Buchi Pure C-810 Operation Manual

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Pure Chromatography Instruments
Operation Manual
11593990 | E en
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Imprint
Product Identification: Operation Manual (Original) Pure Chromatography Instruments 11593990
Publication date: 05.2021
Version E
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........................................................................................................... 8
1.1 Warning notices in this document.......................................................................................... 8
1.2 Symbols.................................................................................................................................8
1.2.1 Warning symbols ........................................................................................................8
1.2.2 Mark-ups and symbols................................................................................................8
1.3 Trademarks ...........................................................................................................................9
1.4 Connected devices ................................................................................................................9
2 Safety..................................................................................................................................10
2.1 Proper use ...........................................................................................................................10
2.2 Use other than intended ......................................................................................................10
2.3 Staff qualification .................................................................................................................10
2.4 Location of warning signs on the product ............................................................................11
2.5 Residual risks ......................................................................................................................11
2.5.1 Faults during operation .............................................................................................11
2.5.2 Malware infection due to connections with other devices or network .......................11
2.5.3 Damage to the internal memory due to incorrect shutting down of the instrument...12
2.6 Personal protective equipment ............................................................................................12
2.7 Modifications........................................................................................................................12
3 Product description...........................................................................................................13
3.1 Description of function .........................................................................................................13
3.2 Configuration .......................................................................................................................14
3.2.1 Front view Pure C-810 / C-815 .................................................................................14
3.2.2 Front view Pure C-830 / C-835 / C-850 ....................................................................15
3.2.3 Rear view..................................................................................................................15
3.2.4 Connections on gradient valve .................................................................................17
3.3 Type plate............................................................................................................................17
3.4 Scope of delivery .................................................................................................................18
3.5 Technical data .....................................................................................................................18
3.5.1 Pure Chromatography Instruments...........................................................................18
3.5.2 Ambient conditions ...................................................................................................20
3.5.3 Material .....................................................................................................................21
4 Transport and storage ......................................................................................................22
4.1 Transport .............................................................................................................................22
4.2 Storage ................................................................................................................................22
4.3 Lifting the instrument ...........................................................................................................23
Operation Manual Pure Chromatography Instruments iii
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Table of contents Büchi Labortechnik AG
5 Installation..........................................................................................................................24
5.1 Before installation ................................................................................................................24
5.2 Installation site.....................................................................................................................24
5.3 Securing against earthquakes .............................................................................................24
5.4 Establishing electrical connections......................................................................................25
5.5 Establishing solvent connection ..........................................................................................25
5.6 Installing the solvent level sensor........................................................................................26
5.7 Assigning solvent to solvent lines........................................................................................26
5.8 Calibrating the solvent level sensor.....................................................................................27
5.9 Installing the exhaust (ELSD only) ......................................................................................28
5.10 Assembling the waste bottle................................................................................................28
5.11 Installing the waste level sensor..........................................................................................28
5.12 Calibrating the waste level sensor.......................................................................................29
5.13 Assembling the dry air supply (option) ................................................................................29
5.14 Assembling the gas connection (option).............................................................................. 30
5.15 Assembling the solvent bottle platform (option)................................................................... 31
5.16 Assembling the sample loop (Prep instruments only) .........................................................32
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Operation Manual Pure Chromatography Instruments
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Büchi Labortechnik AG Table of contents
6 Operation............................................................................................................................33
6.1 Control panel .......................................................................................................................33
6.1.1 Layout of control panel .............................................................................................33
6.1.2 Enter value................................................................................................................34
6.1.3 Menu bar...................................................................................................................35
6.1.4 Conditions panel .......................................................................................................37
6.1.5 Collection panel ........................................................................................................38
6.1.6 Gradient panel ..........................................................................................................39
6.1.7 Run panel .................................................................................................................40
6.1.8 Solvent selection panel.............................................................................................41
6.1.9 Detector selection panel ...........................................................................................41
6.1.10 Slope detection panel ...............................................................................................42
6.2 Editing a method..................................................................................................................42
6.2.1 Selecting a cartridge (Flash mode)...........................................................................42
6.2.2 Selecting a column (Prep mode) ..............................................................................44
6.2.3 Selecting a solvent....................................................................................................45
6.2.4 Editing the gradient...................................................................................................45
6.2.5 Editing detector selection..........................................................................................48
6.2.6 Editing the wavelength for the UV detector ..............................................................48
6.2.7 Editing the fraction collection criteria ........................................................................49
6.2.8 Editing the fraction collection time ............................................................................50
6.2.9 Editing the vapor sensor sensitivity ..........................................................................52
6.2.10 Saving a method.......................................................................................................52
6.3 Editing a solvent ..................................................................................................................53
6.3.1 Adding a new solvent................................................................................................53
6.3.2 Deleting a solvent .....................................................................................................54
6.4 Tasks during a separation ...................................................................................................54
6.4.1 Introducing a sample into the prep system ...............................................................54
6.4.2 Injecting a sample into the flash system ...................................................................55
6.4.3 Installing and removing a cartridge...........................................................................57
6.4.4 Installing and removing a column .............................................................................58
6.4.5 Inserting the fraction collection tray ..........................................................................60
6.4.6 Selecting an existing method....................................................................................61
6.4.7 Selecting values on the dialog box Sample Loading ................................................61
6.5 Performing a Flash separation using a method...................................................................61
6.5.1 Preparing the instrument ..........................................................................................61
6.5.2 Selecting the flash mode (Pure C-850 only) .............................................................62
6.5.3 Starting Flash separation using a method ................................................................62
6.5.4 Changings during a separation.................................................................................62
6.5.5 Ending a Flash separation ........................................................................................63
6.5.6 Shutting down the instrument ...................................................................................63
6.6 Performing a Flash separation manually .............................................................................63
6.6.1 Preparing the instrument ..........................................................................................63
6.6.2 Selecting the flash mode (Pure C-850 only) .............................................................64
6.6.3 Starting Flash separation manually ..........................................................................64
6.6.4 Changings during a separation.................................................................................65
6.6.5 Ending a Flash separation ........................................................................................65
6.6.6 Shutting down the instrument ...................................................................................65
6.7 Performing a Prep separation using a method ....................................................................66
6.7.1 Preparing the instrument ..........................................................................................66
6.7.2 Selecting the prep mode (Pure C-850 only) .............................................................66
Operation Manual Pure Chromatography Instruments v
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Table of contents Büchi Labortechnik AG
6.7.3 Starting a Prep separation using a method ..............................................................66
6.7.4 Changings during a separation.................................................................................67
6.7.5 Ending a Prep separation .........................................................................................67
6.7.6 Shutting down the instrument ...................................................................................67
6.8 Performing a Prep separation manually ..............................................................................67
6.8.1 Preparing the instrument ..........................................................................................68
6.8.2 Selecting the prep mode (Pure C-850 only) .............................................................68
6.8.3 Starting a separation.................................................................................................68
6.8.4 Changings during a separation.................................................................................69
6.8.5 Ending a Prep separation .........................................................................................69
6.8.6 Shutting down the instrument ...................................................................................69
6.9 Identifying fractions..............................................................................................................70
6.9.1 Identifying fractions by peak .....................................................................................70
6.9.2 Identifying fractions per vial ......................................................................................71
6.10 Importing and exporting data...............................................................................................71
6.10.1 Printing a run report ..................................................................................................71
6.10.2 Sending data to USB ................................................................................................72
6.10.3 Sending PDF to USB ................................................................................................72
7 Cleaning and servicing .....................................................................................................73
7.1 Regular maintenance work..................................................................................................73
7.2 Carrying out a data backup .................................................................................................74
7.3 Calibrating the display .........................................................................................................74
7.4 Cleaning the nebulizer.........................................................................................................75
7.5 Cleaning the check valve.....................................................................................................76
7.6 Cleaning the instrument.......................................................................................................77
7.7 Cleaning the solid loader .....................................................................................................78
7.8 Removing solvent from an used cartridge ...........................................................................78
8 Help with faults ..................................................................................................................79
8.1 Faults, possible causes and solutions (general).................................................................. 79
8.2 Faults, possible causes and solutions (cartridge)................................................................ 79
8.3 Faults, possible causes and solutions (solvent delivery).....................................................79
8.4 Faults, possible causes and solutions (sample injection)....................................................81
8.5 Faults, possible causes and solutions (fraction collection)..................................................81
8.6 Faults, possible causes and solutions (detection) ...............................................................82
8.7 Error messages ...................................................................................................................83
8.8 Resetting the Fraction collector arm....................................................................................89
8.9 Replacing the shuttle valve rotor .........................................................................................90
9 Taking out of service and disposal.................................................................................. 92
9.1 Taking out of service ...........................................................................................................92
9.2 Disposal...............................................................................................................................92
9.3 Returning the instrument .....................................................................................................92
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Operation Manual Pure Chromatography Instruments
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Büchi Labortechnik AG Table of contents
10 Appendix ............................................................................................................................93
10.1 Spare parts and accessories ...............................................................................................93
10.1.1 Accessories ..............................................................................................................93
10.1.2 Sample introduction accessories ..............................................................................94
10.1.3 Spare parts ...............................................................................................................95
10.1.4 Tubes........................................................................................................................95
10.1.5 Tools and adapter kits ..............................................................................................95
10.1.6 Wear parts ................................................................................................................96
10.2 Folder locations ...................................................................................................................96
10.3 Finding out separation conditions with the navigator........................................................... 97
10.3.1 Open the navigator ...................................................................................................97
10.3.2 TLC Silica .................................................................................................................97
10.3.3 LC-C18 .....................................................................................................................98
10.3.4 LC-Transfer...............................................................................................................99
Operation Manual Pure Chromatography Instruments vii
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1 | About this document
1 About this document
1.1 Warning notices in this document
Büchi Labortechnik AG
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
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
death or serious injury if not prevented.
CAUTION Indicates a danger with a low level of risk which could result in mi-
nor or medium-severity injury if not prevented.
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
General warning
Dangerous electrical voltage
8/102
Flammable substances
Laser class 1
1.2.2 Mark-ups and symbols
NOTE
This symbol draws attention to useful and important information.
Operation Manual Pure Chromatography Instruments
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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
instructions 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
Tab
Dia log
[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.
Software Windows are marked-up like this.
Tabs are marked-up like this.
Dialogs are marked-up like this.
Operation Manual Pure Chromatography Instruments
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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:
Purification
Separation 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10 and any application that does not comply with the technical specifications (See Chapter3.5 "Technical data", page18) 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 ELSD without connected exhaust.
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
applicable 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.
10/102
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).
Operation Manual Pure Chromatography Instruments
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Büchi Labortechnik AG
2.4 Location of warning signs on the product
Safety | 2
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.
Fig.1: Location of the warning signs
Laser class 1
2.5 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.
2.5.1 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
inform the operator.
u Do not continue to use devices that are damaged.
2.5.2 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.
Operation Manual Pure Chromatography Instruments
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Page 12
2 | Safety
Büchi Labortechnik AG
2.5.3 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33
2.6 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.
2.7 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.
12/102
Operation Manual Pure Chromatography Instruments
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Büchi Labortechnik AG
Gradient valve
UV
detector
Fraction
collection
Solvent 2
Solvent 3
Solvent 4
Solvent 1
Pump
Sample
introduction
Cartridge / column
ELSD
3 Product description
3.1 Description of function
Product description | 3
Pure instruments are purification devices designed to purify complex samples by either flash chromatography, prep chromatography or by both.
Flash chromatography has the ability to separate gram size samples in short
period.
Prep-HPLC has the ability to separate complex samples at high resolution.
Pure instruments allow:
4 different solvents
Injection of liquid or solid sample
Separation on a cartridge or column
Identifying the compounds by UV and/or ELS detection
Collecting the desired fractions
Pure instrument schematic:
Operation Manual Pure Chromatography Instruments
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3 | Product description
5
10
9
8
1
2
3
4
6
7
3.2 Configuration
3.2.1 Front view Pure C-810 / C-815
Büchi Labortechnik AG
Fig.2: Front view Pure C-810 / C-815
1 Control panel 2 RFID reader
3 On/Off switch 4 USB Port
5 Injection port 6 Cartridge holder
7 Flash pump 8 ELSD flow split valve
9 ELSD nebulizer
(C-815 only)
10 Fraction collection bay
(C-815 only)
14/102
Operation Manual Pure Chromatography Instruments
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Büchi Labortechnik AG
10
9
8
7
1
2
3
4
5
6
3.2.2 Front view Pure C-830 / C-835 / C-850
Product description | 3
Fig.3: Front view Pure C-830 / C-835 / C-850
1 Control panel 2 RFID reader
3 On/Off switch 4 USB Port
5 Column holder 6 Prep HPLC pump
7 ELSD flow split valve
(C-835 / C-850 only)
9 Prep sample injection valve 10 Fraction collection bay
3.2.3 Rear view
NOTE
All electrical connections are not limited energy.
(C-850 only)
8 ELSD nebulizer
(C-835 / C-850 only)
Operation Manual Pure Chromatography Instruments
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Page 16
3 | Product description
3
7
8
9
10
2
1
6
5
4
Büchi Labortechnik AG
Fig.4: Rear view
1 Ventilation slot 2 Gradient valve
(See Chapter3.2.4 "Connections on gradient valve", page17 )
3 Exhaust
(used for instruments with ELSD
4 Signal connection
(for external air supply)
only)
5 USB ports 6 Power supply connection
7 Fuse 8 On/Off master switch
9 Pressurized air inlet 10 LAN port
16/102
Operation Manual Pure Chromatography Instruments
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Büchi Labortechnik AG
6
5
4
3
21
10
9
8
7
3.2.4 Connections on gradient valve
Product description | 3
Fig.5: Connections on the rear side
1 Waste line 2 Solvent line 4
3 Solvent line 3 4 Waste level sensor
5 Solvent line 2 6 Solvent line 1
7 Solvent level sensor line 1 8 Solvent level sensor line 2
9 Solvent level sensor line 3 10 Solvent level sensor line 4
3.3 Type plate
The type plate identifies the instrument. The type plate is located at the rear of the instrument.
Operation Manual Pure Chromatography Instruments
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Page 18
3 | Product description
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
Büchi Labortechnik AG
Fig.6: 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
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 Instruments
Pure
C-810
Dimension (W x D x H)
Weight 25 kg 27 kg 31 kg 33 kg 33 kg
Power consumption 350 W 350 W 350 W 350 W 350 W
Connection voltage 100 - 240 V
Frequency 50 - 60 Hz 50 - 60 Hz 50 - 60 Hz 50 - 60 Hz 50 - 60 Hz
Fuse 4 A 4 A 4 A 4 A 4 A
Overvoltage cate-
365 x 570 x 680 mm
± 10 %
II II II II II
gory
Pure
C-815
365 x 570 x 680 mm
100 - 240 V ± 10 %
household waste"
Pure
C-830
365 x 570 x 680 mm
100 - 240 V ± 10 %
Pure
C-835
365 x 570 x 680 mm
100 - 240 V ± 10 %
Pure
C-850
365 x 570 x 680 mm
100 - 240 V ± 10 %
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Operation Manual Pure Chromatography Instruments
Page 19
Büchi Labortechnik AG
Product description | 3
Pure
C-810
Pure
C-815
Pure
C-830
Pure
C-835
Pure
C-850
Pollution degree 2 2 2 2 2
IP Code IP 20 IP 20 IP 20 IP 20 IP 20
Solvents 4 4 4 4 4
Gas pressure
8 bar 8 bar 8 bar 8 bar 8 bar
( maximum)
Compressed air oil and dust
free
oil and dust free
oil and dust free
oil and dust free
oil and dust free
USB port 3 3 3 3 3
LAN port
1 1 1 1 1
(RJ45)
RFID reader
Yes Yes Yes Yes Yes
(racks)
RFID reader
Yes Yes No No Yes
(cartridges)
Fraction collector
closed closed closed closed closed
bay
Lighted fraction col-
Yes Yes Yes Yes Yes
lector bay
Solvent level sensor Yes Yes Yes Yes Yes
Waste level sensor Yes Yes Yes Yes Yes
Vapor sensor Yes Yes Yes Yes Yes
Pump Flash Mode
Pure
C-810
Gradient binary binary - - binary
Pressure range 0 - 50 bar 0 - 50 bar - - 0 - 50 bar
Flow rate 0 - 250 mL/
min
Flow rate accuracy < 2 % < 2 % - - < 2 %
Functional principle self-priming self-priming - - self-priming
Specification 3 pistons
radial ar­ranged
Pure
C-815
0 - 250 mL/ min
3 pistons radial ar-
ranged
Pure
C-830
Pure
C-835
Pure
C-850
- - 0 - 250 mL/ min
- - 2 pistons parallel ar-
ranged
Pump Prep Mode
Pure
C-810
Gradient - - binary binary binary
Operation Manual Pure Chromatography Instruments
Pure
C-815
Pure
C-830
Pure
C-835
Pure
C-850
19/102
Page 20
3 | Product description
Büchi Labortechnik AG
Pure
C-810
Pure
C-815
Pure
C-830
Pure
C-835
Pure
C-850
Pressure range - - 0-300 bar 0-300 bar 0-300 bar
Flow rate - - 0 - 100 ml/
min
0 - 100 ml/ min
0 - 100 ml/ min
Flow rate accuracy - - < 2 % < 2 % < 2 %
Functional principle - - self-priming self-priming self-priming
Specification - - 2 pistons
parallel ar­ranged
2 pistons parallel ar-
ranged
2 pistons parallel ar-
ranged
UV Detector
Pure
C-810
UV - Vis wavelength
200 - 800nm200 - 800nm200 - 800nm200 - 800nm200 - 800
range
Light sources Halogen /
Deuterium
Pure
C-815
Halogen / Deuterium
Pure
C-830
Halogen / Deuterium
Pure
C-835
Halogen / Deuterium
Pure
C-850
nm
Halogen / Deuterium
Detector DAD DAD DAD DAD DAD
DAD scan entire
range
ELSD Detector
Pure
C-810
Light output laser - 0.3 mW - 1 mW 1 mW
Pressure carrier air - ~0.8 bar - ~0.8 bar ~0.8 bar
Pressure spray air - 3 - 3.5 bar - 3 - 3.5 bar 3 - 3.5 bar
Flow rate air - 2 - 2.5 L/
3.5.2 Ambient conditions
For indoor use only.
Max. altitude above sea level 2000 m
Ambient temperature 5‒40°C (25°C)
entire range
Pure
C-815
min
entire range
Pure
C-830
- 2 - 2.5 L/
entire range
Pure
C-835
min
entire range
Pure
C-850
2 - 2.5 L/ min
No maximum performance above 25°C
20/102
Maximum relative humidity 80% for temperatures up to 31°C
Storage temperature max. 45 °C
Operation Manual Pure Chromatography Instruments
Page 21
Büchi Labortechnik AG
3.5.3 Material
Product description | 3
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 Instruments
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Page 22
4 | Transport and storage
4 Transport and storage
4.1 Transport
4.2 Storage
Büchi Labortechnik AG
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
prevent 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.
u Make sure that the ambient conditions are complied with (see Chapter3.5
"Technical data", page18).
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
Transport and storage | 4
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
indicated on the bottom of the instrument.
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5 | Installation
1
Büchi Labortechnik AG
5 Installation
5.1 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.
5.2 Installation site
The installation site must meet the following requirements:
Firm, level surface.
Take into account the maximum product dimensions and weight. See Chapter3.5
"Technical data", page18
Clearance on each side of the instrument must be at least 200 mm.
Do not expose the instrument to any external thermal loads, such as direct solar
radiation.
Do not expose the instrument to increased electromagnetic emissions.
Electromagnetic fields in the frequency range between 200 to 300 MHz can cause the instrument to operate incorrectly.
Make sure that the installation site meets the requirements of the safety data
sheets for all solvents and samples used.
NOTE
Make sure that the power supply can be disconnected at any time in an emergency.
5.3 Securing against earthquakes
The instrument has an earthquake fixing point to protect the device against falling.
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Fig.7: 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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5.4 Establishing electrical connections
Installation | 5
NOTE
Observe the legal requirements when connecting the instrument to the power supply.
u 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
specifications 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14
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
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Precondition: R Make sure that the instrument is not
connected to the power supply.
u Attach all solvent lines to the
instrument. Connections see Chapter3.2.4 "Connections on gradient valve", page17
u Put the other end of the solvent line
into the solvent bottle.
u Assign the solvent to the solvent lines.
See Chapter5.7 "Assigning solvent to solvent lines", page26
u Install the solvent level sensor. See
Chapter5.6 "Installing the solvent level sensor", page26
5.6 Installing the solvent level sensor
Precondition: R Make sure that the instrument is not
connected to the power supply.
u Attach all solvent level sensors to the
instrument. Connections see Chapter3.2.4 "Connections on gradient valve", page17
u Calibrate the solvent level sensors. See
Chapter5.8 "Calibrating the solvent level sensor", page27
5.7 Assigning solvent to solvent lines
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Navigation path
Tools Solvent Loading
Precondition: R The solvent bottle is connected to the instrument. See Chapter5.5 "Establishing
solvent connection", page25
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Installation | 5
R The solvent you wish to use is part of the solvent library. See Chapter6.3 "Editing
a solvent", page53
u Navigate to the
ð The display shows the dialog box
u Tap the drop-down list next to Line 1.
Sol vent Lo ading
dialog according to the navigation path.
Sol vent Lo ading
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.
5.8 Calibrating the solvent level sensor
.
Navigation path
Tools Calibration and Defaults
Precondition: R The solvent level sensor is not covered by solvent.
u Navigate to the
Cal ibra tio n
ð The display shows the dialog box
u Tap [Zero] for the related solvent line. u Tap the button [Close].
ð The dialog box closes.
Operation Manual Pure Chromatography Instruments
dialog according to the navigation path.
Cal ibra tio n
.
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1
2
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5.9 Installing the exhaust (ELSD only)
u Press the exhaust gas hose (2) on the
exhaust (1).
5.10 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.
5.11 Installing the waste level sensor
Precondition: R Make sure that the instrument is not
connected to the power supply.
u Attach the waste level sensor to the
instrument. Connections see Chapter3.2.4 "Connections on gradient valve", page17
u Calibrate the waste level sensor. See
Chapter5.12 "Calibrating the waste level sensor", page29
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5.12 Calibrating the waste level sensor
Installation | 5
Navigation path
Tools Calibration and Defaults
Precondition: R The waste level sensor is not covered by liquid waste.
u Navigate to the
Cal ibra tio n
ð The display shows the dialog box
u Tap [Zero] for [Waste]. u Tap the button [Close].
dialog according to the navigation path.
Cal ibra tio n
ð The dialog box closes.
5.13 Assembling the dry air supply (option)
u Connect the signal cable from the air
supply to the instrument.
u Connect the gas connection. See
Chapter5.14 "Assembling the gas connection (option)", page30.
.
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5 | Installation
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5.14 Assembling the gas connection (option)
Precondition: R The gas supply complies with the
specifications. See Chapter3.5 "Technical data", page18
u Cut 50 mm from the gas tubing.
u Attach the cut tubing to the air filter.
u Secure the tubing in place.
u Attach the tubing from gas supply to the other
side of the air filter.
u Secure the tubing in place.
u Connect the tubing from the gas supply to the
instrument.
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5.15 Assembling the solvent bottle platform (option)
Installation | 5
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.
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
instrument with screws.
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5.16 Assembling the sample loop (Prep instruments only)
u Attach the sample loop to the
instrument at the position indicated.
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5
9
8
7
1
2
3
4
6
6 Operation
6.1 Control panel
6.1.1 Layout of control panel
Operation | 6
Fig.8: Display
No. Description Function
1 [Menu] bar Shows the available menus.
See Chapter6.1.3 "Menu bar", page35
2 [Conditions] panel Shows the properties and default settings
of the installed column / cartridge. See Chapter6.1.4 "Conditions panel",
page37
3 [Wavelength] panel Shows available wavelengths and scan
options.
4 [Collection] panel Shows collection options.
See Chapter6.1.5 "Collection panel", page38
5 [Gradient] panel Shows chromatograms and gradient ta-
ble. See Chapter6.1.6 "Gradient panel",
page39
6 [Run] panel Shows the operation options.
See Chapter6.1.7 "Run panel", page40
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No. Description Function
7 [Solvent selection] panel Shows selectable solvents.
See Chapter6.1.8 "Solvent selection panel", page41
8 [Detector settings] panel Shows selectable detector options and its
settings. See Chapter6.1.9 "Detector selection
panel", page41
9 [Slope detection] panel Shows selectable slope detection options.
See Chapter6.1.10 "Slope detection panel", page42
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.
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6.1.3 Menu bar
Operation | 6
u Tap the button [OK].
ð The value is saved. ð The dialog box closes.
The following menus are available:
Menu Submenu / Action Explanation
[File] [Open Method] Load an existing method.
See Chapter6.4.6 "Selecting an existing method", page61
[Save Method] Save an edited method.
See Chapter6.2.10 "Saving a method", page52
[Save Method as] Save an edited method with another
name. See Chapter6.2.10 "Saving a method",
page52
[Open Run] Load a completed run.
[Print Run Report] See Chapter6.10.1 "Printing a run re-
port", page71
[Print PDF to USB] See Chapter6.10.3 "Sending PDF to USB",
page72
[Exit] Exit the Pure software to Windows® sys-
tem software.
[Shut down] The instrument shuts down.
[Mode] [Flash] Select the Flash mode.
See Chapter6.5.2 "Selecting the flash mode (Pure C-850 only)", page62
[Preparative] Select the Prep mode.
See Chapter6.7.2 "Selecting the prep mode (Pure C-850 only)", page66
[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 instrument
Operation Manual Pure Chromatography Instruments
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5.7 "Assigning solvent to sol­vent lines", page26
[Solvent Definition] Define solvents.
See Chapter6.3 "Editing a solvent", page53
[Vapor Sensors and Limits] Edit the vapor sensor sensitivity.
See Chapter6.2.9 "Editing the vapor sen­sor sensitivity", page52
[Configuration] System configurations.
[Calibration and Defaults] Calibrate the screen.
Set time and date.
Reset UV lamp.
Calibrate solvent level sensors. See Chapter5.8 "Calibrating the solvent
level sensor", page27
Calibrate the waste level sensor. See Chapter5.12 "Calibrating the waste
level sensor", page29
Set alarms
[Manual control] Maintenance actions.
See Chapter7.6 "Cleaning the instru­ment", page77
See Chapter7.7 "Cleaning the solid loader", page78
See Chapter7.8 "Removing solvent from an used cartridge", page78
See Chapter8.8 "Resetting the Fraction collector arm", page89
[NP<>RP] Change back and forth between normal
phase and reverse phase
[Product Services]
(C-810 C-815 C-850 only)
Override max. pressure limit for car­tridges.
[UV Baseline] Adjust the baseline to zero during a run.
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[Language] Select a language.
[Service] BUCHI service technicians only
[Help] [About] The display shows instrument details.
[View Manual] The display shows the Operation manual.
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1
6.1.4 Conditions panel
Operation | 6
1 Information button
(Information about the selected col­umn)
The conditions area contains the following settings:
Action Option Explanation
[Column]
(Prep mode)
[Column]
(Flash mode)
[Flow Rate] Enter value Edit the default flow rate.
[Duration Units] Choice of the duration
Enter value Enter a name for the present car-
tridge.
Select column /auto­matic via RFID
Shows the name of the column in­stalled in the instrument.
The following types are available:
type
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.
Operation Manual Pure Chromatography Instruments
According to the current operation enter the number of column volumes required for the separation.
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Action Option Explanation
[Air Purge Time] Enter value Indicates the period of time that air
is passed through the column after the separation to remove mobile phase
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 changeable:
[Peak] / [Non-Peaks]
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6.1.6 Gradient panel
Operation | 6
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 Chapter "Editing the gradient in
tabular mode", page46
[Navigator] Finding out Flash sepa-
ration conditions
See Chapter10.3 "Finding out sepa­ration conditions with the navigator", page97
[UV scan details] View Shows the following charts:
3D (UV / Time/ Wavelength)
2D (Time / Wavelength)
Absorption maxima
All scan maxima
[Zoom] Function Zoom the graph.
[Options] Select values Graph options.
[Edit] Select between the op-
tions
The graph is in edit mode. See Chap­ter "Editing the gradient in graphic mode", page47
[View] The graph is in view mode.
[Zoom] Zoom the graph.
Operation Manual Pure Chromatography Instruments
(No changes possible)
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Action Option Explanation
[Gradient hold] Function The gradient is held at the current
solvent ratio.
The gradient continues to the origi­nal end-point.
[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
Operation | 6
Select solvents for a separation. See Chapter6.2.3 "Selecting a solvent", page45
6.1.9 Detector selection panel
Action Option Explanation
[ELSD] Enable / Disable
Select value
Operation Manual Pure Chromatography Instruments
Action enabled: Select between Low / High Enter values for threshold
Action disabled: No selection
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Action Option Explanation
[UV] Enable / Disable
Select value / Enter value
[Threshold Detec-
Enter value The threshold defines the value
tion]
6.1.10 Slope detection panel
Action enabled: Low / High Enter values for threshold
Action disabled: No selection
above the fraction collector starts to collect fractions.
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.
u The indication for recognizing the cartridge is a sound.
Fraction collection triggered by slope
Action disabled: No detection
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1
Operation | 6
1 Information button
(Information about the selected col­umn)
Navigation path
Conditions panel
u Navigate to the u Tap the input box next to [Column].
Con diti ons select ion
panel according the navigation path.
ð The display shows a menu with selectable cartridges.
u Select the cartridges you wish to use.
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6.2.2 Selecting a column (Prep mode)
1 Information button
(Information about the selected col­umn)
Navigation path
Conditions panel
u Navigate to the u Tap the input box next to [Column].
Con diti ons select ion
panel according the navigation path.
ð The display shows a dialog with an alphanumeric input box.
u Enter a name for the column. u Tap the button [OK]. u Tap the input box next to [Flow rate].
ð The display shows a dialog box with a numeric input box.
u Enter a value for the flow rate. u Tap the button [OK]. u Tap the input ox next to [Max. Pressure].
ð The display shows a dialog box with a numeric input box.
u Enter the maximum pressure for the column.
u Tap the button [OK].
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6.2.3 Selecting a solvent
Operation | 6
Navigation path
Solvent selection panel
Precondition: R The required solvents lines are connected and assigned. See Chapter5.7
"Assigning solvent to solvent lines", page26
u Navigate to the u Tap the drop-down list next to A: .
Sol vent se lection
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.
6.2.4 Editing the gradient
The composition of the mobile phase as a function of time can be indicated by entering the gradient. Four solvent lines can be used to generate a binary gradient. The solvents used to define the gradient can be altered during the separation.
panel according the navigation path.
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Editing the gradient in tabular mode
The following settings are available:
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 u Tap the button [Table].
Gra dien t
ð The display shows the dialog
u Tap the cell for [Min].
panel according the navigation path.
Gra dien t T able
.
ð The display shows a dialog box with a numeric input box.
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Operation | 6
u Enter the time. u Tap the button [OK]. u Tap the cell for [AB].
ð The display shows a drop-down list with solvent line combinations.
u Select the combination that you want to use. 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
Gra dien 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 u Tap the button [Edit].
Gra dien t
ð The Display shows a drop-down list.
u Select [Edit].
panel according the navigation path.
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.
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Change solvent combinations
u Solvent line combinations can be accessed by clicking on the AB box to reveal a
drop-down list.
6.2.5 Editing detector selection
Navigation path
Detector selection panel
u Navigate to the u Activate checkbox for the detector you wish to use.
Det ecto r s electio n
panel according the navigation path.
ð The detector is activated.
6.2.6 Editing the wavelength for the UV detector
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1
Operation | 6
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 u Activate the checkbock next to [UV].
u Tap the input box next to [UV].
Wav elen gth
panel according the navigation path.
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.
6.2.7 Editing the fraction collection criteria
1 Identifier
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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. u Tap the button [OK].
ð The dialog box closes.
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6.2.8 Editing the fraction collection time
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Operation | 6
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 u Tap the button [Program collect].
Gra dien t
ð The display shows the dialog
u Tap the input box.
panel according the navigation path.
Pro gram co lle ct
.
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.
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.
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6.2.9 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
ð The display shows the dialog box
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.
6.2.10 Saving a method
Vap or S ens ors
dialog according to the navigation path.
Vap or S ens ors
.
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Navigation path
File Save Method as
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Operation | 6
u Navigate to the
Sav e Me tho d as
ð The display shows the dialog box
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
dialog according to the navigation path.
Sav e Me tho d as
.
Navigation path
Tools Solvent Definition
u Navigate to the
ð The display shows the dialog box
u Tap the button [Add Solvent].
ð The display shows the dialog box
u Tap the input box next to [Name].
Sol vent De finitio n
Sol vent De finitio n
Sol vent
dialog according to the navigation path.
.
.
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
Operation Manual Pure Chromatography Instruments
Sol vent Ve rificat ion
.
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6 | Operation
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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
Sol vent De finitio n
6.3.2 Deleting a solvent
Navigation path
Tools Solvent Definition
u Navigate to the
ð The display shows the dialog box
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.
Sol vent De finitio n
closes.
dialog according to the navigation path.
Sol vent De finitio n
.
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6.4 Tasks during a separation
6.4.1 Introducing a sample into the prep system
u Connect the syringe at the sample loop
port.
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Operation | 6
u Press the plunger.
u Wait until the run starts.
u Disconnect the syringe at the inert loop
port.
6.4.2 Injecting a sample into the flash system
Injecting a sample into the flash system at the luer port
CAUTION
Not removed syringe after injection.
A not removed syringe after injection can lead to spill of solvent and injuries.
u Remove the syringe after injection.
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u Connect the syringe at the luer port.
u Press the plunger.
u Disconnect the syringe at the luer port.
Injecting a sample into the flash system with a solid loader
NOTE
Removing is done in reverse sequence.
u Loosen the solvent line on the top of
the cartridge holder.
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Büchi Labortechnik AG
Operation | 6
u Attach the solid loader to the cartridge
holder.
u Attach the solvent line to the solid
loader.
6.4.3 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.
u The indication for recognizing the cartridge is a sound.
u Hold the cartridge above the RFID
reader.
u Wait until the instrument has taken
over the cartridge data.
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u Lift the clamping plate to release the
lock mechanism and pull up the upper part of the cartridge holder.
u Install the cartridge by pushing the
cartridge inlet down into the luer fitting at the bottom plate.
u Lower the upper part of the cartridge
holder over the luer connection.
u Align it. u Firmly press the arm in place to ensure
a proper seal.
6.4.4 Installing and removing a column
NOTE
Removing is done in reverse sequence.
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Operation | 6
u Install the column in the bottom plate
of the column holder.
u Lower down the upper part of the
column holder.
u Remove the tubing from the upper part
of the column holder.
u Attach the tubing to the column.
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6 | Operation
1
2
Büchi Labortechnik AG
u Remove the lower tubing from the
upper part of the column holder.
u Attach the tubing to the column.
6.4.5 Inserting the fraction collection tray
NOTE
By default the first available tube on each tray is reserved for waste.
Changing the setting. See Chapter6.4.7 "Selecting values on the dialog box Sample Loading", page61
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1 Tab 2 Optical sensor slot
u Place the collection tubes in the collection tray.
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6.4.6 Selecting an existing method
Operation | 6
u Place the trays in the fraction collector bay.
u Make sure that the tab is in the optical sensor slot.
Navigation path
File Open Method
u Navigate to the
Ope n Me tho d
ð The display shows the dialog box
u Select the method you wish to use. u The display highlights the selected method black. u Tap the button [OK].
dialog according to the navigation path.
Ope n Me tho d
.
ð The method is selected. ð The dialog box closes.
6.4.7 Selecting values on the dialog box Sample Loading
The display shows the dialog box separation.
The following settings are possible:
Action Explanation
[Lower flow rate for specified time after in­jection]
[Flush 2nd solvent at the
Reduce flow rate for a specified period, when the pressure increases significantly at the start of the run after sample injection.
Automatically cleaning the system and column.
end of the run]
Sam ple Loa din g
during the starting phase of a
[Override Start Vial] Select the start vial according to your needs.
6.5 Performing a Flash separation using a method
NOTE
Pure C-810 / C-815 / C-850 only
6.5.1 Preparing the instrument
Time required: approx. 30 sec.
Precondition: R All commissioning operations have been completed. See Chapter5 "Installation",
page24
u Switch the On/Off master switch to On. u Tap the On/Off switch.
ð The instrument is starting up.
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6 | Operation
6.5.2 Selecting the flash mode (Pure C-850 only)
Navigation path
Mode
Mod e
u Navigate to the u Select [Flash].
menu according to the navigation path.
ð The flash mode is selected.
6.5.3 Starting Flash separation using a method
Precondition: R The instrument is prepared. See Chapter6.5.1 "Preparing the instrument",
page61
R The required solvents are connected and assigned. See Chapter5.7 "Assigning
solvent to solvent lines", page26
R The sample is prepared.
R The waste bottle is empty.
Büchi Labortechnik AG
u Calibrate the solvent level sensor. See Chapter5.8 "Calibrating the solvent level
sensor", page27
u Calibrate the waste level sensor. See Chapter5.12 "Calibrating the waste level
sensor", page29
u Open the protection shield. u Place the fraction collection trays inside the instrument. See Chapter6.4.5
"Inserting the fraction collection tray", page60
u Close the protection shield. u Open an existing method. See Chapter6.4.6 "Selecting an existing method",
page61
u Tap the button [OK]. u Tap the button [Start] on the u According the requirements adjust the file name.
u Tap the button [OK].
ð The display shows the dialog box
u According the requirements adjust the settings. See Chapter6.4.7 "Selecting
Run
panel.
Sam ple Loa din g
.
values on the dialog box Sample Loading", page61
u Follow the instructions on the display.
ð Installing the cartridge. See Chapter6.4.3 "Installing and removing a cartridge",
page57
ð Introducing the sample into the system. See Chapter6.4.2 "Injecting a sample
into the flash system", page55
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6.5.4 Changings during a separation
NOTE
Parameters that can be edited are highlighted in green
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6.5.5 Ending a Flash separation
Operation | 6
Possibilities to edit the gradient during a separation:
Change the gradient. See Chapter "Editing the gradient in graphic mode", page47
Hold the gradient. See Chapter6.1.6 "Gradient panel", page39
Auto gradient hold. See Chapter6.1.6 "Gradient panel", page39
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
u According to the requirements extend the separation time by 5 minutes.
Precondition: R The display shows the dialog box
u Follow the instructions on the display.
ð Purging the instrument with air. See Chapter7.8 "Removing solvent from an
used cartridge", page78
ð Removing the cartridge. See Chapter6.4.3 "Installing and removing a cartridge",
page57
6.5.6 Shutting down the instrument
Navigation path
File
Precondition: R The separation process has ended.
u Purge the instrument with purging solvent. See Chapter7.6 "Cleaning the
instrument", page77
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.
Sep arat ion End
Run com ple ted
.
.
6.6 Performing a Flash separation manually
NOTE
Pure C-810 / C-815 / C-850 only
6.6.1 Preparing the instrument
Time required: approx. 30 sec.
Precondition: R All commissioning operations have been completed. See Chapter5 "Installation",
page24
u Switch the On/Off master switch to On.
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6 | Operation
u Tap the On/Off switch.
ð The instrument is starting up.
6.6.2 Selecting the flash mode (Pure C-850 only)
Navigation path
Mode
Mod e
u Navigate to the u Select [Flash].
menu according to the navigation path.
ð The flash mode is selected.
6.6.3 Starting Flash separation manually
Precondition: R The instrument is prepared. See Chapter6.6.1 "Preparing the instrument",
page63
R The required solvents are connected and assigned. See Chapter5.7 "Assigning
solvent to solvent lines", page26
Büchi Labortechnik AG
R The sample is prepared.
R The waste bottle is empty.
u Calibrate the solvent level sensor. See Chapter5.8 "Calibrating the solvent level
sensor", page27
u Calibrate the waste level sensor. See Chapter5.12 "Calibrating the waste level
sensor", page29
u Open the protection shield. u Place the fraction collection trays inside the instrument. See Chapter6.4.5
"Inserting the fraction collection tray", page60
u Close the protection shield. u Select a cartridge. See Chapter6.2.1 "Selecting a cartridge (Flash mode)", page42
u Tap the drop-down list next to A: on the
Sol vent Se lection
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6.2.4 "Editing the
gradient", page45
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u Select the sample collection in the
Col lect ion
panel. See Chapter6.2.7 "Editing
the fraction collection criteria", page49
u Select the collection criteria in the
u Tap the button [Start] on the
ð The display shows the dialog box
u According the requirements adjust the settings. See Chapter6.4.7 "Selecting
Col lect ion criter ia
Run
panel.
Sam ple Loa din g
panel.
.
values on the dialog box Sample Loading", page61
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6.6.4 Changings during a separation
6.6.5 Ending a Flash separation
Operation | 6
u Follow the instructions on the display.
ð Installing the cartridge. See Chapter6.4.3 "Installing and removing a cartridge",
page57
ð Introducing the sample into the system. See Chapter6.4.2 "Injecting a sample
into the flash system", page55
NOTE
Parameters that can be edited are highlighted in green
Possibilities to edit the gradient during a separation:
Change the gradient. See Chapter "Editing the gradient in graphic mode", page47
Hold the gradient. See Chapter6.1.6 "Gradient panel", page39
Auto gradient hold. See Chapter6.1.6 "Gradient panel", page39
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
u According to the requirements extend the separation time by 5 minutes.
Precondition: R The display shows the dialog box
u Follow the instructions on the display.
ð Purging the instrument with air. See Chapter7.8 "Removing solvent from an
used cartridge", page78
ð Removing the cartridge. See Chapter6.4.3 "Installing and removing a cartridge",
page57
6.6.6 Shutting down the instrument
Navigation path
File
Precondition: R The separation process has ended.
Sep arat ion End
Run com ple ted
.
.
u Purge the instrument with purging solvent. See Chapter7.6 "Cleaning the
instrument", page77
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.
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6.7 Performing a Prep separation using a method
NOTE
Pure C-830 / C-835 / C-850 only
6.7.1 Preparing the instrument
Time required: approx. 30 sec.
Precondition: R All commissioning operations have been completed. See Chapter5 "Installation",
page24
u Switch the On/Off master switch to On. u Tap the On/Off switch.
ð The instrument is starting up.
6.7.2 Selecting the prep mode (Pure C-850 only)
Navigation path
Mode
Mod e
u Navigate to the u Select [Preparative].
menu according to the navigation path.
ð The prep mode is selected.
6.7.3 Starting a Prep separation using a method
Precondition: R The instrument is prepared. See Chapter6.7.1 "Preparing the instrument",
page66
R The required solvents are connected and assigned. See Chapter5.7 "Assigning
solvent to solvent lines", page26
R The sample is prepared.
R The waste bottle is empty.
u Calibrate the solvent level sensor. See Chapter5.8 "Calibrating the solvent level
sensor", page27
u Calibrate the waste level sensor. See Chapter5.12 "Calibrating the waste level
sensor", page29
u Open the protection shield. u Place the fraction collection trays inside the instrument. See Chapter6.4.5
"Inserting the fraction collection tray", page60
u Close the protection shield. u Open an existing method. See Chapter6.4.6 "Selecting an existing method",
page61
u Tap the button [OK].
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u Tap the button [Start] on the u According the requirements adjust the file name.
u Tap the button [OK].
ð The display shows the dialog box
Run
panel.
Sam ple Loa din g
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.
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Büchi Labortechnik AG
6.7.4 Changings during a separation
6.7.5 Ending a Prep separation
Operation | 6
u According the requirements adjust the settings. See Chapter6.4.7 "Selecting
values on the dialog box Sample Loading", page61
u Follow the instructions on the display.
ð Installing the column. See Chapter6.4.4 "Installing and removing a column",
page58
ð Introducing the sample into the system. See Chapter6.4.1 "Introducing a sample
into the prep system", page54
NOTE
Parameters that can be edited are highlighted in green
Possibilities to edit the gradient during a separation:
Change the gradient. See Chapter "Editing the gradient in graphic mode", page47
Hold the gradient. See Chapter6.1.6 "Gradient panel", page39
Auto gradient hold. See Chapter6.1.6 "Gradient panel", page39
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
u According to the requirements extend the separation time by 5 minutes.
6.7.6 Shutting down the instrument
Navigation path
File
Precondition: R The separation process has ended.
u Removing the column. See Chapter6.4.4 "Installing and removing a column",
page58
u Purge the instrument with purging solvent. See Chapter7.6 "Cleaning the
instrument", page77
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.
Sep arat ion End
.
6.8 Performing a Prep separation manually
NOTE
Pure C-830 / C-835 / C-850 only
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6 | Operation
6.8.1 Preparing the instrument
Time required: approx. 30 sec.
Precondition: R All commissioning operations have been completed. See Chapter5 "Installation",
page24
u Switch the On/Off master switch to On. u Tap the On/Off switch.
ð The instrument is starting up.
6.8.2 Selecting the prep mode (Pure C-850 only)
Navigation path
Mode
Mod e
u Navigate to the u Select [Preparative].
ð The prep mode is selected.
menu according to the navigation path.
Büchi Labortechnik AG
6.8.3 Starting a separation
Precondition: R The instrument is prepared. See Chapter6.8.1 "Preparing the instrument",
page68
R The required solvents are connected and assigned. See Chapter5.7 "Assigning
solvent to solvent lines", page26
R The sample is prepared.
R The waste bottle is empty.
u Calibrate the solvent level sensor. See Chapter5.8 "Calibrating the solvent level
sensor", page27
u Calibrate the waste level sensor. See Chapter5.12 "Calibrating the waste level
sensor", page29
u Open the protection shield. u Place the fraction collection trays inside the instrument. See Chapter6.4.5
"Inserting the fraction collection tray", page60
u Close the protection shield. u Install a column. See Chapter6.4.4 "Installing and removing a column", page58
u Tap the drop-down list next to A: on the
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6.2.4 "Editing the
gradient", page45
Sol vent Se lection
panel.
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u Enter the required times in the
Con diti ons
Operation Manual Pure Chromatography Instruments
panel.
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Büchi Labortechnik AG
Operation | 6
u Select the sample collection in the
the fraction collection criteria", page49
u Select the collection criteria in the
u Tap the button [Start] on the
Run
ð The display shows the dialog box
ð The instrument starts the separation.
u According the requirements adjust the settings. See Chapter6.4.7 "Selecting
values on the dialog box Sample Loading", page61
u Follow the instructions on the display.
ð Installing the column. See Chapter6.4.4 "Installing and removing a column",
page58
ð Introducing the sample into the system. See Chapter6.4.1 "Introducing a sample
into the prep system", page54
6.8.4 Changings during a separation
NOTE
Parameters that can be edited are highlighted in green
Possibilities to edit the gradient during a separation:
Col lect ion
panel. See Chapter6.2.7 "Editing
Col lect ion criter ia
panel.
Sam ple Loa din g
panel.
.
Change the gradient. See Chapter "Editing the gradient in graphic mode", page47
Hold the gradient. See Chapter6.1.6 "Gradient panel", page39
Auto gradient hold. See Chapter6.1.6 "Gradient panel", page39
6.8.5 Ending a Prep 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
u According to the requirements extend the separation time by 5 minutes.
6.8.6 Shutting down the instrument
Navigation path
File
Precondition: R The separation process has ended.
Sep arat ion End
.
u Removing the column. See Chapter6.4.4 "Installing and removing a column",
page58
u Purge the instrument with purging solvent. See Chapter7.6 "Cleaning the
instrument", page77
u Navigate to the [File] menu via the navigation path. u Tap the action [Shut down].
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6 | Operation
Büchi Labortechnik AG
u Confirm the secure question with [Yes].
ð The instrument is shutting down.
6.9 Identifying fractions
6.9.1 Identifying fractions by peak
Fig.9: Identifying fractions
Navigation path
Gradient panel
Precondition: R A separation is finished.
u Navigate to the u Tap the peak with the target value.
ð The
Col lect ion
Gra dien t
panel according the navigation path.
panel shows the corresponding vial.
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6.9.2 Identifying fractions per vial
Operation | 6
Fig.10: Identifying fractions
Navigation path
Collection panel
Precondition: R A separation is finished.
u Navigate to the u Tap the target vial.
ð The
Gra dien t
Col lect ion
panel shows the corresponding peak.
panel according the navigation path.
6.10 Importing and exporting data
6.10.1 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 R un Report
ð The display shows the Windows® print dialog.
u Select your printer. u Tap the button [OK].
ð The report is printed.
Operation Manual Pure Chromatography Instruments
dialog according to the navigation path.
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6 | Operation
6.10.2 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 u Tap the button [Data to USB].
Run
ð The instrument saves an Excel file to the USB storage device.
u Confirm the complete message.
ð The data is stored.
6.10.3 Sending PDF to USB
Navigation path
Run panel
Büchi Labortechnik AG
panel according the navigation path.
Precondition: R The instrument is in past run mode.
u Connect a USB storage device to the instrument.
Run
u Navigate to the u Tap the button [PDF to USB].
panel according the navigation path.
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 AG
7 Cleaning and servicing
7.1 Regular maintenance work
Cleaning and servicing | 7
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.
Component Action Frequency
Pumps and valves u Purge the instrument with air. See
Daily Chapter7.8 "Removing solvent from an used cartridge", page78
u Purge the instrument with purging
solvent. See Chapter7.6 "Cleaning the instrument", page77
Tubing u Check for leaks. If a leak is observed,
Daily resolve the issue before continuing.
Fittings u Inspect fittings; if solid material is
Daily deposited on a fitting, clean and tighten (replace) the fitting before continuing.
Drain lines u Check all drain lines to ensure that
Daily liquid can flow through them to the waste container
Waste bottle u Empty the waste bottle Daily
Filters u Check the filters in the solvent bottles
Weekly and clean if necessary.
Fittings u Check and if necessary tighten the
Weekly fitting that secures the tubing from the mobile phase reservoir manifold to the inlet check valve housing
Data u Perform a data backup Weekly
Casing u Wipe down the casing with a damp
u If heavily soiled, use ethanol or a mild
Warning symbols u Check that the warning symbols on the
u If they are dirty, clean them.
Display u Wipe down the display with a damp
Operation Manual Pure Chromatography Instruments
Weekly cloth.
detergent.
Weekly instrument are legible.
Monthly cloth.
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7 | Cleaning and servicing
Büchi Labortechnik AG
Component Action Frequency
Nebulizer u Clean the nebulizer. See Chapter7.4
"Cleaning the nebulizer", page75
Air filter u Replace the air filter. Yearly
7.2 Carrying out a data backup
Monthly
Navigation path
File Exit
Exi t
u Navigate to the u Confirm the secure question.
dialog according to the navigation path.
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96
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
path.
u Tap the button [Calibrate].
u Follow the instructions on the display.
Cal ibra tio n a nd D efa ults
dialog according to the navigation
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Büchi Labortechnik AG
7.4 Cleaning the nebulizer
Cleaning and servicing | 7
Materials Needed:
HPLC-grade 50:50 methanol: water solution
Sonication bath
u Switch the On/Off master switch to Off.
u Disconnect the liquid inlet line from the
nebulizer.
u Disconnect the gas inlet from the nebulizer
u Remove the knurled screws.
u Remove the nebulizer from the drift tube.
u Place the nebulizer in a beaker filled with 50:50
methanol: water solution.
u Sonicate the nebulizer in an ultrasonic bath for
10 minutes.
u If the nebulizer is still completely blocked,
connect a high-pressure air line to the nebulizer inlet to help remove the blockage.
u If the nebulizer cannot be cleaned, replace the
nebulizer.
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7 | Cleaning and servicing
Büchi Labortechnik AG
u Replace the nebulizer wear band.
u Place the nebulizer to the thrift tube.
u Attach the knurled screws.
u Connect the liquid and gas inlet lines to the
nebulizer.
7.5 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.
Pumping detergent through the check valves
Materials needed:
Liquid Laboratory Detergent
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Isopropanol/Water (50/50) or Methanol/Water (50/50)
Operation Manual Pure Chromatography Instruments
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Büchi Labortechnik AG
Cleaning and servicing | 7
Navigation path
Tools Manual Control Column Flushing...
Precondition: R A bypass is installed. See Chapter6.4.4 "Installing and removing a column",
page58
u Navigate to the
Col umn Flu shing
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
using 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.
7.6 Cleaning the instrument
Navigation path
Tools Manual Control Column Flushing...
Precondition: R A purging solvent is assigned to the instrument. See Chapter5.7 "Assigning
solvent to solvent lines", page26
u Install a bypass. See Chapter6.4.4 "Installing and removing a column", page58
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7 | Cleaning and servicing
Büchi Labortechnik AG
u Navigate to the
u Enter the required data according to your needs.
Col umn Flu shing
dialog according to the navigation path.
7.7 Cleaning the solid loader
Navigation path
Tools Manual Control Solid Loader Flushing...
u Install a bypass. See Chapter6.4.4 "Installing and removing a column", page58
u Navigate to the
Sol id L oad er Flus hin g
dialog according to the navigation
path.
7.8 Removing solvent from an used cartridge
Navigation path
Tools Manual Control Air Purging
Precondition: R The cartridge is installed.
u Navigate to the u Enter the purging time according to your needs.
u Tap the button [Column purge].
Air Pur gin g
dialog according to the navigation path.
ð The instrument and the cartridges are cleaned.
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8 Help with faults
8.1 Faults, possible causes and solutions (general)
Help with faults | 8
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
Uninterrupted 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.
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8 | Help with faults
Büchi Labortechnik AG
Malfunction Possible cause Solution
Pulsation of pump Open or close time of the inlet
or outlet valves are not correct
Residues in solvent
Sealing abrasion outlet valve
Inconsistent solvent flow
Loose fitting/air leak into the pump
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 methods with highly volatile solvents such as diethyl ether and methylene chloride)
u Rinse the pump module with
high flowrate with ethanol or hot distilled water.
u Change check valves.
u Find the loose fitting
between mobile phase reservoir manifold and pump inlet fitting and tighten it up.
u Fix the leak/replace the
pump seals.
u Premix the solvents to
reduce solvent volatility.
u Place the highly volatile
solvent bottle in an ice bath to eliminate boiling.
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 replace
it.
Blocked columns or fluidic path
u Locate the component that
caused the blockage, repair, or replace the component.
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
reconnect to the pump sensor.
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
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8.4 Faults, possible causes and solutions (sample injection)
Help with faults | 8
Malfunction Possible cause Solution
Leak around the in­jection port
(Flash mode)
Dried sample or particulate matter interferes with syringe fitting
Defective injection port (Luer
u Clean the injection port with
appropriate solvent or remove particulate matter.
u Replace the injection port.
fitting) adapter
Solid loader leaking Loader hardware is not prop-
erly set up
Leak around the
Loose fitting u Find the loose fitting and
prep injection
u Verify that the loader
hardware is set up correctly.
tighten it up.
valve/sample loop
8.5 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
collection information is set properly.
u Recalibrate the fraction
collector.
Fraction collector (FC) arm does not move
Fraction collector arm did not home properly
Fraction collector arm motor is
u Reset the Fraction collector
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.
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8 | Help with faults
8.6 Faults, possible causes and solutions (detection)
Büchi Labortechnik AG
Malfunction Possible cause Solution
ELSD signal is low or disappears
Sample is too volatile u Sample cannot be detected
by ELSD due to its volatility.
No or low ELSD carrier gas flow u Verify there is gas supplied
to the instrument.
u Check for leak in the gas
lines.
u Verify that there is gas flow
to the nebulizer from the ELSD sampling valve.
u Verify that there is gas flow
to the ELSD sampling valve.
Sample stuck on column u Use stronger solvent or
change column chemistry.
ELSD not equilibrated long enough
u Restart run to re-stabilize
and rezero ELSD baseline.
Blocked nebulizer u Sonicate nebulizer to clean
or replace the nebulizer.
Blocked ELSD line u Trace the blockage and
replace the blocked line.
Poor ELSD Peak shape
Rotor and/or stator in ELSD Sampling valve is worn, dirty, or clogged
Blocked nebulizer or nebulizer tubing
Nebulizer tubing is not prop­erly connected
u Replace the rotor and/or
stator.
u Clean the nebulizer or
replace the nebulizer tubing.
u Reinstall the nebulizer
tubing properly.
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Help with faults | 8
Malfunction Possible cause Solution
Noisy ELSD baseline Dirty or contaminated gas u Replace gas source.
u Replace filter.
Gas is not dry/high humidity environment
Moisture trapped in the gas lines
u Use a dry air supply. u Use nitrogen.
u Remove moisture from lines
by purging the air flow system with nitrogen for 5 minutes.
Mobile phase is contaminated or contains non-volatile modi-
u Use volatile modifiers in the
mobile phase.
fiers
Solvent contains non volatile stabilizers
u Use solvent with volatile
modifiers.
Dirty optics u Clean the optics.
Dirty drift tube u Clean drift tube.
Not correct installed exhaust u Install the exhaust correctly.
See Chapter5.9 "Installing the exhaust (ELSD only)", page28
Electronics - Preamp not grounded properly
u Verify that preamp
grounding cable is in place.
No UV signal UV light burned out u Replace the UV light.
Low UV signal Dirty flow cell u Clean the flow cell.
8.7 Error messages
Error message Possible cause Solution
Instrument Alarm: Solvent pump: Com­munication to the pump cannot be es­tablished.
Instrument Alarm: Solvent pump: Mo­tor overloading.
Instrument Alarm: Solvent pump: Mo­tor regulation error.
Nebulizer is partially blocked u Sonicate nebulizer to clean
or replace.
Silica or packing material leaked out of cartridge
Serial communication dis-
u Replace the cartridge. u Flush the system.
u Restart the instrument.
turbed
- u Contact BUCHI Customer Service.
Hardware error solvent pump u Contact BUCHI Customer
Service.
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8 | Help with faults
Büchi Labortechnik AG
Error message Possible cause Solution
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.
Instrument Alarm: UV detector: Bad block of High Volt­age (HV) generator for lamp or discon­nected lamp or bad lamp.
Instrument Alarm: UV detector: Bad power supply of lamp heater volt­age.
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
Lamp defect u Check the lamp and restart
No lamp
Hardware error UV detector
instrument.
u Contact BUCHI Customer
Service.
Hardware error UV detector u Contact BUCHI Customer
Service.
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.
Lamp defect u Check the lamp and restart
instrument.
Lamp defect u Check the lamp and restart
instrument.
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Help with faults | 8
Error message Possible cause Solution
Instrument Alarm: UV detector: Lamp ignition fails after short douse in AU­TOZERO function and repeated High Voltage impulse and heater cycle fails too.
Instrument Alarm: UV detector: Bad identification of light peak caused by low light intensity.
Instrument Alarm: UV detector: Bad identification of light peak caused by unworkable light in­tensity.
Hardware error UV detector. u Contact BUCHI Customer
Service.
Lamp defective/ Flow cell dirty u Check the lamp and restart
instrument.
Lamp defective/ Flow cell dirty u Check the lamp and restart
instrument.
Instrument Alarm: UV detector: Low 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.
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.
2nd lamp defect u Check the lamp and restart
instrument.
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8 | Help with faults
Büchi Labortechnik AG
Error message Possible cause Solution
Instrument Alarm: UV detector: Any
Hardware error UV detector u Contact BUCHI Customer
Service. fan is not working or any fan is discon­nected or mechani­cal blocked.
Solvent List File Solvent list file corrupted u Shutdown the Pure
software.
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
software.
u Delete the solvent list. u Restart the Pure software.
Software damaged u Uninstall and reinstall
software. formation file and the default solvent information file are missing.
Using Default Sol­vent List: System defaults used in­stead of actual re­source.
Solvent Pressure: Pressure limit has been exceeded.
Solvent file has been deleted u Restart the instrument.
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
Valve stuck in incorrect posi­tion
u Reset valve position. u Contact BUCHI Customer
Service.
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Help with faults | 8
Error message Possible cause Solution
Solvent Pressure 2: Pressure limit has been exceeded.
Error in solvent line calibration file.
Inlet Gas Pressure Out of Range - LOW PRESSURE
Blockage in line after the ELSD sampling valve
u Check the fluidic lines and
components downstream from the pressure sensor 2 (between the ELSD sampling valve and the fraction collector valve, waste line) for the source of blockage.
Calibration file of solvent lines damaged
u Shutdown the Pure
software.
u Delete the calibration list. u Restart the Pure software.
No gas or gas flow is low u Check the gas lines in the
system for leaks.
u Make sure gas source/tank
is available.
The pressure gauge is not set correctly
u Check pressure gauge
setting to make sure that it is set to deliver 2.5 L/min gas flow (Inlet Pressure with Air State off around 85 - 115 psi).
Inlet Gas Pressure Out of Range - LOW PRESSURE (Before run starts)
Inlet gas pressure out of range- HIGH (During run)
Sensor pressure cal­ibration file
Blockage in the system u Check the gas lines in the
system for blockages.
The pressure gauge is not set correctly
u Check pressure gauge
setting to make sure that it is set to deliver 2.5 L/min gas flow (Inlet Pressure with Air State off around 85 - 115 psi).
Blockage in the nebulizer or gas line to the nebulizer
u Check the nebulizer or
tubing to the nebulizer for blockages
u Sonicate the nebulizer in a
suitable solvent or replace nebulizer
Pressure sensor calibration file damaged.
u Shutdown the Pure
software.
u Delete the pressure value
list.
u Restart the Pure software.
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8 | Help with faults
Büchi Labortechnik AG
Error message Possible cause Solution
Instrument Alarm: Vapor
Vapor sensor no sig­nal
Instrument Alarm: Watchdog
Vapor sensor settings are set too sensitive
u Change the vapor limits to a
lower sensitivity. See
Chapter6.2.9 "Editing the
vapor sensor sensitivity",
page52
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 is not connected or is defect
Timing/communication issue in software
u Check the cable to the vapor
sensor.
If in setup mode:
u Restart the instrument.
u
If in run mode:
u Press reset. u Restart after the run is
finish.
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.
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Help with faults | 8
Error message Possible cause Solution
Fraction Collector Arm is obstructed u Check arm path to make
sure there are no obstructions.
u Reset the Fraction Collector
arm. See Chapter8.8 "Resetting the Fraction collector arm", page89
Mode Switching Valve Failure
Prep Injection Valve Failure
Fraction collector arm did not home properly
u Tighten the motor coupler. u Contact BUCHI Customer
Service.
Fraction collector arm motor is slipping
u Contact BUCHI Customer
Service.
Home position sensor is bad u Contact BUCHI Customer
Service.
Fraction collector arm motor has no power
The Mode Switching valve failed to switch.
u Contact BUCHI Customer
Service.
u Press Reset button to stop
the alarm.
u Contact BUCHI Customer
Service.
Prep Injection Valve failed to switch.
Only Flash mode runs can be performed.
u Press Reset button to stop
the alarm.
u Contact BUCHI Customer
Service.
Low Disk Space The disk space on this unit is
almost full.
Solvent Safety Sen­sor alert
More solvent required u Add solvent to bottle.
Solvent safety sensor was not calibrated
Waste Safety Sensor alert
Waste container is full u Empty waste container.
Waste safety sensor was not calibrated
8.8 Resetting the Fraction collector arm
Navigation path
Tools Manual Control Fraction Collector Arm Reset
u Navigate to the
navigation path.
Fra ctio n C ollecto r A rm R ese t
u Back up and delete data. u Contact BUCHI Customer
Service.
u Calibrate/zero the solvent
safety sensor properly.
u Calibrate/zero the solvent
safety sensor properly.
dialog according to the
Operation Manual Pure Chromatography Instruments
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8 | Help with faults
8.9 Replacing the shuttle valve rotor
Büchi Labortechnik AG
u Confirm the secure question.
ð The Fraction collector arm is resetted.
Materials needed:
Torx wrench T10
Pure sampling valve kit
u Switch the On/Off master switch to Off.
Precondition: R Make sure that all tubings are marked for later
installation.
u Remove all tubings.
u Loosen the screws with the Torx wrench. u Remove the valve head.
u Remove the valve rotor.
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Help with faults | 8
u Make sure that the holes in the new rotor and
the pins inside the valve match.
u Attache the valve head to the instrument with
screws.
u Attach all tubings to the instrument.
Operation Manual Pure Chromatography Instruments
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Page 92
9 | Taking out of service and disposal
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
requirements regarding waste disposal.
u When disposing, observe the disposal regulations of the materials used. Materials
used see Chapter3.5 "Technical data", page18
9.3 Returning the instrument
Before returning the instrument, contact the BÜCHI Labortechnik AG Service Department. https://www.buchi.com/contact
Büchi Labortechnik AG
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10 Appendix
10.1 Spare parts and accessories
10.1.1 Accessories
Appendix | 10
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.
Order no. Image
Pure rack type 1
Rack for 12 x 75 mm glass tubes, 1 pc.
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.
Pure rack type 8 (funnel rack)
Rack for 6 funnels
Pure rack type 9
Rack for 16 x 100 mm glass tubes, 1 pc.
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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)
Retaining container
Retaining container for solvent bottle platform for more safety regarding leaking
Pure Dry Air Supply unit 11069026
Loading Pump
with flow rates from 2.5 to 250 mL/min, incl. tubing and fit­ting
Pure cartridge holder XXL
Cartridge holder for cartridges of 800 g to 5000 g
Pure column holder XL
Column holder for column diameters 50 to 70 mm
Pure nebulizer set 11069464
10.1.2 Sample introduction accessories
Pure Solid loader S set, incl. adapter set, sleeve, tubes (20 pcs.) and frits (40 pcs.)
Pure Solid loader M set, incl. adapter set, sleeve, tubes (20 pcs.) and frits (40 pcs.)
Pure Solid loader frits S (40 pcs.) 11068969
Pure Solid loader frits M (40 pcs.) 11069654
Pure Solid loader tubes S (20 pcs.) 11068971
Pure Solid loader tubes M (20 pcs.) 11069653
Pure Solid loader insertion rod S (1 pc.) 11068973
Pure Solid loader insertion rod M (1 pc.) 11070569
Pure sample loop 2 ml, 1 pc. 11068476
Order no.
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Pure sample loop 5 ml, 1 pc. 11068205
Pure sample loop 10 ml, 1 pc. 11068206
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10.1.3 Spare parts
Appendix | 10
Order no. Image
Pure cartridge holder
Cartridge holder for cartridges for 4 g to 330 g
Pure column holder
Column holder for columns diameters 10mm to 50mm
Injection valve UNF 1/4"-28 044867
Pure transfer line ELSD 11069409
Touch-screen stylus 11068360
Sample injection stator 11069688
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.
Pure Glass Tubes 25 x 150 mm
500 pcs.
Pure Squared bottles 480 mL
24 pcs.
10.1.5 Tools and adapter kits
Luer lock connection set
Set of 2 luer lock adapters
Order no.
148623414
148623416
148623410
148623411
148623412
Order no.
Operation Manual Pure Chromatography Instruments
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10 | Appendix
Büchi Labortechnik AG
Order no.
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 prep
Wrenches, Fittings (1/8", 1/16"), One piece fitting, 1/16", Tubing (pneumatic, FEP 1/8", PEEK 1/16"), SS nut and ferrule, Reductions, Fuses
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
Pure solvent line kit
Package with 4 solvent lines and 5 level sensing lines
10.1.6 Wear parts
Pure air filter 11066049
Order no. Image
O-Ring for Pure nebulizer 11066421
Pure nebulizer 11066423
Pure UV flow cell 0.3 mm
For all C-8xx
Pure UV flow cell 1.3 mm
For all C-8xx, for enhanced sensitivity
Shuttle valve rotor & head 11068229
Hose SV-ELSD cpl. 11069457
Pure Solid loader test 20 pcs 11069686
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10.2 Folder locations
Explanation Type Folder
Method files .gfm C:\Users\Public\Documents\Buchi\Pure
\methods
Run files .gkfr C:\Users\Public\Documents\Buchi\Pure\runs
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10.3 Finding out separation conditions with the navigator
10.3.1 Open the navigator
Appendix | 10
Navigation path
Gradient panel
u Navigate to the u Tap the button [Navigator].
ð The display shows the dialog
10.3.2 TLC Silica
Gra dien t
panel according the navigation path.
Nav igat or
.
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
navigator", page97
u Select the 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.
Operation Manual Pure Chromatography Instruments
TLC - Si lic a
tab.
Nav igat or
. See Chapter10.3.1 "Open the
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10 | Appendix
Büchi Labortechnik AG
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.
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.
10.3.3 LC-C18
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The LC-C18 Tool uses isocratic HPLC separation data to provide a recommended gradient for reversed phase separations of 2 components.
Operation Manual Pure Chromatography Instruments
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Appendix | 10
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
Nav igat or
. See Chapter10.3.1 "Open the
navigator", page97
u Select the 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
LC- C18
tab.
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.
u Tap the button [Accept].
ð The gradient is saved for a run. ð The dialog box closes.
10.3.4 LC-Transfer
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10 | Appendix
Büchi Labortechnik AG
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
Nav igat or
. See Chapter10.3.1 "Open the
navigator", page97
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.
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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Operation Manual Pure Chromatography Instruments
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