Buchi Pure C-805 Operation Manual

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Pure Chromatography Instrument C-805 Operation Manual
11594236 | B en
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Imprint
Product Identification: Operation Manual (Original) Pure Chromatography Instrument C-805 11594236
Publication date: 12.2020
BÜCHI Labortechnik AG Meierseggstrasse 40 Postfach CH-9230 Flawil 1
E-Mail: quality@buchi.com
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experi­ence, especially with respect to structure, illustrations and technical details.
This manual is copyrighted. Information from it may neither be reproduced, distributed, or used for com­petitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without prior written agreement is also prohibited.
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BÜCHI Labortechnik AG Table of contents
Table of contents
1 About this document........................................................................................................... 6
1.1 Warning notices in this document........................................................................................................ 6
1.2 Symbols............................................................................................................................................... 6
1.2.1 Warning symbols .....................................................................................................................6
1.2.2 Mark-ups and symbols.............................................................................................................6
1.3 Trademarks.......................................................................................................................................... 7
1.4 Connected devices .............................................................................................................................. 7
2 Safety....................................................................................................................................8
2.1 Proper use ........................................................................................................................................... 8
2.2 Use other than intended ...................................................................................................................... 8
2.3 Staff qualification ................................................................................................................................. 8
2.4 Residual risks ...................................................................................................................................... 9
2.4.1 Faults during operation ............................................................................................................ 9
2.4.2 Malware infection due to connections with other devices or network ...................................... 9
2.4.3 Damage to the internal memory due to incorrect shutting down of the instrument..................9
2.5 Personal protective equipment ............................................................................................................ 9
2.6 Modifications........................................................................................................................................ 9
3 Product description...........................................................................................................10
3.1 Description of function ....................................................................................................................... 10
3.2 Configuration ..................................................................................................................................... 11
3.2.1 Front view ..............................................................................................................................11
3.2.2 Rear view ...............................................................................................................................11
3.2.3 Connections on gradient valve...............................................................................................13
3.3 Type plate.......................................................................................................................................... 13
3.4 Scope of delivery ............................................................................................................................... 14
3.5 Technical data ................................................................................................................................... 14
3.5.1 Pure Chromatography Instrument C-805...............................................................................14
3.5.2 Ambient conditions.................................................................................................................15
3.5.3 Material .................................................................................................................................. 15
4 Transport and storage ......................................................................................................16
4.1 Transport ........................................................................................................................................... 16
4.2 Storage .............................................................................................................................................. 16
4.3 Lifting the instrument ......................................................................................................................... 17
5 Installation..........................................................................................................................18
5.1 Installation site................................................................................................................................... 18
5.2 Before installation .............................................................................................................................. 18
5.3 Securing against earthquakes ........................................................................................................... 18
5.4 Establishing electrical connections.................................................................................................... 19
5.5 Establishing solvent connection......................................................................................................... 19
5.6 Assigning solvent to solvent lines...................................................................................................... 20
5.7 Assembling the waste bottle.............................................................................................................. 21
5.8 Assembling the solvent bottle platform (option)................................................................................. 21
Operation Manual Pure Chromatography Instrument C-805 iii
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Table of contents BÜCHI Labortechnik AG
6 Operation............................................................................................................................23
6.1 Control panel ..................................................................................................................................... 23
6.1.1 Layout of control panel...........................................................................................................23
6.1.2 Enter value.............................................................................................................................24
6.1.3 Menu bar................................................................................................................................25
6.1.4 Conditions panel .................................................................................................................... 27
6.1.5 Collection panel .....................................................................................................................28
6.1.6 Gradient panel .......................................................................................................................29
6.1.7 Run panel...............................................................................................................................30
6.1.8 Solvent selection panel..........................................................................................................31
6.1.9 Detector selection panel ........................................................................................................31
6.1.10 Slope detection panel ............................................................................................................32
6.2 Editing a method................................................................................................................................ 32
6.2.1 Selecting a cartridge (Flash mode)........................................................................................32
6.2.2 Selecting a solvent.................................................................................................................33
6.2.3 Editing the gradient................................................................................................................34
6.2.4 Editing the wavelength for the UV detector............................................................................36
6.2.5 Editing the fraction collection criteria .....................................................................................37
6.2.6 Editing the fraction collection time .........................................................................................38
6.2.7 Editing the vapor sensor sensitivity........................................................................................39
6.2.8 Saving a method....................................................................................................................40
6.3 Editing a solvent ................................................................................................................................ 40
6.3.1 Adding a new solvent.............................................................................................................40
6.3.2 Deleting a solvent ..................................................................................................................41
6.4 Tasks during a separation ................................................................................................................. 42
6.4.1 Injecting a sample into the flash system ................................................................................ 42
6.4.2 Installing and removing a cartridge........................................................................................43
6.4.3 Inserting the fraction collection tray .......................................................................................44
6.4.4 Selecting an existing method.................................................................................................44
6.4.5 Selecting values on the dialog box Sample Loading .............................................................45
6.5 Performing a Flash separation using a method................................................................................. 45
6.5.1 Preparing the instrument........................................................................................................45
6.5.2 Starting Flash separation using a method .............................................................................45
6.5.3 Changings during a separation..............................................................................................46
6.5.4 Ending a Flash separation ..................................................................................................... 46
6.5.5 Shutting down the instrument ................................................................................................46
6.6 Performing a Flash separation manually ........................................................................................... 46
6.6.1 Preparing the instrument........................................................................................................46
6.6.2 Starting Flash separation manually........................................................................................47
6.6.3 Changings during a separation..............................................................................................47
6.6.4 Ending a Flash separation ..................................................................................................... 48
6.6.5 Shutting down the instrument ................................................................................................48
6.7 Identifying fractions............................................................................................................................ 48
6.7.1 Identifying fractions by peak ..................................................................................................48
6.7.2 Identifying fractions per vial ...................................................................................................49
6.8 Importing and exporting data............................................................................................................. 49
6.8.1 Printing a run report ............................................................................................................... 49
6.8.2 Sending data to USB .............................................................................................................50
6.8.3 Sending PDF to USB ............................................................................................................. 50
7 Cleaning and servicing .....................................................................................................51
7.1 Regular maintenance work................................................................................................................ 51
7.2 Carrying out a data backup................................................................................................................ 52
7.3 Calibrating the display ....................................................................................................................... 52
7.4 Cleaning the check valve................................................................................................................... 52
7.5 Cleaning the instrument..................................................................................................................... 53
iv Operation Manual Pure Chromatography Instrument C-805
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BÜCHI Labortechnik AG Table of contents
8 Help with faults ..................................................................................................................55
8.1 Faults, possible causes and solutions (general)................................................................................ 55
8.2 Faults, possible causes and solutions (cartridge).............................................................................. 55
8.3 Faults, possible causes and solutions (solvent delivery)................................................................... 55
8.4 Faults, possible causes and solutions (fraction collection)................................................................ 56
8.5 Faults, possible causes and solutions (detection) ............................................................................. 57
8.6 Error messages ................................................................................................................................. 57
8.7 Resetting the Fraction collector arm.................................................................................................. 61
9 Taking out of service and disposal.................................................................................. 62
9.1 Taking out of service.......................................................................................................................... 62
9.2 Disposal............................................................................................................................................. 62
9.3 Returning the instrument ................................................................................................................... 62
10 Appendix ............................................................................................................................63
10.1 Spare parts and accessories ............................................................................................................. 63
10.1.1 Accessories............................................................................................................................63
10.1.2 Spare parts ............................................................................................................................64
10.1.3 Tools and adapter kits............................................................................................................64
10.1.4 Tubes .....................................................................................................................................64
10.1.5 Wear parts .............................................................................................................................65
10.2 Folder locations ................................................................................................................................. 65
10.3 Finding out separation conditions with the navigator......................................................................... 65
10.3.1 Open the navigator ................................................................................................................65
10.3.2 TLC Silica...............................................................................................................................66
10.3.3 LC-C18...................................................................................................................................67
10.3.4 LC-Transfer............................................................................................................................68
Operation Manual Pure Chromatography Instrument C-805 v
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1 | About this document BÜCHI Labortechnik AG
1 About this document
This operation manual is applicable for all variants of the instrument.
Read this operation manual before operating the instrument and follow the instruc­tions to ensure safe and trouble-free operation.
Keep this operation manual for later use and pass it on to any subsequent user or owner.
BÜCHI Labortechnik AG accepts no liability for damage, faults and malfunctions re­sulting from not following this operation manual.
If you have any questions after reading this operation manual:
u Contact BÜCHI Labortechnik AG Customer Service.
https://www.buchi.com/contact
1.1 Warning notices in this document
Warning notices warn you of dangers that can occur when handling the device. There are four danger levels, each identifiable by the signal word used.
Signal word Meaning
DANGER Indicates a danger with a high level of risk which could result in
death or serious injury if not prevented.
WARNING Indicates a danger with a medium level of risk which could result in
CAUTION Indicates a danger with a low level of risk which could result in mi-
NOTICE Indicates a danger that could result in damage to property.
1.2 Symbols
The following symbols are displayed in this operation manual or on the device:
1.2.1 Warning symbols
Symbol Meaning
death or serious injury if not prevented.
nor or medium-severity injury if not prevented.
General warning
Dangerous electrical voltage
Flammable substances
Laser class 1
1.2.2 Mark-ups and symbols
NOTE
This symbol draws attention to useful and important information.
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BÜCHI Labortechnik AG About this document | 1
R This character draws attention to a requirement that must be met before the in-
structions below are carried out.
u This character indicates an instruction that must be carried out by the user.
ð This character indicates the result of a correctly carried out instruction.
Mark-up Explanation
Win dow Software Windows are marked-up like this.
Tab Tabs are marked-up like this.
Dia log Dialogs are marked-up like this.
[Button] Buttons are marked-up like this.
[Field names] Field names are marked-up like this.
[Menu / Menu item] Menus or menu items are marked-up like this.
Status Status is marked-up like this.
Signal Signals are marked-up like this.
1.3 Trademarks
Product names and registered or unregistered trademarks that are used in this docu­ment are used only for identification and remain the property of the owner in each case.
1.4 Connected devices
In addition to these operating instructions, follow the instructions and specifications in the documentation for the connected devices.
Operation Manual Pure Chromatography Instrument C-805 7/70
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2 | Safety BÜCHI Labortechnik AG
2 Safety
2.1 Proper use
The instrument is designed and built for laboratories.
The instrument can be used for the following tasks:
PurificationSeparation of one or more compounds from a mixture
2.2 Use other than intended
Use of any kind other than that described in Chapter2.1 "Proper use", page8 and any application that does not comply with the technical specifications (See Chap­ter3.5 "Technical data", page14) constitutes use other than intended.
In particular, the following applications are not permissible:
Use of the instrument in areas which require explosion-safe instruments.Use of the instrument with solvents containing peroxides.Use the instrument for production purposes.
2.3 Staff qualification
Unqualified persons are unable to identify risks and are therefore exposed to greater dangers.
The device may only be operated by suitably qualified laboratory staff.
These operating instructions are aimed at the following target groups:
Users
Users are persons that meet the following criteria:
They have been instructed in the use of the device.They are familiar with the contents of these operating instructions and the applica-
ble safety regulations and apply them.
They are able on the basis of their training or professional experience to assess
the risks associated with the use of the device.
Operator
The operator (generally the laboratory manager) is responsible for the following as­pects:
The device must be correctly installed, commissioned, operated and serviced.Only suitably qualified staff may be assigned the task of performing the operations
described in these operating instructions.
The staff must comply with the local applicable requirements and regulations for
safe and hazard-conscious working practices.
Safety-related incidents that occur while using the device should be reported to the
manufacturer (quality@buchi.com).
BUCHI service technicians
Service technicians authorized by BUCHI have attended special training courses and are authorized by BÜCHI Labortechnik AG to carry out special servicing and repair measures.
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BÜCHI Labortechnik AG Safety | 2
2.4 Residual risks
The device has been developed and manufactured using the latest technological ad­vances. Nevertheless, risks to persons, property or the environment can arise if the device is used incorrectly.
Appropriate warnings in this manual serve to alert the user to these residual dangers.
2.4.1 Faults during operation
If a device is damaged, sharp edges, moving parts or exposed electrical wires can cause injuries.
u Regularly check device for visible damage. u If faults occur, switch off the device immediately, unplug the power cord and in-
form the operator.
u Do not continue to use devices that are damaged.
2.4.2 Malware infection due to connections with other devices or network
Connections with other devices or a network can cause a malware infection to the in­strument.
u Install antivirus software and firewall on the instrument before connecting it to
other devices or network.
2.4.3 Damage to the internal memory due to incorrect shutting down of the instrument
Incorrect shutting down of the instrument can cause damage to the internal memory.
u Shut down the instrument as described. See Chapter6 "Operation", page23
2.5 Personal protective equipment
Depending on the application, hazards due to heat and/or corrosive chemicals may arise.
u Always wear appropriate personal protective equipment such as safety goggles,
protective clothing and gloves.
u Make sure that the personal protective equipment meets the requirements of the
safety data sheets for all chemicals used.
2.6 Modifications
Unauthorized modifications can effect safety and lead to accidents.
u Use only genuine BUCHI accessories, spare parts and consumables. u Carry out technical changes only with prior written approval from BUCHI. u Only allow changes to be made by BUCHI service technicians.
BUCHI accepts no liability for damage, faults and malfunctions resulting from unau­thorized modifications.
Operation Manual Pure Chromatography Instrument C-805 9/70
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3 | Product description BÜCHI Labortechnik AG
Gradient valve
UV
detector
Fraction
collection
Solvent 2
Solvent 1
Pump
Sample
introduction
Cartridge
3 Product description
3.1 Description of function
The instrument is a purification device designed to purify complex samples by flash chromatography.
Flash chromatography has the ability to separate gram size samples in short pe-
riod.
The instrument allows:
2 different solventsInjection of liquid or solid sampleSeparation on a cartridgeIdentifying the compounds by UVCollecting the desired fractions
Instrument schematic:
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BÜCHI Labortechnik AG Product description | 3
5
7
1
2 3
4
6
3.2 Configuration
3.2.1 Front view
Fig.1: Front view
1 Control panel 2 RFID reader 3 On/Off switch 4 USB Port 5 Cartridge holder 6 Flash pump 7 Fraction collection bay
3.2.2 Rear view
NOTE
All electrical connections are not limited energy.
Operation Manual Pure Chromatography Instrument C-805 11/70
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3 | Product description BÜCHI Labortechnik AG
9
8
7 6
1
2
3
4
5
Fig.2: Rear view
1 Ventilation slot 2 Gradient valve
(See Chapter3.2.3 "Connections on gradient valve", page13 )
3 Signal connection
4 LAN port
(for external air supply) 5 Power supply connection 6 Fuse 7 On/Off master switch 8 USB ports 9 Type plate
(See Chapter3.3 "Type plate",
page13
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BÜCHI Labortechnik AG Product description | 3
3
2
1
Buchi Labortechnik AG 9230 Flawil / Switzerland
Type: xxx SN: 10xxxxxxxx Volt: xxx-xxx VAC Frequ.: xx Hz Power: xxxx W Built: 20xx
Made in Switzerland
6
5
4
1
3
2
7
8
9
10
9
3.2.3 Connections on gradient valve
Fig.3: Connections on the gradient valve
1 Waste line 2 Solvent line 2 3 Solvent line 1
3.3 Type plate
The type plate identifies the instrument. The type plate is located at the rear of the in­strument.
Fig.4: Type Plate
1 Company name and address 2 Instrument name 3 Serial number 4 Input voltage range 5 Frequency 6 Power consumption maximum 7 Year of manufacture 8 Product code 9 Approvals 10 Symbol for "Do not dispose of as
household waste"
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3 | Product description BÜCHI Labortechnik AG
3.4 Scope of delivery
NOTE
The scope of delivery depends of the configuration of the purchase order.
Accessories are delivered as per the purchase order, order confirmation, and deliv­ery note.
3.5 Technical data
3.5.1 Pure Chromatography Instrument C-805
Pure C-805
Dimension (W x D x H)
Weight 24 kg
Clearance on each side of the instrument 200 mm
Power consumption 350 W
Connection voltage 100 - 240 V ± 10 %
365 x 570 x 680 mm
Frequency 50 - 60 Hz
Fuse 4 A
Overvoltage category II
Pollution degree 2
IP Code IP 20
Solvents 2
USB port 3
LAN port (RJ45)
RFID reader (racks)
RFID reader (cartridges)
Fraction collector bay closed
Lighted fraction collector bay Yes
Vapor sensor Yes
Pump Flash Mode
1
Yes
Yes
Pure C-805
Gradient binary
Pressure range 0 - 50 bar
Flow rate 0 - 250 mL/min
Flow rate accuracy < 2 %
Functional principle self-priming
Specification 3 pistons
radial arranged
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BÜCHI Labortechnik AG Product description | 3
UV Detector
Pure C-805
UV wavelength range 200 - 400 nm
Light sources Deuterium
Detector DAD
3.5.2 Ambient conditions
For indoor use only.
Max. altitude above sea level 2000 m
Ambient temperature 5‒40°C (25°C)
No maximum performance above 25°C
Maximum relative humidity 80% for temperatures up to 31°C
Storage temperature max. 45 °C
3.5.3 Material
Component Materials of construction
Housing Powder coated steel 1.4301
Fraction collection bay PMMA / PET
Pump head PEEK
Pump cover PP
Pump excenter housing Aluminum
Tubings FEP
Fitting POM
Valve screw fitting POM
Ferrule ETFE
Cone ring POM
Radial seal PTFE
Pistons Ceramic
Operation Manual Pure Chromatography Instrument C-805 15/70
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4 | Transport and storage BÜCHI Labortechnik AG
4 Transport and storage
4.1 Transport
NOTICE
Risk of breakage due to incorrect transportation
u Make sure that all parts of the device are safely packed in such a way as to pre-
vent breakage, ideally in the original box.
u Avoid sharp movements during transit.
u After transportation, check the device for damage. u Damage that has occurred in transit should be reported to the carrier. u Keep packing for future transportation.
4.2 Storage
u Make sure that the ambient conditions are complied with (see Chapter3.5 "Tech-
nical data", page14).
u Make sure a clean solvent like ethanol or isopropanol is in the pump. u Wherever possible, store the device in its original packaging. u After storage, check the device, all seals and tubing for damage and replace if
necessary.
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4.3 Lifting the instrument
WARNING
Danger due to incorrect transportation
The possible consequences are crushing injuries, cuts and breakages.
u The instrument should be transported by two persons at the same time. u Lift the instrument at the points indicated.
u Lift the instrument – this requires two persons each lifting at one of the points indi-
cated on the bottom of the instrument.
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5 | Installation BÜCHI Labortechnik AG
1
5 Installation
5.1 Installation site
The installation site must meet the following requirements:
The installation site has a firm, level surface.The installation site meets the specifications according to the technical data (e.g.
weight, dimension, etc.). See Chapter3.5 "Technical data", page14
The installation site has no obstacles (e.g. water taps, drains, etc.).The installation site is not exposed to external thermal loads, such as direct solar
radiation.
The installation site has a own mains outlet socket for the instrument.The installation site has enough space that cables / tubes can be routed safely.The installation site allows that the power supply can be disconnected at any time
in an emergency.
The installation site is not exposed to increased electromagnetic emissions.
Electromagnetic fields in the frequency range between 200 to 300 MHz can cause the instrument to operate incorrectly.
The installation site meets the requirements of the safety data sheets for all sol-
vents and samples used.
5.2 Before installation
NOTICE
Instrument damage due to switching it on too early.
Switching on the instrument too early after transportation can cause damage.
u Climatize the instrument after transportation.
5.3 Securing against earthquakes
The instrument has an earthquake fixing point to protect the device against falling.
Fig.5: Securing against earthquakes
1 Fixing point
u Tie the lashing mount to a fixed point using strong cord or a wire.
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BÜCHI Labortechnik AG Installation | 5
5.4 Establishing electrical connections
NOTE
Observe the legal requirements when connecting the instrument to the power supply.
4 Use additional electrical safety features (e.g., residual-current circuit breakers) to
comply with local laws and regulations.
The power supply must fulfil the following conditions:
1. Provide the mains voltage and frequency specified on the type plate of the instru­ment.
2. Be designed for the load imposed by the instruments connected.
3. Be equipped with suitable fuses and electrical safety features.
4. Be equipped with proper earthing.
NOTICE
Risk of property damage and diminished performance due to use of un­suitable power cables.
The power supply cables supplied with the product by BUCHI precisely match the re­quirements of the device. If other power cables that do not meet those requirements are used, the device may be damaged and/or its performance diminished.
u Use only the power supply cables supplied with the product or ordered separately
from BUCHI.
u If using any other power supply cables, make sure that they match the specifica-
tions on the type plate.
u Make sure that all connected devices are earthed. u Plug the power cable into the connection on the instrument. See Chapter3.2
"Configuration", page11
u Plug the mains plug into the mains outlet socket.
5.5 Establishing solvent connection
NOTICE
Solvent bottles on top of the instrument.
Solvent bottles on top of the instrument can cause property damages.
u Locate the solvent bottles next to the instrument. u Use the optional solvent bottle platform.
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5 | Installation BÜCHI Labortechnik AG
Precondition:
R Make sure that the instrument is not con-
nected to the power supply.
u Attach all solvent lines to the instrument. Con-
nections see Chapter3.2 "Configuration", page11
u Put the other end of the solvent line into the
solvent bottle.
u Assign the solvent to the solvent lines. See
Chapter5.6 "Assigning solvent to solvent lines", page20
5.6 Assigning solvent to solvent lines
Navigation path
Tools Solvent Loading
Precondition: R The solvent bottle is connected to the instrument. See Establishing solvent con-
nection
R The solvent you wish to use is part of the solvent library. See Chapter6.3 "Editing
a solvent", page40
u Navigate to the Sol ven t Loadi ng dialog according to the navigation path.
ð The display shows the dialog box S olv ent Loa din g.
u Tap the drop-down list next to Line 1.
ð The display shows a drop-down list with selectable solvents.
u Select the solvent which is connected to solvent line 1.
ð The solvent for Line 1 is assigned. ð The drop-down list closes.
u Repeat the solvent selection for each line. u Activate the checkbox next to the line you wish to prime. u Tap the button [Auto Prime]. u Wait till priming finished. u Tap the button [Close].
ð All lines are assigned with solvents. ð The dialog box closes.
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BÜCHI Labortechnik AG Installation | 5
5.7 Assembling the waste bottle
NOTICE
Waste bottle on top of the instrument
Waste bottle on top of the instrument can cause property damages.
u Make sure that there is a decline between the connection on the instrument and
the waste bottle.
u Put the waste line into the waste bottle.
5.8 Assembling the solvent bottle platform (option)
NOTICE
Waste bottle on top of the instrument
Waste bottle on top of the instrument can cause property damages.
u Do not place the waste bottle an the solvent bottle platform.
u Turn the solvent bottle platform upside down.
Operation Manual Pure Chromatography Instrument C-805 21/70
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5 | Installation BÜCHI Labortechnik AG
u Attach the drain line adapter to the solvent
bottle platform
u Attach the drain line to the drain line adapter.
u Attach the solvent bottle platform to the instru-
ment with screws.
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BÜCHI Labortechnik AG Operation | 6
5
9
8
7
1
2
3
4
6
6 Operation
6.1 Control panel
6.1.1 Layout of control panel
Fig.6: Display
No. Description Function
1 [Menu] bar Shows the available menus.
See Menu bar
2 [Conditions] panel Shows the properties and default set-
3 [Wavelength] panel Shows available wavelengths and scan
4 [Collection] panel Shows collection options.
5 [Gradient] panel Shows chromatograms and gradient ta-
6 [Run] panel Shows the operation options.
7 [Solvent selection] panel Shows selectable solvents.
tings of the installed column / cartridge. See Conditions panel
options.
See Chapter6.1.5 "Collection panel", page28
ble. See Gradient panel
See Chapter6.1.7 "Run panel", page30
See Chapter6.1.8 "Solvent selection panel", page31
Operation Manual Pure Chromatography Instrument C-805 23/70
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6 | Operation BÜCHI Labortechnik AG
No. Description Function
8 [Detector settings] panel Shows selectable detector options and
its settings. See Detector selection panel
9 [Slope detection] panel Shows selectable slope detection op-
tions. See Chapter6.1.10 "Slope detection
panel", page32
6.1.2 Enter value
Enter numbers
u Tab on an entry field.
ð The display shows a dialog box with a numeric input box.
u Enter the value. u Tap the button [OK].
ð The value is saved. ð The dialog box closes.
Enter names
u Tab on an entry field.
ð The display shows a dialog with an alphanumeric input box.
u Enter the value. u Tap the button [OK].
ð The value is saved. ð The dialog box closes.
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BÜCHI Labortechnik AG Operation | 6
6.1.3 Menu bar
The following menus are available:
Menu Submenu / Action Explanation
[File] [Open Method] Load an existing method.
See Chapter6.4.4 "Selecting an existing method", page44
[Save Method] Save an edited method.
See Chapter6.2.8 "Saving a method", page40
[Save Method as] Save an edited method with another
name. See Chapter6.2.8 "Saving a method",
page40
[Open Run] Load a completed run.
[Print Run Report] See Chapter6.8.1 "Printing a run report",
page49
[Print PDF to USB] See Chapter6.8.3 "Sending PDF to
USB", page50
[Exit] Exit the Pure software to Windows® sys-
tem software.
[Shut down] The instrument shuts down.
[View] [Setup] If [Setup] is marked up, the instrument is
in setup mode.
[Run in Progress] If [Run in Progress] is marked, a run is in
progress.
[Past Run] If [Past Run] is marked up, the instru-
ment is in the past run mode.
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Menu Submenu / Action Explanation
[Tools] [Solvent Loading] Assign a solvent to a solvent line.
See Chapter5.6 "Assigning solvent to solvent lines", page20
[Solvent Definition] Define solvents.
See Chapter6.3 "Editing a solvent", page40
[Vapor Sensors and Limits] Edit the vapor sensor sensitivity.
See Chapter6.2.7 "Editing the vapor sensor sensitivity", page39
[Configuration] System configurations.
[Calibration and Defaults] Calibrate the screen.
Set time and date.
Reset UV lamp.
Set alarms
[Manual control] Maintenance actions.
See Chapter7.5 "Cleaning the instru­ment", page53
See Chapter8.7 "Resetting the Fraction collector arm", page61
[NP<>RP] Change back and forth between normal
phase and reverse phase
[Product Services] Override max. pressure limit for car-
tridges.
[UV Baseline] Adjust the baseline to zero during a run.
[Language] Select a language.
[Service] BUCHI service technicians only
[Help] [About] The display shows instrument details.
[View Manual] The display shows the Operation man-
ual.
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6.1.4 Conditions panel
1 Information button
(Information about the selected col­umn)
The conditions area contains the following settings:
Action Option Explanation
[Column] Automatic via RFID Shows the name of the cartridge in-
stalled in the instrument.
[Flow Rate] Enter value Edit the default flow rate.
[Duration Units] Choice of the duration
type
The following types are available: minutes / column volumes
[Equilibration] Enter value Indicates the period of time or num-
ber of column volumes that the mo­bile phase flows through the column before the sample is injected.
[Run Length] Enter value According to the current operation
enter the time for the separation.
According to the current operation enter the number of column volumes required for the separation.
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1
6.1.5 Collection panel
1 Tray number
The collection vial matrix corresponds to the trays. The trays are detected by the auto recognition. The estimated number of vials required for the separation is displayed below the solvent usage list in the lower left corner of the Setup window.
The fraction collection area contains the following settings:
Action Option Explanation
Fraction collection options
Select value The following options are available:
[Collect Peaks] / [Collect All] / [Col­lect None]
[Per-Vial Volume] View / Enter value The following values are change-
able: [Peak] / [Non-Peaks]
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6.1.6 Gradient panel
Edit the gradient and see separation details.
NOTE
According to the instrument status different options are available.
Action Option Explanation
[Table] Create a gradient See Editing the gradient in tabular
mode
[Navigator] Finding out Flash sepa-
ration conditions
[UV scan details] View Shows the following charts:
[Zoom] Function Zoom the graph.
[Options] Select values Graph options.
[Edit] Select between the op-
tions
See Chapter10.3 "Finding out sepa­ration conditions with the navigator", page65
3D (UV / Time/ Wavelength)2D (Time / Wavelength)Absorption maximaAll scan maxima
The graph is in edit mode. See Edit­ing the gradient in graphic mode
[View] The graph is in view mode.
(No changes possible)
[Zoom] Zoom the graph.
[Gradient hold] Function The gradient is held at the current
solvent ratio.
The gradient continues to the origi­nal end-point.
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Action Option Explanation
[Auto gradient hold] Function The gradient will be held every time
the signal goes over the set thresh­old.
6.1.7 Run panel
The run panel shows available functions according to the current operation.
Symbol Description Meaning
[Start] Is used to start the run or re-start the
actual operation if the system has been paused.
[Stop] Is used to terminate the operation of
the system.
[Pause] Is used to stop the actual operation.
If the system is paused due to an er­ror, this button will change to yellow.
[Advance] Is used to advance to the next step
during equilibration.
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6.1.8 Solvent selection panel
Select solvents for a separation. See Chapter6.2.2 "Selecting a solvent", page33
6.1.9 Detector selection panel
Action Option Explanation
[UV] Enable / Disable
Select value / Enter value
Action enabled: Low / High Enter values for threshold
Action disabled: No selection
[Threshold Detec­tion]
Enter value The threshold defines the value
above the fraction collector starts to collect fractions.
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6.1.10 Slope detection panel
Action Option Explanation
[Slope detection] Enable / Disable Action enabled:
6.2 Editing a method
6.2.1 Selecting a cartridge (Flash mode)
NOTE
The automatic reading of the cartridge information can only be done with specific BUCHI RFID tagged cartridges.
4 The indication for recognizing the cartridge is a sound.
Fraction collection triggered by slope
Action disabled: No detection
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1
1 Information button
(Information about the selected col­umn)
Navigation path
Conditions panel
u Navigate to the Con dit ions se lec tio n panel according the navigation path. u Tap the input box next to [Column].
ð The display shows a menu with selectable cartridges.
u Select the cartridges you wish to use.
6.2.2 Selecting a solvent
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Navigation path
Solvent selection panel
Precondition: R The required solvents lines are connected and assigned. See Chapter5.6 "As-
signing solvent to solvent lines", page20
u Navigate to the Sol ven t selec tio n panel according the navigation path. u Tap the drop-down list next to A: .
ð The display shows a drop-down list with the assigned solvents.
u Tap the required solvent.
ð The solvent is selected ð The drop-down list closes.
u Select more solvents for the mobile phase according to your needs.
6.2.3 Editing the gradient
The composition of the mobile phase as a function of time can be indicated by enter­ing the gradient. Solvent lines can be used to generate a binary gradient.
Editing the gradient in tabular mode
The following settings are available:
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Action Option Explanation
[Min] Enter value Enter the time until the value in col-
umn [% 2nd] is reached.
[Solvents] Select value Select solvent line combinations.
[% 2nd] Enter value Enter the percentage rate for the
second solvent.
Navigation path
Gradient panel
u Navigate to the Gra die nt panel according the navigation path. u Tap the button [Table].
ð The display shows the dialog G rad ient Ta ble .
u Tap the cell for [Min].
ð The display shows a dialog box with a numeric input box.
u Enter the time. u Tap the button [OK]. u Tap the cell for [% 2nd].
ð The display shows a dialog box with a numeric input box.
u Enter the percentage for the second solvent. u Tap the button [OK]. u Tap the button [Close].
ð The gradient is saved ð The dialog Gradient table closes ð The G rad ien t panel shows the set gradient.
Add additional lines to the Gradient table
u Tap the number field (e.g. 1►).
ð The display shows a drop-down list with selectable actions.
u Select if the line should be added above or below the selected line.
ð A line is added.
Deleting lines from the Gradient table
u Tap the number field (e.g. 1►).
ð The display shows a drop-down list with selectable actions.
u Select delete.
ð The line is deleted.
Editing the gradient in graphic mode
Navigation path
Gradient panel
u Navigate to the Gra die nt panel according the navigation path. u Tap the button [Edit].
ð The Display shows a drop-down list.
u Select [Edit].
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Add steps to the Gradient graphic
u Tap on the line at the time for which you want to edit the gradient and drag it to the
desired %B, then release.
Deleting steps from the Gradient graphic
u To remove a step, drag the point to the baseline or to any gray area around the
graph until a red X is visible, then release.
6.2.4 Editing the wavelength for the UV detector
Status Checkbox Explanation Explanation
On The instrument collects fractions.
Monitoring The instrument records the data from the
UV detector but does not collect the frac­tions.
Off The instrument does not record data
from the UV detector and does not col­lect fractions.
Navigation path
Wavelength selection panel
Precondition: R The UV detector is selected.
u Navigate to the Wav ele ngth panel according the navigation path. u Activate the checkbock next to [UV]. u Tap the input box next to [UV].
ð The display shows a dialog box with a numeric input box.
u Enter a value for the wavelength. u Tap the button [OK].
ð The dialog box closes. ð The wavelength is saved.
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6.2.5 Editing the fraction collection criteria
1 Identifier
The following fraction collection criteria are available:
Criteria Meaning
[Collect Peaks] The instrument collects fractions if one detector signal is
above the set threshold.
[Collect All] The instrument collects all the fractions regardless of de-
tection signals.
[Collect None] The instrument collects no fractions.
NOTE
[Peak] and [Non-Peaks] default is the maximum volume of the vial.
Navigation path
Collection panel
u Tap the radio button next to criteria you wish to use.
ð The criteria is selected.
u Tap the input box next to [Peak].
ð The display shows a dialog box with a numeric input box.
u Enter a the volume you wish to collect. u Tap the button [OK].
ð The dialog box closes. ð The value for the volume is saved.
u Tap the input box next to [Non-Peaks].
ð The display shows a dialog box with a numeric input box.
u Enter the volume you wish to collect.
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u Tap the button [OK].
ð The dialog box closes.
6.2.6 Editing the fraction collection time
Program Collect allows to turn off fraction collection for a specific time.
The fraction collector defaults to collect the full run length unless the values from Pro­gram Collect override the collection.
Navigation path
Gradient panel
u Navigate to the Gra die nt panel according the navigation path. u Tap the button [Program collect].
ð The display shows the dialog P rog ram col lec t.
u Tap the input box.
ð The display shows a dialog box with a numeric input box.
u Enter the time. u Tap the button [OK].
ð The time is saved. ð The dialog box closes.
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Add additional lines to the program collection
u Tap the number field (1►).
ð The display shows a drop-down list with selectable actions.
u Select if the line should be added above or below the selected line.
ð A line is added.
Deleting lines from the program collection
u Tap the number field (1►).
ð The display shows a drop-down list with selectable actions.
u Select delete.
ð The line is deleted.
6.2.7 Editing the vapor sensor sensitivity
The vapor sensor detects solvent concentration in the ambient air.
The following sensitivity limits are available:
Sensitivity Meaning
High Used for non-volatile solvents
Medium Compromise between the low and high setting
Low Used for volatile or semi-volatile solvents
Off The vapor sensor is off
Navigation path
Tools Vapor Sensor and Limits
u Navigate to the Vap or Sensors dialog according to the navigation path.
ð The display shows the dialog box V apo r Senso rs.
u Tap the drop-down list next [Vapor alarm sensitivity]. u Select the sensitivity value you wish to use. u Tap the button [Close].
ð The dialog box closes.
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6.2.8 Saving a method
Navigation path
File Save Method as
u Navigate to the Sav e M ethod a s dialog according to the navigation path.
ð The display shows the dialog box S ave Met hod as .
u Tap the input box [Enter method name].
ð The display shows a dialog with an alphanumeric input box.
u Enter the name of the method. u Tap the button [OK].
ð The dialog box closes.
u Tap the button [OK].
ð The method is saved. ð The dialog box closes.
6.3 Editing a solvent
6.3.1 Adding a new solvent
Navigation path
Tools Solvent Definition
u Navigate to the Sol ven t Defin iti on dialog according to the navigation path.
ð The display shows the dialog box S olv ent Def ini tio n.
u Tap the button [Add Solvent].
ð The display shows the dialog box S olv ent.
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u Tap the input box next to [Name].
ð The display shows a dialog with an alphanumeric input box.
u Enter the name for the solvent. u Tap the button [OK].
ð The dialog box closes.
u Tap the input box next to [Info].
ð The display shows a dialog with an alphanumeric input box.
u Enter information to the solvent according to your requirements. u Tap the button [OK].
ð The dialog box closes.
u Tap the button [Verify Solvents].
ð The display shows the dialog box S olv ent Ver ifi cat ion .
u Select solvent group for the defined solvent. u Tap the button [OK].
ð The dialog box closes. ð The solvent is added.
u Tap the button [Close].
ð The dialog box S olv ent Def ini tio n closes.
6.3.2 Deleting a solvent
Navigation path
Tools Solvent Definition
u Navigate to the Sol ven t Defin iti on dialog according to the navigation path.
ð The display shows the dialog box S olv ent Def ini tio n.
u Select the solvent you wish to delete. u Tap the button [Delete Solvent]. u Answer the secure question with [Yes].
ð The solvent is deleted.
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6.4 Tasks during a separation
6.4.1 Injecting a sample into the flash system
Injecting a sample into the cartridge
u Remove the solvent line from the cartridge.
u Connect the syringe to the cartridge.
u Press the plunger.
u Disconnect the syringe.
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u Connect the solvent line.
6.4.2 Installing and removing a cartridge
NOTE
Removing is done in reverse sequence.
NOTE
Instead of a cartridge a bypass can be installed.
NOTE
The automatic reading of the cartridge information can only be done with specific BUCHI RFID tagged cartridges.
4 The indication for recognizing the cartridge is a sound.
u Open the solvent line at the point indicated.
u Hold the cartridge above the RFID reader. u Wait until the instrument has taken over the
cartridge data.
u Attach the cartridge to the cartridge holder.
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1
2
u Attach the solvent lines to the cartridge.
6.4.3 Inserting the fraction collection tray
NOTE
By default the first available tube on each tray is reserved for waste.
Changing the setting. See Chapter6.4.5 "Selecting values on the dialog box Sample Loading", page45
1 Tab 2 Optical sensor slot
u Place the collection tubes in the collection tray. u Place the trays in the fraction collector bay. u Make sure that the tab is in the optical sensor slot.
6.4.4 Selecting an existing method
Navigation path
File Open Method
u Navigate to the Ope n M ethod dialog according to the navigation path.
ð The display shows the dialog box O pen Met hod .
u Select the method you wish to use. u The display highlights the selected method black. u Tap the button [OK].
ð The method is selected. ð The dialog box closes.
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6.4.5 Selecting values on the dialog box Sample Loading
The display shows the dialog box Sam ple Lo adin g during the starting phase of a separation.
The following settings are possible:
Action Explanation
[Lower flow rate for specified time after in­jection]
Reduce flow rate for a specified period, when the pressure increases significantly at the start of the run after sample injection.
[Flush 2nd solvent at
Automatically cleaning the system and column.
the end of the run]
[Override Start Vial] Select the start vial according to your needs.
6.5 Performing a Flash separation using a method
6.5.1 Preparing the instrument
Time required: approx. 30 sec.
Precondition: R All commissioning operations have been completed. See Chapter5 "Installation",
page18
u Switch the On/Off master switch to On. u Tap the On/Off switch.
ð The instrument is starting up.
6.5.2 Starting Flash separation using a method
Precondition: R The instrument is prepared. See Chapter6.5.1 "Preparing the instrument",
page45
R The required solvents are connected and assigned. See Chapter5.6 "Assigning
solvent to solvent lines", page20
R The sample is prepared.
R The waste bottle is empty.
u Open the protection shield. u Place the fraction collection trays inside the instrument. See Chapter6.4.3 "Insert-
ing the fraction collection tray", page44
u Close the protection shield. u Open an existing method. See Chapter6.4.4 "Selecting an existing method",
page44
u Tap the button [OK]. u Tap the button [Start] on the Run panel. u According the requirements adjust the file name. u Tap the button [OK].
ð The display shows the dialog box S amp le Load ing .
u According the requirements adjust the settings. See Chapter6.4.5 "Selecting val-
ues on the dialog box Sample Loading", page45
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u Follow the instructions on the display.
ð Installing the cartridge. See Chapter6.4.2 "Installing and removing a car-
tridge", page43
ð Introducing the sample into the system. See Chapter6.4.1 "Injecting a sample
into the flash system", page42
6.5.3 Changings during a separation
NOTE
Parameters that can be edited are highlighted in green
Possibilities to edit the gradient during a separation:
Change the gradient. See Editing the gradient in graphic modeHold the gradient. See Gradient panelAuto gradient hold. See Gradient panel
6.5.4 Ending a Flash separation
NOTE
The separation extends automatically by 5 minutes if the baseline at the end of the separation is not below the set threshold.
Precondition: R The display shows the dialog box Se para tio n E nd.
u According to the requirements extend the separation time by 5 minutes.
Precondition: R The display shows the dialog box Ru n co mpl ete d.
u Follow the instructions on the display.
ð Removing the cartridge. See Installing and removing a cartridge
6.5.5 Shutting down the instrument
Navigation path
File
Precondition: R The separation process has ended.
u Purge the instrument with purging solvent. See Chapter7.5 "Cleaning the instru-
ment", page53
u Navigate to the [File] menu via the navigation path. u Tap the action [Shut down]. u Confirm the secure question with [Yes].
ð The instrument is shutting down.
6.6 Performing a Flash separation manually
6.6.1 Preparing the instrument
Time required: approx. 30 sec.
Precondition: R All commissioning operations have been completed. See Chapter5 "Installation",
page18
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u Switch the On/Off master switch to On. u Tap the On/Off switch.
ð The instrument is starting up.
6.6.2 Starting Flash separation manually
Precondition: R The instrument is prepared. See Chapter6.6.1 "Preparing the instrument",
page46
R The required solvents are connected and assigned. See Chapter5.6 "Assigning
solvent to solvent lines", page20
R The sample is prepared.
R The waste bottle is empty.
u Open the protection shield. u Place the fraction collection trays inside the instrument. See Chapter6.4.3 "Insert-
ing the fraction collection tray", page44
u Close the protection shield. u Select a cartridge. See Chapter6.2.1 "Selecting a cartridge (Flash mode)",
page32
u Tap the drop-down list next to A: on the Sol ven t Selec tio n panel.
ð The display shows a drop-down list with the assigned solvents.
u Tap the required solvent.
ð The solvent is selected ð The drop-down list closes.
u Select more solvents for the mobile phase according to your needs. u Edit the gradient according to your needs. See Chapter6.2.3 "Editing the gradi-
ent", page34
u Select the sample collection in the Col lec tion panel. See Chapter6.2.5 "Editing
the fraction collection criteria", page37
u Select the collection criteria in the Col lec tion cr ite ria panel. u Tap the button [Start] on the Run panel.
ð The display shows the dialog box S amp le Load ing .
u According the requirements adjust the settings. See Chapter6.4.5 "Selecting val-
ues on the dialog box Sample Loading", page45
u Follow the instructions on the display.
ð Installing the cartridge. See Installing and Removing a cartridge ð Introducing the sample into the system. See Chapter6.4.1 "Injecting a sample
into the flash system", page42
6.6.3 Changings during a separation
NOTE
Parameters that can be edited are highlighted in green
Possibilities to edit the gradient during a separation:
Change the gradient. See Editing the gradient in graphic modeHold the gradient. See Gradient panelAuto gradient hold. See Gradient panel
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6.6.4 Ending a Flash separation
NOTE
The separation extends automatically by 5 minutes if the baseline at the end of the separation is not below the set threshold.
Precondition: R The display shows the dialog box Se para tio n E nd.
u According to the requirements extend the separation time by 5 minutes.
Precondition: R The display shows the dialog box Ru n co mpl ete d.
u Follow the instructions on the display.
ð Removing the cartridge. See Installing and removing a cartridge
6.6.5 Shutting down the instrument
Navigation path
File
Precondition: R The separation process has ended.
u Purge the instrument with purging solvent. See Chapter7.5 "Cleaning the instru-
ment", page53
u Navigate to the [File] menu via the navigation path. u Tap the action [Shut down]. u Confirm the secure question with [Yes].
ð The instrument is shutting down.
6.7 Identifying fractions
6.7.1 Identifying fractions by peak
Fig.7: Identifying fractions
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Navigation path
Gradient panel
Precondition: R A separation is finished.
u Navigate to the Gra die nt panel according the navigation path. u Tap the peak with the target value.
ð The C oll ection panel shows the corresponding vial.
6.7.2 Identifying fractions per vial
Fig.8: Identifying fractions
Navigation path
Collection panel
Precondition: R A separation is finished.
u Navigate to the Col lec tion panel according the navigation path. u Tap the target vial.
ð The G rad ien t panel shows the corresponding peak.
6.8 Importing and exporting data
6.8.1 Printing a run report
Navigation path
File Print Run Report
Precondition: R The instrument is in past run mode.
u Navigate to the Pri nt Run Rep ort dialog according to the navigation path.
ð The display shows the Windows® print dialog.
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u Select your printer. u Tap the button [OK].
ð The report is printed.
6.8.2 Sending data to USB
Navigation path
Run panel
Precondition: R The instrument is in past run mode.
u Connect a USB storage device to the instrument. u Navigate to the Run panel according the navigation path. u Tap the button [Data to USB].
ð The instrument saves an Excel file to the USB storage device.
u Confirm the complete message.
ð The data is stored.
6.8.3 Sending PDF to USB
Navigation path
Run panel
Precondition: R The instrument is in past run mode.
u Connect a USB storage device to the instrument. u Navigate to the Run panel according the navigation path. u Tap the button [PDF to USB].
ð The instrument saves a PDF file to the USB storage device.
u Confirm the complete message.
ð The data is saved.
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7 Cleaning and servicing
NOTE
Users may only carry out the servicing and cleaning operations described in this sec­tion.
Any servicing and repair work which involves opening up the casing may only be car­ried out by BUCHI service technicians.
u Use only genuine BUCHI consumables and spare parts in order to ensure correct
operation of the device and preserve the warranty.
7.1 Regular maintenance work
Component Action Frequency
Pumps and valves u Purge the instrument with purging solvent.
See Chapter7.5 "Cleaning the instru­ment", page53
Daily
Tubing u Check for leaks. If a leak is observed, re-
solve the issue before continuing.
Fittings u Inspect fittings; if solid material is de-
posited on a fitting, clean and tighten (re­place) the fitting before continuing.
Drain lines u Check all drain lines to ensure that liquid
can flow through them to the waste con­tainer
Waste bottle u Empty the waste bottle Daily
Cartridge holder u Check the holding capability of the car-
tridge holder.
u If necessary, replace the hock-and-loop
strap.
Filters u Check the filters in the solvent bottles and
clean if necessary.
Fittings u Check and if necessary tighten the fitting
that secures the tubing from the mobile phase reservoir manifold to the inlet check valve housing
Data u Perform a data backup Weekly
Daily
Daily
Daily
Weekly
Weekly
Weekly
Casing u Wipe down the casing with a damp cloth.
u If heavily soiled, use ethanol or a mild de-
tergent.
Warning symbols u Check that the warning symbols on the in-
strument are legible.
u If they are dirty, clean them.
Display u Wipe down the display with a damp cloth. Monthly
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Weekly
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7.2 Carrying out a data backup
Navigation path
File Exit
u Navigate to the Exi t dialog according to the navigation path. u Confirm the secure question.
ð The Pure software is shutting down. ð The display shows a Windows® system.
u Connect a USB storage device to the instrument. u Open the Windows® Explorer. u Navigate to the data you wish to backup. See Chapter10.2 "Folder locations",
page65
u Copy the needed data to the USB storage devices.
7.3 Calibrating the display
Navigation path
Tools Calibration and Defaults
u Navigate to the Cal ibr ation a nd Def aul ts dialog according to the navigation
path.
u Tap the button [Calibrate]. u Follow the instructions on the display.
7.4 Cleaning the check valve
NOTE
Most check valve problems can be solved by pumping a strong solution of liquid lab­oratory grade detergent through the check valves at a rate of 20 mL/min for one hour.
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BÜCHI Labortechnik AG Cleaning and servicing | 7
Pumping detergent through the check valves
Materials needed:
Liquid Laboratory DetergentIsopropanol/Water (50/50) or Methanol/Water (50/50)
Navigation path
Tools Manual Control Column Flushing...
Precondition: R A bypass is installed. See Installing and removing a column
u Navigate to the Col umn Flushi ng dialog according to the navigation path.
Sonicate the check valve
Materials needed:
Open-end wrench, ½”, 9/16" x 5/16"Torque wrench
u Switch the On/Off master switch to Off. u Disconnect the mobile phase tubing from the inlet (bottom) of the pump head us-
ing the 9/16” open-end wrench.
u Disconnect the mobile phase outlet tubing from the top of the pump head using
the 5/16” open end wrench.
u Remove both check valve housings from the pump head using the ½” open-end
wrench.
ð The check valve capsule is accessible.
u Sonicating the check valve for 10 min in the appropriate solvent. u Install the check valve. u Install the check valve housings back into the pump head. u Tighten the check valve housing to 75 inch pounds with the ½” torque wrench.
7.5 Cleaning the instrument
Navigation path
Tools Manual Control Column Flushing...
Precondition: R A purging solvent is assigned to the instrument. See Chapter5.6 "Assigning sol-
vent to solvent lines", page20
Operation Manual Pure Chromatography Instrument C-805 53/70
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7 | Cleaning and servicing BÜCHI Labortechnik AG
u Install a bypass. See Installing and removing a column u Navigate to the Col umn Flushi ng dialog according to the navigation path. u Enter the required data according to your needs.
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BÜCHI Labortechnik AG Help with faults | 8
8 Help with faults
8.1 Faults, possible causes and solutions (general)
Malfunction Possible cause Solution
The instrument does not power up
Power is not being supplied to the system
u Verify that the power cord
is plugged in.
u Make sure that the voltage,
amperage and frequency meet the instrument speci­fications.
u Make sure that both power
switches are switched on.
u Verify that the fuse wire is
not broken and fuses are correctly installed in the in­strument.
System shuts down automatically
Major fluctuations in line power are present
u Connect system to a Unin-
terrupted Power Supply line.
The touch screen is not responsive
The touch screen is out of cal­ibration
u Recalibrate the touch
screen.
8.2 Faults, possible causes and solutions (cartridge)
Malfunction Possible cause Solution
Cartridge is not de­tected
RFID tag is not facing the RFID reader
u Turn cartridge so that RFID
tag faces RFID reader.
RFID tag is bad u Use new cartridge.
8.3 Faults, possible causes and solutions (solvent delivery)
Malfunction Possible cause Solution
No solvent flow Empty solvent bottle u Refill the solvent bottle.
Pump not primed u Prime the pump.
u Remove the check valve
and clean it by sonicating the check valve in IPA.
u If sonication does not work
replace the check valve with a new check valve.
Air bubbles in solvent line u Prime the pump.
Pump seals worn out u Replace the pump seals.
Pulsation of pump Open or close time of the inlet
or outlet valves are not correct
Residues in solvent
Sealing abrasion outlet valve
Operation Manual Pure Chromatography Instrument C-805 55/70
u Rinse the pump module
with high flowrate with ethanol or hot distilled wa­ter.
u Change check valves.
Page 56
8 | Help with faults BÜCHI Labortechnik AG
Malfunction Possible cause Solution
Inconsistent solvent flow
Loose fitting/air leak into the pump
u Find the loose fitting be-
tween mobile phase reser­voir manifold and pump in­let fitting and tighten it up.
Liquid leak/pump seals worn out
Pump head temperature reaches solvent boiling tem­perature, causing the pump to lose prime and stop flow (this is likely to occur when running
u Fix the leak/replace the
pump seals.
u Premix the solvents to re-
duce solvent volatility.
u Place the highly volatile
solvent bottle in an ice
bath to eliminate boiling. methods with highly volatile solvents such as diethyl ether and methylene chloride)
System pump pres­sure is higher than expected
Blocked solvent lines u Find the blocked lines and
replace it.
Over-tightened fitting u Loosen the fitting or re-
place it.
Blocked columns or fluidic path
u Locate the component that
caused the blockage, re-
pair, or replace the compo-
nent.
Leaks Fitting connection not tight u Find the loose fitting and
tighten it up.
Damaged solvent line u Find the damaged solvent
line and replace it.
Pump not running Pump sensor cable becomes
disconnected
u Locate the cable and re-
connect to the pump sen-
sor.
Pump power cable becomes disconnected
u Locate the power cable
and reconnect to the main
board or to the pump.
Incorrect flow path Incorrect fluidic connections
to/from the mode switching
u Check/correct the fluidic
connections. valve
8.4 Faults, possible causes and solutions (fraction collection)
Malfunction Possible cause Solution
Liquid not being collected in fraction tubes
Liquid not centered in fraction tube
Incorrect fraction collection settings
Fraction collector is not cali­brated
u Verify that fraction collec-
tion information is set prop-
erly.
u Recalibrate the fraction
collector.
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BÜCHI Labortechnik AG Help with faults | 8
Malfunction Possible cause Solution
Fraction collector (FC) arm does not move
Fraction collector arm did not home properly
Fraction collector arm motor is
u Reset the Fraction collec-
tor arm.
u Tighten the motor coupler.
slipping
Fraction collector arm is ob­structed
u Check for cable or burr in
the fraction collector arm path and remove any ob­struction.
Tray not detected RFID tag is bad u Put another tray into the
same position to see if it is recognized to confirm the cause.
u Replace RFID tag.
8.5 Faults, possible causes and solutions (detection)
Malfunction Possible cause Solution
No UV signal UV light burned out u Replace the UV light.
Low UV signal Dirty flow cell u Clean the flow cell.
8.6 Error messages
Error message Possible cause Solution
Instrument Alarm: Solvent pump: Communication to the pump cannot be established.
Serial communication dis­turbed
u Restart the instrument.
Instrument Alarm: Solvent pump: Mo­tor overloading.
Instrument Alarm: Solvent pump: Mo­tor regulation error.
Instrument Alarm: Solvent pump: Power supply error.
Instrument Alarm: Solvent pump: Sol­vent pump motor fan is not working.
Instrument Alarm: UV detector: Com­munication error occurred.
- u Contact BUCHI Customer Service.
Hardware error solvent pump u Contact BUCHI Customer
Service.
Hardware error solvent pump u Contact BUCHI Customer
Service.
Hardware error fan solvent pump
Serial communication dis-
u Contact BUCHI Customer
Service.
u Restart the instrument.
turbed
Operation Manual Pure Chromatography Instrument C-805 57/70
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8 | Help with faults BÜCHI Labortechnik AG
Error message Possible cause Solution
Instrument Alarm: UV detector: Bad block of High Volt­age (HV) generator
Lamp defect u Check the lamp and restart
No lamp
Hardware error UV detector
instrument.
u Contact BUCHI Customer
Service. for lamp or discon­nected lamp or bad lamp.
Instrument Alarm: UV detector: Bad power supply of lamp heater volt­age.
Instrument Alarm: UV detector: Bad power supply of lamp anodic volt­age.
Instrument Alarm: UV detector: Bad power supply of de­tector analog or digital voltage.
Instrument Alarm: UV detector: 4th cycle of lamp igni­tion fails.
Instrument Alarm: UV detector: Lamp spontaneously douse during unit working.
Hardware error UV detector u Contact BUCHI Customer
Service.
Hardware error UV detector u Contact BUCHI Customer
Service.
Hardware error UV detector u Contact BUCHI Customer
Service.
Lamp defect u Check the lamp and restart
instrument.
Lamp defect u Check the lamp and restart
instrument.
Instrument Alarm: UV detector: Lamp
Hardware error UV detector. u Contact BUCHI Customer
Service. ignition fails after short douse in AU­TOZERO function and repeated High Voltage impulse and heater cycle fails too.
Instrument Alarm: UV detector: Bad
Lamp defective/ Flow cell dirty u Check the lamp and restart
instrument. identification of light peak caused by low light intensity.
Instrument Alarm: UV detector: Bad
Lamp defective/ Flow cell dirty u Check the lamp and restart
instrument. identification of light peak caused by un­workable light in­tensity.
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BÜCHI Labortechnik AG Help with faults | 8
Error message Possible cause Solution
Instrument Alarm: UV detector: Low
Hardware error UV detector u Contact BUCHI Customer
Service. light intensity was found on some photo elements of CCD sensor.
Instrument Alarm: UV detector: Spon­taneously failure on analog or digital power supply.
Instrument Alarm: UV detector: Error or base offset of unit, bad CCD sen­sor, monochroma­tor is open.
Instrument Alarm: UV detector: Sec­ondary lamp is not working or lamp spontaneously douse.
Instrument Alarm: UV detector: Any fan is not working or any fan is dis­connected or me­chanical blocked.
Hardware error UV detector u Contact BUCHI Customer
Service.
Hardware error UV detector u Contact BUCHI Customer
Service.
2nd lamp defect u Check the lamp and restart
instrument.
Hardware error UV detector u Contact BUCHI Customer
Service.
Solvent List File Solvent list file corrupted u Shutdown the Pure soft-
ware.
u Delete the solvent list. u Restart the Pure software.
Solvent Lines File: Invalid program ex­ecution.
Solvent Defaults File: The solvent in-
Solvent lines file corrupted u Shutdown the Pure soft-
ware.
u Delete the solvent list. u Restart the Pure software.
Software damaged u Uninstall and reinstall soft-
ware. formation file and the default solvent information file are missing.
Using Default Sol-
Solvent file has been deleted u Restart the instrument. vent List: System defaults used in­stead of actual re­source.
Operation Manual Pure Chromatography Instrument C-805 59/70
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8 | Help with faults BÜCHI Labortechnik AG
Error message Possible cause Solution
Solvent Pressure: Pressure limit has been exceeded.
Blockage in the line u Remove column.
u Replace with bypass. u Determine if column is not
the source of blockage.
u If not column is the source
of blockage, then check all fluidic lines.
Sample crashing/precipitate u Purge lines/system with a
strong or appropriate sol­vent that will dissolve the sample
Error in solvent line calibration file.
Sensor pressure calibration file
Instrument Alarm: Vapor
Valve stuck in incorrect posi­tion
u Reset valve position. u Contact BUCHI Customer
Service.
Calibration file of solvent lines damaged
Pressure sensor calibration file damaged.
u Shutdown the Pure soft-
ware.
u Delete the calibration list. u Restart the Pure software.
u Shutdown the Pure soft-
ware.
u Delete the pressure value
list.
u Restart the Pure software.
Vapor sensor settings are set too sensitive
u Change the vapor limits to
a lower sensitivity. See Chapter6.2.7 "Editing the vapor sensor sensitivity", page39
Leaks u Check for any leaks in the
solvent flow paths.
Solvent vapors in work area u Solvent vapors in the work
area may set on the alarm. Use the instrument in a hood or well ventilated area with no open solvents near the system.
Vapor sensor no signal
Instrument Alarm: Watchdog
Vapor sensor is not connected or is defect
Timing/communication issue in software
u Check the cable to the va-
por sensor.
If in setup mode:
u Restart the instrument. u
If in run mode:
u Press reset. u Restart after the run is fin-
ish.
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BÜCHI Labortechnik AG Help with faults | 8
Error message Possible cause Solution
Solvent Pressure Solvent pressure limit has
been exceeded
u Remove column. u Replace with bypass. u Determine if column is not
the source of blockage.
u If not column is the source
of blockage, then check all fluidic lines.
Fraction Collector Arm is obstructed u Check arm path to make
sure there are no obstruc­tions.
u Reset the Fraction Collec-
tor arm. See Chapter8.7 "Resetting the Fraction col­lector arm", page61
Fraction collector arm did not
home properly
Fraction collector arm motor is
slipping
Home position sensor is bad u Contact BUCHI Customer
Fraction collector arm motor
has no power
Low Disk Space The disk space on this unit is
almost full.
8.7 Resetting the Fraction collector arm
Navigation path
Tools Manual Control Fraction Collector Arm Reset
u Navigate to the Fra cti on Coll ect or Arm Re set dialog according to the naviga-
tion path.
u Confirm the secure question.
ð The Fraction collector arm is resetted.
u Tighten the motor coupler. u Contact BUCHI Customer
Service.
u Contact BUCHI Customer
Service.
Service.
u Contact BUCHI Customer
Service.
u Back up and delete data. u Contact BUCHI Customer
Service.
Operation Manual Pure Chromatography Instrument C-805 61/70
Page 62
9 | Taking out of service and disposal BÜCHI Labortechnik AG
9 Taking out of service and disposal
9.1 Taking out of service
u Switch off the instrument and disconnect it from the mains power supply. u Remove all tubing and communication cables from the device.
9.2 Disposal
The operator is responsible for proper disposal of the instrument.
u When disposing of equipment observe the local regulations and statutory require-
ments regarding waste disposal.
u When disposing, observe the disposal regulations of the materials used. Materials
used see Chapter3.5 "Technical data", page14
9.3 Returning the instrument
Before returning the instrument, contact the BÜCHI Labortechnik AG Service Depart­ment.
https://www.buchi.com/contact
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BÜCHI Labortechnik AG Appendix | 10
10 Appendix
10.1 Spare parts and accessories
Use only genuine BUCHI consumables and spare parts in order to ensure correct, safe and reliable operation of the system.
NOTE
Any modifications of spare parts or assemblies are only allowed with the prior written permission of BUCHI.
10.1.1 Accessories
Order no. Image
Pure rack type 1
Rack for 12 x 75 mm glass tubes, 1 pc.
11066672
Pure rack type 2
Rack for 13 x 100 mm glass tubes, 1 pc.
Pure rack type 3
Rack for 16 x 125 mm glass tubes, 1 pc.
Pure rack type 4
Rack for 16 x 150 mm glass tubes, 1 pc.
Pure rack type 5
Rack for 18 x 150 mm glass tubes, 1 pc.
Pure rack type 6
Rack for 25 x 150 mm glass tubes, 1 pc.
Pure rack type 7
Rack for 9 squared bottles of 480 mL, 1 pc.
11066673
11066674
11066675
11066676
11066677
11068452
Pure rack type 8 (funnel rack)
Rack for 6 funnels
Pure rack type 9
Rack for 16 x 100 mm glass tubes, 1 pc.
Operation Manual Pure Chromatography Instrument C-805 63/70
11069407
11069242
Page 64
10 | Appendix BÜCHI Labortechnik AG
Order no. Image
Solvent bottle platform kit
Solvent bottle platform on top of the instrument. For maximum 4 bottles (volume 4 L each)
11069285
Retaining container
Retaining container for solvent bottle platform for more safety regarding leaking
Loading Pump
with flow rates from 2.5 to 250 mL/min, incl. tubing and fitting
10.1.2 Spare parts
Injection valve UNF 1/4"-28 044867
Touch-screen stylus 11068360
Hook-and-loop strap 11071732
11068468
11071418
Order no. Image
10.1.3 Tools and adapter kits
Luer lock connection set
Set of 2 luer lock adapters
Advanced adapter kit flash
Tube cutter, Fittings (1/8", 1/16"), Tubing (pneumatic, FEP 1/8", FEP 1/16"), Luer Lock adapters, Pneumatic reduction, Fuses, Injection valve
Advanced adapter kit flash/prep
Tube cutter, Wrenches, Fittings (1/8", 1/16"), One piece fitting, 1/16", Tubing (pneumatic, FEP 1/8", FEP PEEK 1/16"), SS nut and ferrule, Reductions, Luer Lock adapters, Fuses, Injection valve
10.1.4 Tubes
Pure Glass Tubes 13 x 100 mm
1000 pcs.
Pure Glass Tubes 16 x 150 mm
1000 pcs.
Pure Glass Tubes 18 x 150 mm
500 pcs.
Order no.
11068242
11068361
11068363
Order no.
148623414
148623416
148623410
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BÜCHI Labortechnik AG Appendix | 10
Order no.
Pure Glass Tubes 25 x 150 mm
500 pcs.
Pure Squared bottles 480 mL
24 pcs.
148623411
148623412
10.1.5 Wear parts
Order no. Image
Pure UV flow cell 0.3 mm
For all C-8xx
11068210
Pure UV flow cell 1.3 mm
For all C-8xx, for enhanced sensitivity
Pure Solid loader test 20 pcs 11069686
10.2 Folder locations
NOTE
Hidden folders
By default settings the following folder locations are hidden.
4 Start the software [Windows Explorer] on the instrument. 4 Navigate to folder options via the following navigation path: View Folder Op-
tions View
4 Activate the function [Show hidden files, folders and drives].
Explanation Type Folder
Method files .gfm C:\Users\Public\Documents\Buchi\Pure
Run files .gkfr C:\Users\Public\Documents\Buchi\Pure\runs
11068214
\methods
10.3 Finding out separation conditions with the navigator
10.3.1 Open the navigator
Navigation path
Gradient panel
u Navigate to the Gra die nt panel according the navigation path. u Tap the button [Navigator].
ð The display shows the dialog N avi gator.
Operation Manual Pure Chromatography Instrument C-805 65/70
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10 | Appendix BÜCHI Labortechnik AG
10.3.2 TLC Silica
The TLC-Silica tool uses TLC separation data to provide a recommended gradient for silica separations of 2 or 3 components.
Specification of the samples needed:
Two different solvent concentrationsTwo separationsSilica TLC plates
Precondition: R The display shows the dialog Na viga tor . See Chapter10.3.1 "Open the naviga-
tor", page65
u Select the TLC - S ilica tab. u Select the radio button for two or three components. u Select the weaker solvent at drop-down list A. u Select the stronger solvent at drop-down list B. u Enter the solvent B concentrations used in the TLC separations. u Measure the distance the spot moved on the silica TLC plates. u Divide the measured value by the distance the solvent traveled.
ð This is your Rf- value.
u Enter the value in the Rf entry field. u Select the column you wish to use from the drop-down list
ð The column is selected. ð The display shows the default flow rate.
u Adjust the flow rate according to your needs. u Select the radio button for Speed or Purity. u Tap the button [Calculate].
ð The display shows the results.
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BÜCHI Labortechnik AG Appendix | 10
u Adjust the following values if necessary:
ColumnFlow rateSpeed / Purity
u Tap the button [Accept].
ð The gradient is saved for a run. ð The dialog box closes.
10.3.3 LC-C18
The LC-C18 Tool uses isocratic HPLC separation data to provide a recommended gradient for reversed phase separations of 2 components.
Specification of the samples needed:
Two isocratic runs on a HPLC columnDifferent mobile phase solvent concentrationsRetention times (t1 and t2) of the components from the chromatograms.
Precondition: R The display shows the dialog Na viga tor . See Chapter10.3.1 "Open the naviga-
tor", page65
u Select the LC- C18 tab. u Select the HPLC column used from the drop-down list. u Select the weaker solvent at drop-down list A. u Select the stronger solvent at drop-down list B. u Enter the solvent concentrations used in the HPLC separations. u Enter the retention times for each separation under each chromatograph. u Select the column you wish to use from the drop-down list
ð The column is selected. ð The display shows the default flow rate.
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10 | Appendix BÜCHI Labortechnik AG
u Adjust the flow rate according to your needs. u Select the radio button for Speed or Purity. u Tap the button [Calculate].
ð The display shows the results.
u Tap the button [Accept].
ð The gradient is saved for a run. ð The dialog box closes.
10.3.4 LC-Transfer
The LC-Transfer tool converts an HPLC gradient into a Flash Chromatography gradi­ent.
Specification of the sample needed:
One run on a HPLC column (in gradient elution mode)Times %B changes (t1, t2 and t3)
Precondition: R The display shows the dialog Na viga tor . See Chapter10.3.1 "Open the naviga-
tor", page65
u Select the LC-Transfer tab. u Select the HPLC column type used from the drop-down list. u Enter the flow rate used in the HPLC separation. u Enter the following HPLC gradient conditions:
lower and higher %Btimes t1, t2 and t3
u Select the cartridge you wish to use for the Flash separation from the drop-down
list.
ð The cartridge is selected. ð The display shows the default flow rate.
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BÜCHI Labortechnik AG Appendix | 10
u Adjust the flow rate according to your needs. u Tap the button [Calculate].
ð The display shows the results.
u Adjust the following values if necessary:
Flow rate
u Tap the button [Accept].
ð The gradient is saved for a run. ð The dialog box closes.
Operation Manual Pure Chromatography Instrument C-805 69/70
Page 70
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