edward (ed.).
Routledge Encyclopedia of Philosophy.
· Webster, Charles (2013) [1982]. From Paracelsus to Newton: Magic and the Making of Modern Science.
Cambridge University Press.

24 25
9. Appendices

9.1 Table of solvents 1,1,2,2,-Tetrachloroethane C2H2Cl4 167.9 45.71 146 1.595 0.198
1,1,1,-Trichloroethane C2H3Cl3 133.4 32.50 74 1.339 0.206
Solvent Formula MW Heat of bp ºC Density Constant Tetrachloroethylene C2Cl4 165.8 39.68 121 1.623 0.202
vaporizaton [g/cm3] b Tetrahydrofuran (THF) C 4H 8 O 72.1 31.99 67 0.889 0.192
[kJ/mol] Toluene C7H8 92.2 38.01 111 0.867 0.202
Acetic Acid C2H4O2 60.0 23.36 118 1.049 0.183 Trichloroethylene C2HCl3 131.3 34.54 87 1.464 0.202
Acetone C3 H 6 O 58.1 30.99 56 0.790 0.196 Water H2O 18.0 43.98 100 1.000 0.167
Acetonitrile CH3CN 41.1 32.94 82 0.786 0.195
Xylene (Isomers mixture) C8H10 106.2 0.199
1-Butanol C4H10O 74.1 52.35 118 0.810 0.155
(o) 43.43 144 0.880
tert. Butanol,
(m) 42.65 139 0.864
2-Methyl-2-Propanol C4H10O 74.1 46.69 82 0.789 0.54
(p) 42.40 138 0.861
Chlorobenzene C6H5Cl 112.6 40.97 132 1.106 0.202
Chloroform CHCl3 119.4 31.28 62 1.483 0.203
Cyclohexane C6H12 84.0 33.01 81 0.779 0.206

Diethyl ether C4H10O 74.0 27.10 35 0.714 0.200


Cis-1,2,-Dichloroethylene C2H2Cl2 97.0 - 60 1.284 0.196
Trans-1,2,-Dichloroethylene C2H2Cl7 97.0 - 48 1.257 0.196
Diisopropyl ether C6H14O 102.0 32.12 68 0.724 0.207
Dimethylformamide (DMF) C3H7NO 73.1 46.89 153 0.949 0.180
Dichloromethane,
methylene chloride CH2Cl2 84.9 28.82 40 1.327 0.194
1,4-Dioxane C4H8O2 88.1 38.60 101 1.034 0.200

Ethanol C2H6O 46.0 42.32 79 0.789 0.159


Ethyl acetate C4H8O2 88.0 35.60 77 0.900 0.189

Heptane C7H16 100.2 36.57 98 0.684 0.200


Hexane C6H14 86.2 31.56 69 0.660 0.206

Isopropopanol C3 H8 O 60.1 45.39 82 0.786 0.154


Isoamyl alcohol,
3-Methyl-1-Butanol C5H12O 88.01 55.61 129 0.809 0.158

Methyl ethyl ketone C 4H 8 O 72.1 34.79 80 0.805 0.206


Methanol CH4O 32.0 37.43 65 0.791 0.167

Pentane C5H12 72.1 26.34 36 0.626 0.214


1-Propanol C3 H8 O 60.1 47.45 97 0.804 0.154
Pentachlorethane C2HCl5 202.3 - 162 1.680 0.207
1-Pentanol C5H12O 88.1 57.02 137 0.814 0.158

26 27
9.2 Working pressures for different vapor temperatures of various solvents (mbar) Solvent bp. 20 ºC bp. 30 ºC bp. 40 ºC bp. 50 ºC bp. 60 ºC

1,1,2,2,-Tetrachloroethane 7 12 20 33 52
Solvent bp. 20 ºC bp. 30 ºC bp. 40 ºC bp. 50 ºC bp. 60 ºC
Tetrachloroethylene 20 37 66 114 191
Acetic acid 15 26 44 72 114
Tetrachloroethane 116 181 273 401 577
Acetone 239 369 555 814 atmospheric
Tetrahydrofurane (THF) 161 254 389 581 847
Acetonitrile 85 136 211 319 471
1,1,1,-Trichloroethane 129 200 300 441 632
1-Butanol 7 14 25 45 77
Trichloroethylene 65 102 166 255 381
tert. Butanol 42 76 134 226 371
Toluene 30 49 78 119 179
Chlorobenzene 13 22 36 57 87
Water 24 42 72 120 194
Chloroform 206 316 471 685 atmospheric
Xylene 9 15 25 40 63
Cyclohexane 100 156 237 350 506

Diethy lether 574 855 atmospheric atmospheric atmospheric

Cis-1,2-Dichloroethylene 203 316 477 702 atmospheric

Trans-1,2-Dichloroethylene 321 491 732 atmospheric atmospheric

Dichloromethane, 451 685 atmospheric atmospheric atmospheric


methylene chloride

Diisopropyl ether 162 248 370 538 766

1,4-Dioxan 41 67 106 162 242

Dimethylformamid (DMF) 3 6 10 17 29

Ethanol 57 101 173 285 458

Ethylacetat 94 153 239 365 542

Heptane 47 75 118 181 269

Hexane 158 243 364 530 756

Isoamylalcohol 4 8 15 26 45

Isopropanol 42 77 135 227 373

Methanol 124 210 343 544 124

Methylethylketone (MEK) 105 163 247 364 525

Pentachlorethane 5 8 13 21 34

Pentane 562 818 atmospheric atmospheric atmospheric

1-Pentanol 3 6 11 19 33

1-Propanol 20 37 66 114 191

28 29
9.3 Glossary of terms Recirculating Chiller: A device used to cool equipment and samples in laboratories by continuously
Azeotropic: Refers to a mixture of liquids that maintains a constant boiling point and composition throughout circulating a coolant.
distillation. Azeotropes cannot be separated by simple distillation.
Rectifying Columns: Columns used in distillation and chemical processing to achieve a higher degree of
Baffle plates: These are present in some drying flasks designed to increase surface area, improve heat separation of mixtures by repeated condensation and evaporation.
transfer, or create turbulence, thereby enhancing the drying process.
Reflux Reactions: A technique involving the condensation of vapors and the return of this condensate to the
Boiling Curve: A graph depicting the relationship between the heat flux on the surface of an object system from which it originated.
submerged in a liquid and the excess temperature. “Excess temperature” refers to the difference between the
object’s surface temperature and the saturation temperature of the liquid in which it is immersed. Rotary Evaporation: A technique for efficiently and gently removing solvents from a sample by evaporation.
It involves a rotating flask placed in a heating bath while a vacuum is applied to the system. The rotation
Boiling Point: The temperature at which a liquid’s vapor pressure equals the external pressure, causing the spreads the liquid in a thin film across the surface of the flask, which speeds up the rate of evaporation and
liquid to boil. helps prevent bumping.

Boiling Stones/Chips: Small, porous stones that are added to liquids to promote smooth boiling by providing Superheating: The process of heating a liquid above its boiling point without it actually boiling. This phenomenon
nucleation sites for bubble formation. can occur when the liquid is heated in a very clean and smooth container, which prevents bubble formation.

Collection Flask: A flask used to collect the distillate or evaporated solvent. Thermal Capacity: The amount of heat energy required to raise the temperature of a substance.

Critical Point: At pressures and temperatures above this point, no boundaries exist between the gas and Thermal Conductivity: A measure of a material’s ability to conduct heat.
liquid phases.
Thermal Pump: A process where heat energy is used to drive the movement of vapor, typically in a distillation
Distillation: Separating components or substances from a liquid mixture by selective boiling and or evaporation process.
condensation.
Triple Point: This is the point where a certain pressure and a certain temperature are present at which all three
Drying Flask: A flask used in rotary evaporators for containing the sample being concentrated or dried. phases are in equilibrium. This combination of values for p and T is referred to as the “triple point”.

Evaporation: Evaporation is a type of vaporization that can occur at conditions below the boiling point. Vapor Pressure: The pressure exerted by a vapor in thermodynamic equilibrium with its condensed phases at
a given temperature in a closed system.
Heat Capacity = Thermal Capacity: The amount of heat energy required to raise the temperature of a
substance. Vacuum Controller: A device used to control the vacuum level within rotary evaporators and other laboratory
equipment.
Heat (or Enthalpy) of Vaporization: The amount of heat energy that must be added to a liquid to turn a
specific mass of the liquid into a vapor without a rise in the temperature of the liquid.

Ideal Gas: A theoretical gas composed of molecules that do not attract or repel each other.

Melting Point: The temperature at which the solid and liquid forms of a pure substance can exist in
equilibrium, causing the solid to melt.

Molar Volume: The volume occupied by one mole of a substance at a given temperature and pressure.

Multistage Distillation: A process where a mixture is separated into its components through multiple stages
of evaporation and condensation, with each stage optimized for different boiling points.

Receiving Flask: A flask used to collect the condensed vapor or distillate in a distillation setup.

30 31
Follow us on:

@büchi-labortechnik-ag

@buchilabequipment

@buchilabequipment

@buchilabequipment

@buchilabeqpt

@buchilabequipment

BÜCHI Labortechnik AG Meierseggstrasse 40 Switzerland – 9230 Flawil


T+41 71 394 63 63 [email protected] www.buchi.com

You might also like