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Productivity HandbookFor Industrial Evaporation
Improve your industrial evaporationTips and tricks for the Industrial Rotavapor® R-220 Pro
Achieve best results and performance of your application with handy expert advice. This interactive guide provides a wide range of general recommendations for your industrial evaporation as well as specific suggestions for the Industrial Rotavapor® R-220 Pro. Use your mouse or touchscreen and roll over or click the buttons showing visualizations wherever the sign indicates interaction.
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Setup: The right choice is key Quick and easy description of the Industrial Rotavapor® R-220 Pro
Learn about the major components of the Rotavapor® R-220 Pro by scrolling over the instrument graphic or the description boxes. Using the correct setup for the intended application is the basic prerequisite to achieve best performance and maximum productivity.
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Setup: Glass configurationVariety of glass assemblies for your needs
The choice of the glass configuration strongly depends on the desired application. There are basically two types of configurations: reflux and descending. Both come in different sub-variations, each designed for a specific pur-pose. Scroll over the versions below to learn more about their intended use and further benefits.
RefluxSpecifically designed assembly for distillations under reflux and high boiling solvents.
Low temperture coolingFor example dry ice is used as cooling agent.
Foaming samplesTendency to foam or bump during distillation.
Recrystallizations
System requirements
Applications
Solvent recycling
DescendingUniversal assembly for most standard distillations and low boiling solvents.
Reduced heightHeight restrictions for the instrument exist.
Low boiling pointHighly volatile solvents are used.
Drying samples
Concentration of samples
Reactions under reflux conditions
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D DB2 RD2 RBDB C
Using a reflux configuration with an open reflux valve, the condensate can therefore run out directly to the receiving flask avoiding potential flow back to the evaporation flask as is possible with the descending setup.
Second condenserThe descending assembly can be extended by an additional condenser. The second condenser acts as a post condenser and reduces emissions of low boiling solvents. Hereby, the distillation rate is not affected as the solvent is fully condensed in the first condenser.
Distillate coolerAs the vapor path indicates, the condensed solvent comes close to the hot vapor entering the condenser. This heats up the condensed solvent and may lead to solvents boiling in the receiving flask, particularly if the boiling point is close to ambient temperature. Hence, the distillate cooler cools down the potentially warm solvents.
High boiling solvents may condense in the expansion vessel due to the difference in vapor and ambient temperature. The condensed solvent may flow back into the evaporating flask and can cause a reduction of the distillation rate of up to 5%.
Setup: Glass configurationVariety of glass assemblies for your needs
Descending configurationThe descending glass configuration is applicable for most standard distillations. Due to its design, it is particularly suitable for low boiling solvents as well as for foaming and bumping products. Compared to the reflux configuration, the vapor path of a descending assembly is unidirectional and the condensate is clearly separated from the entering hot vapor.
Reflux configurationThe reflux assembly is particularly designed for reactions under reflux (e.g. extractions or recrystallizations). In addition, the reflux configuration is preferred for high boiling solvents.
The descending setup is ideal for foaming and bumping products and can even be automated with the optional foam sensor.
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Setup: Glass configurationSpecial assemblies and receiving flasks
Glass assembly C (Reflux) Based on the reflux setup, the glass configuration C is equipped with a cold trap instead of a standard condenser. The cold trap can be filled with various cooling mixtures, such as dry-ice/acetone or others. Very low cooling is required if highly volatile solvents are to be collected.
Glass assembly VThe V assembly is a basic glass configuration only available for the Rotavapor® R-220 Pro Essential. Although similar to the reflux setup, the V assembly is not capable of reflux applications (no reflux tap). This assembly fulfills the same specifications as the equivalent of the lab-size Rotavapor®. The 3-way valve can be used as a feed or for aeration.
Receiving vessels All glass assemblies (expect V) are available with a single or dual receiver. The scaled flask has a volume of 10 liter. The receiving flasks can be drained without interrupting the distillation with the use of a shut-off tap. The dual receiver setup further allows for continuous distillations with one flask being drained while distillation takes place in the second flask.
Different boiling pointsDistillation of solvents of different boiling points is made easy with two receiving vessels. Solvent separation is possible without interrupting the distillation by simply collecting the distinct solvents in different flasks. Once the first solvent (lower boiling point) is distilled, close the tap and distill the second solvent with a lower vacuum in the second receiving flask. This prevents the first solvent from boiling in the receiving flask.
This glass configuration is therefore particularly suitable for reactions under reflux and/or solvents of a very low boiling point.
The V assembly is applicable for most distillations, however, not for foaming or bumping products, and only with one receiving flask.
Single receiver Dual receiver
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The distillation rate mainly depends on the available heating power of the system. The heating element of the Rotavapor® and the heat of vaporization of the product to be distilled together define the theoretical distillation rate. In practice, the theoretically determined distillation rate is not achievable as each setup has distinct system characteristics and ideal system parameters are often not feasible. First of all, it is important to understand the basics to evaluate the distillation rate, as well as the system limitations.
Heat of vaporizationEvery solvent has a unique heat of vaporization (also known as heat of evaporation or enthalpy of vaporization). The heat of vaporization is the energy required to transform a given quantity of a substance into a gas at a given pressure. In other words, the heat of vaporization is the energy needed to evaporate a substance. Please find a list of a wide range of solvents in the instruction manuals of all Rotavapors® and vacuum controllers or in relevant literature. The heat of vaporization is usually stated as ∆Hvap and is defined in J/g.
Different heating elementsConsidering that the distillation rate directly depends on the heating power, three heating elements of different capacities are available for the Rotavapor® R-220 Pro. The standard heating unit has a power output of 3600 W, there are more powerful units offering a 4200 W heater and a high performance unit at 6300 W. The chart to the right shows the maximum achievable distillation rate of acetone using each version of the Rotavapor® R-220 Pro.
Important system parameters The maximum distillation rate is calculated assuming ideal conditions for a fast distillation. Several system parameters influence the distillation rate which should be considered. For the Rotavapor® R-220 Pro these are:
Water: ∆Hvap = 2261 J/g = 2261 Ws/gEnergy required to evaporate 1 kg of water:
Heating capacity R-220 Pro = 3600 WTheoretical distillation rate:
Effectiveness: 70% 4 kg/h
Max. distillation rate of water: 4 l/h
Calculation
2261 W · s · h · 1000 gg · 3600 s · kg
3600 W628 Wh
628 Wh
5.7 kg/h=
=
• Maximum rotation speed• Temperature difference between bath
and boiling point of about 40 °C• Cooling temperature at least 10 °C
(better 20 °C) below vapor temperature • Adequately high cooling flow (outlet
temperature about 5 °C below vapor temperature)
• Cooling medium: water• Strong vacuum source
Ideal setup
However, for various reasons the ideal system parameters may often not be realistic, such as:• maximum rotation is not possible (foaming or
bumping product)• unable to achieve the required temperature
difference (thermosensitive product)• the solvent to be distilled is usually not pure• oil is used as heating medium (lower heat
transfer properties than water)
3600 W
30
15
25
10
20
5
04200 W 6300 W
Dis
tilla
tion
rate
(L/h
)
Maximum distillation rate of acetone
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Efficiency: Increase the performance Distillation rate and influencing parameters
Temperature difference between bath and vapor (°C)
5
10
15
20
25
10 20 30 40Dis
tilla
tion
rate
of
acet
one
(L/h
)
Acetone distillation as a function of
In order to achieve the maximum distillation rate at a specific heating power, it is important to consider the following critical system parameters; temperature difference, rotation speed and flask size as well as flask immersion.
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Efficiency: Increase the performance Distillation rate and influencing parameters
Cooling may not have an equally strong effect on the distillation rate as the temperature difference and the rotation have. However, it is necessary to provide sufficient cooling to facilitate complete condensation. Poor cooling results in less condensation and in vapor escaping the system through the vacuum pump. Solvent emissions in the lab pose serious health and environmental risks and should be avoided. Further, insufficient cooling may result in a reduced recovery rate.
ExamplesMaximum distillation rates of selected solvents
SolventMaximum
distillation rate in liter / hour
Ethyl acetat 25.5Heptane 35.4Hexane 37.2Isopropyl alcohol 16.53-Methyl-1-butan 18.8Methylethylketone 23.8Methanol 9.3Pentane 37.9n-Propylalcohol 14.31,1,2,2-Tetrachloroethane 231,1,1-Trichloroethylen 23.8Toluene 24.4Trichloroethylene 26.4Water 4Xylene 26.7
Crucial cooling parametersTwo parameters are important when it comes to cooling; the coolant flow rate and the temperature difference between coolant and vapor. It is vital to maintain sufficient coolant flow throughout the system. For the Rotavapor® R-220 Pro 120-150 L/h are required whereas 200-250 L/h are adequate for the Rotavapor® R-250. In terms of temperature difference between coolant and vapor, approximately 10 °C are sufficient.
SolventMaximum
distillation rate in liter / hour
Acetic acid 12.4Acetone 20.7Acetonitrile 13.6n-Pentanol 18.7Benzene 18.8n-Butanol 18Chloroform 23.1Cyclohexane 29.8Dichloromethane 18.3Diethylether 32.61,2-Dichloroethane 21.9Diisopropylether 39.3Dioxane 21.5Dimethylformamide 16.5Ethanol 13
9 © 2017 BÜCHI Labortechnik AG
Efficiency: Increase the perfomance Cooling influence
Further automation accessories:
The Rotavapor® R-220 Pro offers various levels of automation; built-in features of the standard R-220 Pro already allow for certain degree of automation while a fully automated system requires some additional accessories. The following modes are included in any Rotavapor® R-220 Pro model:
• Timer: Automatic switch into standby and rotation stop after a set time. Further, the heating is stopped and the heating bath is lowered.
• Method: Program and store different methods or SOPs.• App: Process supervision by smartphone or tablet. Push notifications if the distillation is complete or an error
occurs. Simply download the free app and connect to the Rotavapor® via the internet.
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Automation: Get more out of your system Minimize user interaction
Additional safety add-ons:
The Rotavapor® R-220 Pro includes various safety aspects as standard features, such as plastic coated glass parts ("P+G" certificate) or the snap flange coupling for the evaporation flask. Depending on its use and environment, additional measures may be necessary to further protect the system.
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Safety: Always well-protected Included and additional safety features
The Rotavapor® R-220 Pro is designed for easy and safe operation. For even further comfort, a range of additional accessories are availble.
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Comfort: Further accessories Make your life easier
In some applications, it is required to cool down the evaporating flask. The customer requesting a solution had so far added ice for cooling, however, this was neither precise nor practical. An inlet cooling coil is connected to the recirculating chiller allowing for exact bath temperature control, also below room temperature.
Inlet cooling coil
In addition to the coated glass parts, this customer asked for more metal protection of the glass parts. Special protection for all cylindrical glass parts was designed and custom made. The material used is a combination of a metal net and the BÜCHI plastic coating.
Additional protection
This customer expressed the desire to wash down the assembly by additional ports on the top of the Rotavapor®. Three large openings with caps were added to the glass part.
Additional glass ports
Dealing with light sensitive products is challenging. For the Rotavapor® R-220 Pro, a straighforward solution could be found. Amber coating is applied to the evaporating flask to protect the product. Branding of the coating guarantees equally good performance as the standard flask.
Amber glass flask
Contact us to discuss your requirements and ideas. We are always happy to help and develop ideal customer solutions tailored to your needs. In general, the following components can be modfied: • glass parts (type and number of connections,
dimensions or even new parts)• mechanical parts (depending on suppliers)• electronic and software modifications (time-
and test intensive)
Much more
Customization of various system components are easily possible. The following represents a small selection of customized parts, however, many more have been realized.
Several glass assemblies are available at reduced height, however, this customer requested an even shorter setup. BÜCHI glass assemblies are made in house. Hence, adaptations to special demands are easily possible. Further height reduction was achieved by redimensioning the glass assembly.
Modified glass assembly
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Comfort: Customize to your needs We are happy to help
My product is...
However, many products require adjustments to achieve best results. The following section lists the most common challenges in concentration applications and according solutions given by experts.
The most common use of the industrial Rotavapor® is the concentration of products. As wide as the range of products to be processed by the Rotavapor®, as various are the methods to do so. Generally, the goal is to achieve a gentle concentration of the product in the shortest possible time. For regular and trouble-free samples (e.g. heat resistant, no tendency to foam or bump during distillation), the following settings are recommended: • bath temperature: 60 °C• vacuum: recommended pressure according to the solvent list (b.p. of 40 °C)• cooling: 20 °C or lower• rotation speed: maximum
14 © 2017 BÜCHI Labortechnik AG
Applications: Concentration Recommendations for your application
My product...
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Applications: Concentration Recommendations for your application
Purification or solvent recycling Unlike in the concentration use, the main interest in purification applications lies in the solvent and not the product. Here, the goal is to purify or recycle a solvent with minimal loss. In general, the recommendations are equivalent to those given in the concentration section, however, the focus is somewhat different.
DryingAnother important application is drying of a product. The product to be dried in the flask may already be concentrated or can even be a slurry. The main goal is to dry the product with minimal loss in the shortest time possible. Generally, the recommendations are equivalent to those given in the concentration section, however, with a slightly different focus.
Other applicationsNumerous applications can be performed using an Industrial Rotavapor®. The tips given above help to optimize almost any application. Test your application on a lab-size Rotavapor® and scale it up.
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Applications: Purification & Drying Recommendations for your application
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Appendix: Solvent list Important parameters
Solvent Formula Molar mass in g/
mol
Heat of vaporiza-tion in J/g
Boiling point at
1013mbar in °C
Density in g/cm3
Recommended vacuum for a
boiling point of 40°C in mbar
Acetic acid C2H4O2 60.0 695 118 1.049 44
Acetone CH3H6O 58.1 553 56 0.790 556
Acetonitrile C2H3N 41.1 853 82 0.780 208
n-amylalcohol, n-pentanol C5H12O 88.1 595 37 0.814 11
Benzene C6H6 78.1 548 80 0.877 236
n-butanol C4H10O 74.1 620 118 0.810 25
tert. butanol
(2-methyl-2-Propanol)
C4H10O 74.1 590 82 0.789 130
Chlorobenzene C6H5Cl 112.6 377 132 1.106 36
Chloroform CHCl3 119.4 264 62 1.483 474
Cyclohexane C6H12 84.0 389 81 0.779 235
Diethylether C4H10O 74.0 389 35 0.714 850
1,2-dichloroethane C2H4Cl2 99.0 335 84 1.235 210
1,2-dichloroethylene(cis) C2H2Cl2 97.0 322 60 1.284 479
1,2-dichloroethylene(trans) C2H2Cl2 97.0 314 48 1.257 751
DiisoPropyl ether C6H14O 102.0 318 68 0.724 375
Dioxane C4H8O2 88.1 406 101 1.034 107
Dimethyl-formamide (DMF) C3H7NO 73.1 73.1 153 0.949 11
Dimethylsulfoxide C2H6OS 78.1 678 189 1.104 4
Ethanol C2H6O 46.0 879 79 0.789 175
Ethylacetate C4H8O2 88.1 394 77 0.900 240
Heptane C7H16 100.2 373 98 0.684 120
Hexane C6H14 86.2 368 69 0.660 360
IsoPropylalcohol C3H8O 60.1 699 82 0.786 137
Isoamylalcohol
(3-methyl-1-butanol)
C5H12O 88.1 595 129 0.809 14
Methylethylketone C4H8O 72.1 473 80 0.805 243
Methanol CH4O 32.0 1227 65 0.791 337
Methylene chloride,
dichloromethane
CH2CI2 84.9 373 40 1.327 850
Pentane C5H12 72.1 381 36 06.26 850
n-Propylalcohol C3H8O 60.1 787 97 0.804 67
Pentachloroethane C2HCl5 202.3 201 162 1.680 13
Pyridine C5H5N 79.1 511 115 0.980 61
1,1,2,2-tetra-chloroethane C2H2Cl4 167.9 247 146 1.595 20
1,1,1-trichloroethane C2H3Cl3 133.4 251 74 1.339 300
Tetra-chloro-ethylene C2Cl4 165.8 234 121 1.623 53
THF
(tetrahydrofurane)
C4H8O 72.1 72.1 67 0.889 374
Toluene C7H8 92.2 427 111 0.867 77
Trichloroethylene C2HCl3 131.3 264 87 1.464 183
Water H2O 18.0 2261 100 1.000 72
Xylene (mixture)
o-xylene
m-xylene
p-xylene
C8H10
C8H10
C8H10
C8H10
106.2
106.2
106.2
106.2
389
144
139
138
0.880
0.864
0.861
25
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Appendix: Solvent list Recommended vacuum for different boiling points:
Solvent Boiling point0 °C
Boiling point10 °C
Boiling point20 °C
Boiling point30 °C
Boiling point40 °C
Boiling point50 °C
Boiling point60 °C
Acetic acid 4 8 15 26 44 72 113
Acetone 91 150 239 370 556 815 Atmos.
Acetonitrile 29 50 83 134 208 315 465
n-amylalcohol, n-pentanol 1 1 3 6 11 19 33
Benzene 36 60 98 155 236 352 511
n-butanol 2 4 7 14 26 47 80
tert. butanol
(2-methyl-2-Propanol)
11 23 43 78 136 231 378
Chlorobenzene 4 7 13 22 36 56 86
Chloroform 77 126 199 306 457 665 947
Cyclohexane 40 66 107 166 252 372 536
Diethylether 242 382 585 871 Atmos Atmos Atmos
1,2-dichloroethane 30 51 83 132 203 304 444
1,2-dichloroethylene(cis) 77 127 204 317 479 705 Atmos
1,2-dichloroethylene(trans) 129 209 330 505 751 Atmos Atmos
DiisoPropyl ether 63 104 164 251 375 545 776
Dioxane 14 25 42 68 108 165 246
Dimethyl-formamide (DMF) 1 2 3 6 10 17 28
Dimethylsulfoxide 0 1 1 2 4 7 12
Ethanol 16 31 58 102 175 289 463
Ethylacetate 33 57 95 153 240 366 544
Heptane 16 28 47 77 120 183 273
Hexane 60 99 156 241 360 525 750
IsoPropylalcohol 11 23 43 78 136 231 378
Isoamylalcohol
(3-methyl-1-butanol)
1 2 4 9 16 29 49
Methylethylketone 38 64 103 160 243 359 518
Methanol 38 70 122 206 337 534 824
Methylene chloride,
dichloromethane
178 288 451 685 Atmos. Atmos. Atmos.
Pentane 245 377 563 819 Atmos. Atmos. Atmos.
n-Propylalcohol 5 10 20 37 67 115 193
Pentachloroethane 1 3 5 8 13 21 34
Pyridine 7 13 22 38 61 95 146
1,1,2,2-tetra-chloroethane 2 4 7 12 20 32 50
1,1,1-trichloroethane 49 81 129 200 301 442 634
Tetra-chloro-ethylene 6 12 20 33 53 83 126
THF
(tetrahydrofurane)
53 91 148 234 360 539 788
Toluene 10 17 29 48 76 118 177
Trichloroethylene 22 39 65 106 167 257 383
Water 6 13 23 42 72 120 194
Xylene (mixture) 3 5 9 15 25 40 63
(Atmos. = atmospheric pressure)
19 © 2017 BÜCHI Labortechnik AG
Appendix: Glass configuration table Overview of glass assemblies
Applications D D2 DB2 DB RB R C
Foaming samples • • • •
Low boiling point (highly volatile) • • • • •
Reflux distillation • • •
Low temperature cooling (e.g. dry ice) •
Reduced height • • •
Recrystallizations • • •
Drying samples • • • • • • •
Solvent recycling • • • • • • •
Concentration of samples • • • • • • •
Reactions under reflux conditions • • •
D DB2 RD2 RBDB C
Low boiling points and/or foaming products
Minimum emissions Reflux reactions
Reduced height
High boiling points Very low boiling point
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