Pure Chromatography Instrument C-805
Operation Manual
11594236 | B en
Page 2
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.
Page 3
BÜCHI Labortechnik AGTable of contents
Table of contents
1About this document........................................................................................................... 6
1.1Warning notices in this document........................................................................................................ 6
2.1Proper use ........................................................................................................................................... 8
2.2Use other than intended ...................................................................................................................... 8
3.4Scope of delivery ............................................................................................................................... 14
3.5Technical data ................................................................................................................................... 14
4.3Lifting the instrument ......................................................................................................................... 17
6.2Editing a method................................................................................................................................ 32
6.2.1Selecting a cartridge (Flash mode)........................................................................................32
6.2.2Selecting a solvent.................................................................................................................33
6.2.3Editing the gradient................................................................................................................34
6.2.4Editing the wavelength for the UV detector............................................................................36
6.2.5Editing the fraction collection criteria .....................................................................................37
6.2.6Editing the fraction collection time .........................................................................................38
6.2.7Editing the vapor sensor sensitivity........................................................................................39
6.2.8Saving a method....................................................................................................................40
6.3Editing a solvent ................................................................................................................................ 40
6.3.1Adding a new solvent.............................................................................................................40
6.3.2Deleting a solvent ..................................................................................................................41
6.4Tasks during a separation ................................................................................................................. 42
6.4.1Injecting a sample into the flash system ................................................................................ 42
6.4.2Installing and removing a cartridge........................................................................................43
6.4.3Inserting the fraction collection tray .......................................................................................44
6.4.4Selecting an existing method.................................................................................................44
6.4.5Selecting values on the dialog box Sample Loading .............................................................45
6.5Performing a Flash separation using a method................................................................................. 45
6.5.1Preparing the instrument........................................................................................................45
6.5.2Starting Flash separation using a method .............................................................................45
6.5.3Changings during a separation..............................................................................................46
6.5.4Ending a Flash separation ..................................................................................................... 46
6.5.5Shutting down the instrument ................................................................................................46
6.6Performing a Flash separation manually ........................................................................................... 46
6.6.1Preparing the instrument........................................................................................................46
Operation Manual Pure Chromatography Instrument C-805v
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1 | About this documentBÜCHI Labortechnik AG
1About 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
1.1Warning 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 wordMeaning
DANGERIndicates a danger with a high level of risk which could result in
death or serious injury if not prevented.
WARNINGIndicates a danger with a medium level of risk which could result in
CAUTIONIndicates a danger with a low level of risk which could result in mi-
NOTICEIndicates a danger that could result in damage to property.
1.2Symbols
The following symbols are displayed in this operation manual or on the device:
1.2.1Warning symbols
SymbolMeaning
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
1.2.2Mark-ups and symbols
NOTE
This symbol draws attention to useful and important information.
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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-upExplanation
Win dowSoftware Windows are marked-up like this.
TabTabs are marked-up like this.
Dia logDialogs 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.
StatusStatus is marked-up like this.
SignalSignals are marked-up like this.
1.3Trademarks
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.
1.4Connected 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-8057/70
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2 | SafetyBÜCHI Labortechnik AG
2Safety
2.1Proper use
The instrument is designed and built for laboratories.
The instrument can be used for the following tasks:
Purification
Separation of one or more compounds from a mixture
2.2Use other than intended
Use of any kind other than that described in Chapter2.1 "Proper use", page8 and
any application that does not comply with the technical specifications (See Chapter3.5 "Technical data", page14) 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.
2.3Staff 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 AGSafety | 2
2.4Residual 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.
2.4.1Faults 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.
2.4.2Malware 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.
2.4.3Damage 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 Chapter6 "Operation", page23
2.5Personal 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.
2.6Modifications
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.
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3 | Product descriptionBÜCHI Labortechnik AG
Gradient valve
UV
detector
Fraction
collection
Solvent 2
Solvent 1
Pump
Sample
introduction
Cartridge
3Product description
3.1Description 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 solvents
Injection of liquid or solid sample
Separation on a cartridge
Identifying the compounds by UV
Collecting the desired fractions
Instrument schematic:
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1
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4
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3.2Configuration
3.2.1Front view
Fig.1: Front view
1Control panel2RFID reader
3On/Off switch4USB Port
5Cartridge holder6Flash pump
7Fraction collection bay
3.2.2Rear view
NOTE
All electrical connections are not limited energy.
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3 | Product descriptionBÜCHI Labortechnik AG
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8
7
6
1
2
3
4
5
Fig.2: Rear view
1Ventilation slot2Gradient valve
(See Chapter3.2.3 "Connections on
gradient valve", page13 )
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BÜCHI Labortechnik AGProduct 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
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9
10
9
3.2.3Connections on gradient valve
Fig.3: Connections on the gradient valve
1Waste line2Solvent line 2
3Solvent line 1
3.3Type plate
The type plate identifies the instrument. The type plate is located at the rear of the instrument.
Fig.4: Type Plate
1Company name and address2Instrument name
3Serial number4Input voltage range
5Frequency6Power consumption maximum
7Year of manufacture8Product code
9Approvals10 Symbol for "Do not dispose of as
household waste"
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3 | Product descriptionBÜCHI Labortechnik AG
3.4Scope 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.
3.5Technical data
3.5.1Pure Chromatography Instrument C-805
Pure C-805
Dimension
(W x D x H)
Weight24 kg
Clearance on each side of the instrument200 mm
Power consumption350 W
Connection voltage100 - 240 V ± 10 %
365 x 570 x 680 mm
Frequency50 - 60 Hz
Fuse4 A
Overvoltage categoryII
Pollution degree2
IP CodeIP 20
Solvents2
USB port3
LAN port
(RJ45)
RFID reader
(racks)
RFID reader
(cartridges)
Fraction collector bayclosed
Lighted fraction collector bayYes
Vapor sensorYes
Pump Flash Mode
1
Yes
Yes
Pure C-805
Gradientbinary
Pressure range0 - 50 bar
Flow rate0 - 250 mL/min
Flow rate accuracy< 2 %
Functional principleself-priming
Specification3 pistons
radial arranged
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BÜCHI Labortechnik AGProduct description | 3
UV Detector
Pure C-805
UV wavelength range200 - 400 nm
Light sourcesDeuterium
DetectorDAD
3.5.2Ambient conditions
For indoor use only.
Max. altitude above sea level2000 m
Ambient temperature5‒40°C (25°C)
No maximum performance above 25°C
Maximum relative humidity80% for temperatures up to 31°C
Storage temperaturemax. 45 °C
3.5.3Material
ComponentMaterials of construction
HousingPowder coated steel 1.4301
Fraction collection bayPMMA / PET
Pump headPEEK
Pump coverPP
Pump excenter housingAluminum
TubingsFEP
FittingPOM
Valve screw fittingPOM
FerruleETFE
Cone ringPOM
Radial sealPTFE
PistonsCeramic
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4 | Transport and storageBÜCHI Labortechnik AG
4Transport and storage
4.1Transport
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.
4.2Storage
u Make sure that the ambient conditions are complied with (see Chapter3.5 "Tech-
nical data", page14).
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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4.3Lifting 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 | InstallationBÜCHI Labortechnik AG
1
5Installation
5.1Installation 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 Chapter3.5 "Technical data", page14
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.
5.2Before 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.
5.3Securing against earthquakes
The instrument has an earthquake fixing point to protect the device against falling.
Fig.5: Securing against earthquakes
1Fixing point
u Tie the lashing mount to a fixed point using strong cord or a wire.
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5.4Establishing 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 Chapter3.2
"Configuration", page11
u Plug the mains plug into the mains outlet socket.
5.5Establishing 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 | InstallationBÜCHI 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 Chapter3.2 "Configuration",
page11
u Put the other end of the solvent line into the
solvent bottle.
u Assign the solvent to the solvent lines. See
Chapter5.6 "Assigning solvent to solvent
lines", page20
5.6Assigning 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 Chapter6.3 "Editing
a solvent", page40
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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5.7Assembling 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.
5.8Assembling 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.
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5 | InstallationBÜCHI 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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8
7
1
2
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4
6
6Operation
6.1Control panel
6.1.1Layout of control panel
Fig.6: Display
No.DescriptionFunction
1[Menu] barShows the available menus.
See Menu bar
2[Conditions] panelShows the properties and default set-
3[Wavelength] panelShows available wavelengths and scan
4[Collection] panelShows collection options.
5[Gradient] panelShows chromatograms and gradient ta-
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1
6.1.4Conditions panel
1Information button
(Information about the selected column)
The conditions area contains the following settings:
ActionOptionExplanation
[Column]Automatic via RFIDShows the name of the cartridge in-
stalled in the instrument.
[Flow Rate]Enter valueEdit the default flow rate.
[Duration Units]Choice of the duration
type
The following types are available:
minutes / column volumes
[Equilibration]Enter valueIndicates 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 valueAccording 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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6 | OperationBÜCHI Labortechnik AG
1
6.1.5Collection panel
1Tray 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:
ActionOptionExplanation
Fraction collection
options
Select valueThe following options are available:
[Collect Peaks] / [Collect All] / [Collect None]
[Per-Vial Volume]View / Enter valueThe following values are change-
able:
[Peak] / [Non-Peaks]
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6.1.6Gradient panel
Edit the gradient and see separation details.
NOTE
According to the instrument status different options are available.
ActionOptionExplanation
[Table]Create a gradientSee Editing the gradient in tabular
mode
[Navigator]Finding out Flash sepa-
ration conditions
[UV scan details]ViewShows the following charts:
[Zoom]FunctionZoom the graph.
[Options]Select valuesGraph options.
[Edit]Select between the op-
tions
See Chapter10.3 "Finding out separation conditions with the navigator",
page65
3D (UV / Time/ Wavelength)
2D (Time / Wavelength)
Absorption maxima
All 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]FunctionThe gradient is held at the current
solvent ratio.
The gradient continues to the original end-point.
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ActionOptionExplanation
[Auto gradient hold] FunctionThe gradient will be held every time
the signal goes over the set threshold.
6.1.7Run panel
The run panel shows available functions according to the current operation.
SymbolDescriptionMeaning
[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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6.1.8Solvent selection panel
Select solvents for a separation. See Chapter6.2.2 "Selecting a solvent", page33
6.1.9Detector selection panel
ActionOptionExplanation
[UV]Enable / Disable
Select value / Enter
value
Action enabled:
Low / High
Enter values for threshold
Action disabled:
No selection
[Threshold Detection]
Enter valueThe threshold defines the value
above the fraction collector starts to
collect fractions.
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6 | OperationBÜCHI Labortechnik AG
6.1.10Slope detection panel
ActionOptionExplanation
[Slope detection]Enable / DisableAction enabled:
6.2Editing a method
6.2.1Selecting 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
1Information 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.
6.2.2Selecting a solvent
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Navigation path
➔ Solvent selection panel
Precondition:
R The required solvents lines are connected and assigned. See Chapter5.6 "As-
signing solvent to solvent lines", page20
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.
6.2.3Editing 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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ActionOptionExplanation
[Min]Enter valueEnter the time until the value in col-
umn [% 2nd] is reached.
[Solvents]Select valueSelect solvent line combinations.
[% 2nd]Enter valueEnter 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.
6.2.4Editing the wavelength for the UV detector
Status CheckboxExplanationExplanation
OnThe instrument collects fractions.
MonitoringThe instrument records the data from the
UV detector but does not collect the fractions.
OffThe 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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1
6.2.5Editing the fraction collection criteria
1Identifier
The following fraction collection criteria are available:
CriteriaMeaning
[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.
6.2.6Editing 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.
6.2.7Editing the vapor sensor sensitivity
The vapor sensor detects solvent concentration in the ambient air.
The following sensitivity limits are available:
SensitivityMeaning
HighUsed for non-volatile solvents
MediumCompromise between the low and high setting
LowUsed for volatile or semi-volatile solvents
OffThe 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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6.2.8Saving 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.
6.3Editing a solvent
6.3.1Adding 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.
6.3.2Deleting 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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6.4Tasks during a separation
6.4.1Injecting 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.
6.4.2Installing 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.
6.4.3Inserting the fraction collection tray
NOTE
By default the first available tube on each tray is reserved for waste.
Changing the setting. See Chapter6.4.5 "Selecting values on the dialog box Sample
Loading", page45
1Tab2Optical 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.
6.4.4Selecting 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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6.4.5Selecting 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:
ActionExplanation
[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.
6.5Performing a Flash separation using a method
6.5.1Preparing the instrument
Time required:approx. 30 sec.
Precondition:
R All commissioning operations have been completed. See Chapter5 "Installation",
page18
u Switch the On/Off master switch to On.
u Tap the On/Off switch.
ð The instrument is starting up.
6.5.2Starting Flash separation using a method
Precondition:
R The instrument is prepared. See Chapter6.5.1 "Preparing the instrument",
page45
R The required solvents are connected and assigned. See Chapter5.6 "Assigning
solvent to solvent lines", page20
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 Chapter6.4.3 "Insert-
ing the fraction collection tray", page44
u Close the protection shield.
u Open an existing method. See Chapter6.4.4 "Selecting an existing method",
page44
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 Chapter6.4.5 "Selecting val-
ues on the dialog box Sample Loading", page45
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u Follow the instructions on the display.
ð Installing the cartridge. See Chapter6.4.2 "Installing and removing a car-
tridge", page43
ð Introducing the sample into the system. See Chapter6.4.1 "Injecting a sample
into the flash system", page42
6.5.3Changings 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 mode
Hold the gradient. See Gradient panel
Auto gradient hold. See Gradient panel
6.5.4Ending 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
6.5.5Shutting down the instrument
Navigation path
➔ File
Precondition:
R The separation process has ended.
u Purge the instrument with purging solvent. See Chapter7.5 "Cleaning the instru-
ment", page53
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.
6.6Performing a Flash separation manually
6.6.1Preparing the instrument
Time required:approx. 30 sec.
Precondition:
R All commissioning operations have been completed. See Chapter5 "Installation",
page18
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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.
6.6.2Starting Flash separation manually
Precondition:
R The instrument is prepared. See Chapter6.6.1 "Preparing the instrument",
page46
R The required solvents are connected and assigned. See Chapter5.6 "Assigning
solvent to solvent lines", page20
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 Chapter6.4.3 "Insert-
ing the fraction collection tray", page44
u Close the protection shield.
u Select a cartridge. See Chapter6.2.1 "Selecting a cartridge (Flash mode)",
page32
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 Chapter6.2.3 "Editing the gradi-
ent", page34
u Select the sample collection in the Col lec tion panel. See Chapter6.2.5 "Editing
the fraction collection criteria", page37
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 Chapter6.4.5 "Selecting val-
ues on the dialog box Sample Loading", page45
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 Chapter6.4.1 "Injecting a sample
into the flash system", page42
6.6.3Changings 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 mode
Hold the gradient. See Gradient panel
Auto gradient hold. See Gradient panel
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6.6.4Ending 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
6.6.5Shutting down the instrument
Navigation path
➔ File
Precondition:
R The separation process has ended.
u Purge the instrument with purging solvent. See Chapter7.5 "Cleaning the instru-
ment", page53
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.
6.7Identifying fractions
6.7.1Identifying 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.
6.7.2Identifying 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.
6.8Importing and exporting data
6.8.1Printing 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.
6.8.2Sending 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.
6.8.3Sending 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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BÜCHI Labortechnik AGCleaning and servicing | 7
7Cleaning 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.
7.1Regular maintenance work
ComponentActionFrequency
Pumps and valvesu Purge the instrument with purging solvent.
See Chapter7.5 "Cleaning the instrument", page53
Daily
Tubingu Check for leaks. If a leak is observed, re-
solve the issue before continuing.
Fittingsu Inspect fittings; if solid material is de-
posited on a fitting, clean and tighten (replace) the fitting before continuing.
Drain linesu Check all drain lines to ensure that liquid
can flow through them to the waste container
Waste bottleu Empty the waste bottleDaily
Cartridge holderu Check the holding capability of the car-
tridge holder.
u If necessary, replace the hock-and-loop
strap.
Filtersu Check the filters in the solvent bottles and
clean if necessary.
Fittingsu Check and if necessary tighten the fitting
that secures the tubing from the mobile
phase reservoir manifold to the inlet check
valve housing
Datau Perform a data backupWeekly
Daily
Daily
Daily
Weekly
Weekly
Weekly
Casingu Wipe down the casing with a damp cloth.
u If heavily soiled, use ethanol or a mild de-
tergent.
Warning symbolsu Check that the warning symbols on the in-
strument are legible.
u If they are dirty, clean them.
Displayu Wipe down the display with a damp cloth.Monthly
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Weekly
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7 | Cleaning and servicingBÜCHI Labortechnik AG
7.2Carrying 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 Chapter10.2 "Folder locations",
page65
u Copy the needed data to the USB storage devices.
7.3Calibrating 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.
7.4Cleaning 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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Pumping detergent through the check valves
Materials needed:
Liquid Laboratory Detergent
Isopropanol/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.
7.5Cleaning the instrument
Navigation path
➔ Tools ➔ Manual Control ➔ Column Flushing...
Precondition:
R A purging solvent is assigned to the instrument. See Chapter5.6 "Assigning sol-
vent to solvent lines", page20
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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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8Help with faults
8.1Faults, possible causes and solutions (general)
MalfunctionPossible causeSolution
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.
8.2Faults, possible causes and solutions (cartridge)
MalfunctionPossible causeSolution
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 badu Use new cartridge.
8.3Faults, possible causes and solutions (solvent delivery)
MalfunctionPossible causeSolution
No solvent flowEmpty solvent bottleu Refill the solvent bottle.
Pump not primedu 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 lineu Prime the pump.
Pump seals worn outu Replace the pump seals.
Pulsation of pumpOpen or close time of the inlet
or outlet valves are not correct
Residues in solvent
Sealing abrasion outlet valve
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u Rinse the pump module
with high flowrate with
ethanol or hot distilled water.
u Change check valves.
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8 | Help with faultsBÜCHI Labortechnik AG
MalfunctionPossible causeSolution
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 linesu Find the blocked lines and
replace it.
Over-tightened fittingu 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.
LeaksFitting connection not tightu Find the loose fitting and
tighten it up.
Damaged solvent lineu Find the damaged solvent
line and replace it.
Pump not runningPump 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 pathIncorrect fluidic connections
to/from the mode switching
u Check/correct the fluidic
connections.
valve
8.4Faults, possible causes and solutions (fraction collection)
MalfunctionPossible causeSolution
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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MalfunctionPossible causeSolution
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 detectedRFID tag is badu Put another tray into the
same position to see if it is
recognized to confirm the
cause.
u Replace RFID tag.
8.5Faults, possible causes and solutions (detection)
MalfunctionPossible causeSolution
No UV signalUV light burned outu Replace the UV light.
Low UV signalDirty flow cellu Clean the flow cell.
8.6Error messages
Error messagePossible causeSolution
Instrument Alarm:
Solvent pump:
Communication to
the pump cannot
be established.
Run files.gkfrC:\Users\Public\Documents\Buchi\Pure\runs
11068214
\methods
10.3Finding out separation conditions with the navigator
10.3.1Open 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.
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10.3.2TLC 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 concentrations
Two separations
Silica TLC plates
Precondition:
R The display shows the dialog Na viga tor . See Chapter10.3.1 "Open the naviga-
tor", page65
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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u Adjust the following values if necessary:
Column
Flow rate
Speed / Purity
u Tap the button [Accept].
ð The gradient is saved for a run.
ð The dialog box closes.
10.3.3LC-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 column
Different mobile phase solvent concentrations
Retention times (t1 and t2) of the components from the chromatograms.
Precondition:
R The display shows the dialog Na viga tor . See Chapter10.3.1 "Open the naviga-
tor", page65
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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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.
10.3.4LC-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 Chapter10.3.1 "Open the naviga-
tor", page65
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 %B
times 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 AGAppendix | 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.
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