RotaChrom rCPC User manual
RotaChrom
rCPC
Operation Manual
Version number: OPM-rCPC-121818
Reviewed by Attila Babits
Issued by Zsuzsanna Friedman
RotaChrom Technologies LLC
151 Fő út
Dabas, 2370, Hungary
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RotaChrom rCPC Operation Manual
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Revision History
This document applies to the latest software listed and higher versions. When a subsequent software
version changes the information in this document, a new issue will be released.
OPM-rCPC-121818, December 2018
Software version 1.0
This document was created to:
■Replace the previous Operation Manual
■Improve the content and usability of the instructions
■Update the Hazards section
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Warranty
The system is covered by and subject to the provisions of the warranty included in your contractual
agreement for the system.
The customer is responsible for routine preventive maintenance procedures. The cost of repairs,
arising from the failure to perform these maintenance procedures at the indicated time intervals
according to the specifications provided by RotaChrom, is not covered in the warranty; therefore, it is
the expense of the costumer.
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Safety Notice
Read all manuals and consult with RotaChrom-trained personnel before you operate the system. Do
not perform any procedure before you carefully read all instructions. Always follow the product labels
and the recommendations from the manufacturer. For more information, please contact RotaChrom.
Alerts for Warning, Caution and Note
WARNING
Warning sign indicates a potentially hazardous situation which, if not avoided, could cause
death or serious injury.
CAUTION
Caution sign indicates a potentially hazardous situation which, if not avoided, can cause
minor or moderate injury. Caution can also alert against unsafe practices.
NOTE
Note sign indicates notable information must be followed.
Summary of Hazards
This section describes the possible hazards of the system. The hazards of individual procedures in this
manual are included in the warnings or cautions within the instructions.
Read this section before you operate this system.
Follow the power requirements in the system specifications. Follow the procedures and safety
warnings throughout this manual.
If you use the system in a manner not specified by RotaChrom, the protection provided by the system
can be impaired or system failure can occur.
Chemical Materials
Observe all chemical hazard precautions when doing maintenance, service, or troubleshooting on the
system. Chemical hazard precautions include, but are not limited to: wearing gloves, eye shields and
lab coats, and washing hands after working on contaminated parts of the system.
Follow all laboratory procedures and policies for handling chemical preparations.
Avoid skin contact with chemical preparations. Wear Personal Protective Equipment (PPE) to work
with chemical preparations used with the system. For more information, see the corresponding MSDS
(Material Safety Data Sheet) for all chemicals.
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Clean spills immediately of potentially hazardous substances on the system. If the system must be
decontaminated, contact RotaChrom.
Follow your laboratory procedure for the disposal of hazardous material.
Electric Shock
Do not replace or service any components where you can contact hazardous parts that could cause
electric shock. These maintenances must be performed by RotaChrom.
Electrical Ground
WARNING
Never operate the system until the power cord is connected correctly to an electrical
ground.
Use a three-pronged (grounded) power cord to connect the system to a matching three wire grounded
outlet. A three-phase AC outlet is required with free ends supplying 1 × 16A, with pins P+N+E. Line
frequency should be 50 or 60 Hz, with line voltage of 230V +/- 5%.
Electromagnetic Compatibility
The system generates, uses, and can radiate radio frequency energy. If the system is not installed and
operated correctly, this energy can cause interference with other equipment.
In addition, other equipment can radiate radio frequency energy to which the system is sensitive. If
you suspect interference between the system and other equipment, please contact RotaChrom.
Moving Parts
While the system is in operation, do not touch or go close to any moving parts. Close all covers during
operation. Failure to close covers correctly can cause injury or death.
Liquid Waste
Some liquid waste can require special treatment before disposal. Follow your laboratory procedure
that corresponds the regulations of your country.
Some substances in the chemical preparations may have different storage and disposal regulations.
Follow your operation procedure that corresponds the regulations of your country.
rCPC Hazards
Only a RotaChrom representative can install the system. If the system installation needs modification,
please contact RotaChrom.
■If the system malfunctions, power off the system completely using the main breaker located on
the left side of the rCPC unit before any repair service.
■To confirm system performance, maintain and inspect the system periodically by replacing the
parts according to the instructions in this guide.
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▪Have and follow a maintenance schedule for this system.
▪Create a maintenance routine for the computer software and hardware, including
frequent backing up of data.
▪Do not store backups onsite. Keep one copy on-site for reference and one copy offsite.
■Dedicate the computer hardware to only running the system software. Do not connect the
computer hardware to the Internet, unless instructed to do so by RotaChrom.
■Keep the system’s safety coverings and top coverings closed except for startup procedures and
maintenance.
■All covers (including front door) must be attached and sealed before plugging the instrument into
the main outlet. Before removing any cover or removing safety screws of the front door, shut
down the system.
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Table of Contents
Introduction............................................................................................................................................. 9
Safety precautions................................................................................................................................. 10
RotaChrom cell design........................................................................................................................... 10
Instrument installation.......................................................................................................................... 11
Starting of the instrument..................................................................................................................... 15
Normal operation of the instrument..................................................................................................... 19
Method creating in the software .......................................................................................................... 20
Cleaning and maintenance.................................................................................................................... 23
Cleaning............................................................................................................................................. 23
Cell disassembly for cleaning and cleaning validation................................................................ 23
Cell assembly after cleaning........................................................................................................ 24
Maintenance and service .................................................................................................................. 28
Mounting of the rotor................................................................................................................. 28
Pump seals and check valves replacement................................................................................. 31
Detector lamp replacement:....................................................................................................... 33
Electrical and communication cable disconnection:................................................................... 34
Rotary union replacement: ......................................................................................................... 34
Spare parts ........................................................................................................................................ 36
Warranty ............................................................................................................................................... 37
Troubleshooting .................................................................................................................................... 37
General Safety Information................................................................................................................... 38
General.............................................................................................................................................. 38
Operation .......................................................................................................................................... 38
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Introduction
RotaChrom rCPC is a research & development purpose Centrifugal Partition Chromatography system
intended for pilot scale purification of compounds. Centrifugal Partition Chromatography is a liquid-
liquid chromatographic technique, where both stationary and mobile phases are liquids, and the liquid
stationary phase is immobilized by a strong centrifugal force.
CPC system consists of two interconnected parts:
1. Preparative unit composed of the following items:
■Stainless steel stand
■Input selector valve with the built in control system
■Liquid pump with solvent selector valve –4 inputs, capable of 300 mL/min (0.079 gpm),
at 150 bar (2 175 psi)
■UV detector –200-400 nm range
■Fraction collector (spider) –10 outputs
1. figure: Preparative units
2. CPC rotor with extraction cells (with Variable Frequency Drive) –max 1 500 rpm
2. figure: CPC rotor
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This manual contains the operating instructions of the rCPC system, as well as cleaning instructions
and maintenance instructions.
3. figure: rCPC with connected vessels
Safety precautions
Be aware that all covers (including front door) should be mounted before plugging instrument into
the mains outlet. Before removing any cover or removing safety screws of the front door, shut down
the system and remove mains plug.
RotaChrom cell design
RotaChrom’s unique cell design represents the Keep It Simple Straight (KISS) concept, and so cells are
constructed with easily assembled parts of the following:
Cell tube wall –two 3/8” NPT internal threads, 20 mm hex form, M22 outside fine thread
■PEEK plug –3/8” NPT thread for cell connection, Swagelok connector for tubing
■Stainless Steel wool filling –available in different materials (standard: SS434)
■1/8” SS tubing for connection
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4. figure: RotaChrom rCPC cells in holder
Instrument installation
RotaChrom rCPC system installation is always carried out by qualified personnel trained by RotaChrom
or its partners. User may disconnect some connections and reinstall them by the instructions described
in this chapter.
The flow connection is described on the figure below:
5. figure: schematic of flow connection
6. figure: operation of ASC/DSC valve
Gradient valve
- Upper phase
- Lower phase
- Sample
- Cleaninc solvent
Pump
- 300 mL/min max
- 150 bar max
rCPC rotor
through ASC/DSC
valve
- 100 cells
- 2 L total volume
DAD detector
-200-400 nm
Fraction collector
- 10 outputs
3/16” FEP
tubing
1/8” SS
tubing
1/8”
FEP
1/8” FEP
tubing
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Solvent vessels can be connected to gradient valve by 3/16” FEP tubing. The gradient valve is
connected to the pump with 3/16” FEP tubing.
7. figure: Gradient box
8. figure: Pump
These FEP tubing utilize PEEK nuts with inverted ferrules. Pump should be connected to the ASC/DSC
valve with 1/8” SS tubing, with VICI nut and SS/PEEK ferrule at both ends. ASC/DSC valve should be
connected to the rotor with 1/8” SS tubing, with VICI nut and SS/PEEK ferrule at valve end and
Swagelok nut and ferrule at rotor front (DSC).
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9. figure: ASC/DSC valve
Rotor back (ASC) should be connected to the ASC/DSC valve with 1/8” SS tubing, Swagelok nut and
ferrule at rotor end, and VICI nut and SS/PEEK ferrule at valve. Valve should be connected to the
detector with inverted ferrule at detector end.
10. figure: UV-VIS detector
Detector should be connected to fraction collector with 1/8” FEP or PEEK tubing, with PEEK nuts and
inverted ferrules. Fraction collector has 10 output connections, recommended tubing is 1/8” FEP or
PEEK with PEEK nuts and inverted ferrules.
11. figure: Fraction collector
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See the figures below for guidance:
12. figure: Flow connections on units
Pay special attention to the front and rear of the rotor connection. The rotary seals are standard units
(see spare parts list) and are connected to rotor with ¼” G threads and can be removed by a wrench.
There is a Swagelok 1/8” tubing to ¼” G thread adapter, with SS304 seal. Check the connection tubing
for bending. Check the interconnects for proper connection and fixing.
13. figure: Rotary seals and interconnects
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The server communicates with the peripherals with different ports. RS485 items are daisy-chained
through a common RS-485 bus and connected into an RS232-RS485 adapter (converter), which is
connected to one of the RS-232 ports of the server. ECP2300 pump, Flash 14 DAD 400 detector and
fraction collector communicates with the server through their own RS232 ports. Server is accessible
through LAN by Remote Desktop.
14. figure: Communication connection of peripherals
Default IP setting for the Instrument Data server is DHCP assigned. It is recommended to note the
MAC-address of the instrument and set a fixed IP-assignment on router (contact IT) based on the
instrument’s MAC address. Using a fixed IP to address the instruments minimizes communication
problems, latency and provides easy access from web browser.
Starting of the instrument
Connect the instrument to mains AC and turn on the mains switch.
15. figure: Mains switch
LAN network
LAN
Server
RS232 Port
DSUB9 connector
RS-232 -RS-485
adapter
DSUB9 connector
Rotor VFD
RS485 - RJ45
connector
RS232 Port
DSUB9 connector
Flash 14 PDA
detector
RS232 Port
DSUB9 connector
ECP2300 pump
RS232 Port
DSUB9 connector
Fraction collector
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Let some time the server to boot up and use Remote Desktop to connect to the server.
16. figure: Remote Desktop connection
Give the fix IP address, username and password in the Remote Desktop Connection window.
After successful installation of software please contact info@rotachrom.com or +36-70-885-6922 for
registration key. (Normally the registration is done by RotaChrom during the installation.)
After you execute ECOMAC application you can see next window or similar one. It is the main window
running as Station 1. Main part of the window is the graph where application shows measured data.
State of your analysis or the application is displayed on status bar (analysis time, cursor position or
selection, analysis status, application's status icons) at bottom of the window.
17. figure: Main window of software
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Method file contains all settings of station configuration. Method configuration dialog is accessible
from main menu Method >Setup. You should set device configuration at first. Open Method
configuration dialog by choosing Method >Devices. On the left side of section are displayed supported
devices to you.
18. figure: Device configuration window
You can add selected device to the right by pressing Add button. Devices on the right side are those
which application should connect at start time (initiation phase). Check the list for main components
of rCPC instrument (CPC, ECP pump, Flash detector and Vici actuator /spider).
19. figure: Device identification
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Pressing Test button (for added devices) initiates application to test a connection with device and
returning device's identification (if available). Most of the parameters are disabled often, because
other settings are not possible, or parameter is not used.
20. figure: Communication test of device
After communication tests click on Control button. Time table allows doing available actions in
specified time of analysis. Use right click on area under preview graph to manipulate with this table.
21. figure: Method setup
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For normal operation of instrument, you should add the following: Flow rate, RPM, Inlet % (A,B,C,D),
Detector wavelength (A,B), Position (outlet), Pump and Rotation.
22. figure: Required tabs for normal operation
After method development (table filled with timings and actions) make sure to save method changes.
Repeat these steps to write individual start, loop and stop methods. Before analysis set up a sequence.
Click on Sequence button and fill table as you can see below, then save your sequence.
23. figure: Setup of sequence
Before you run an analysis you have to initiate devices (click on Method >Init Device or press Alt+I).
Ready state is useful for stabilization of devices (warming up, settle signals, etc.) and you can observe
this process at real time. You can change devices' parameters now through Devices' On-line
Configuration dialog (click on Method >Online configuration or press F10). If ready state is set it is
possible to start analysis. Choose Method >Run menu item or choose Run analysis menu item from
context menu to start analysis manually.
For more see Software manual for detailed usage of software.
Make sure that input liquids are connected to the gradient box and are in adequate amount and quality
for the operation. Connect waste container to fraction collector output 1 and connect fraction vessels
if necessary.
Normal operation of the instrument
The timing tab of the GUI is responsible for the order of the sequences. Normally it consists of 3 steps:
■Start –startup of the instrument (detector wavelength, filling with stationary phase, spin up
of rotor)
■Loop –injection cycle (injection, elution, fraction collection, extrusion)
■Stop –stopping of the instrument
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Method creating in the software
Before the method creating the operator prepared and connected the solvents and the dissolved
sample to the rCPC. The gradient box inlet connections are the next:
•connect the mobile phase to the A line
•connect the stationary phase to the B line
•connect the sample to the C line
Firstly, the operator has to write a start method. In the start method filling up the rotor with
stationary phase and set up the detector wavelength. The end of the start method the set up speed
of the rotor has to be the operating speed.
24. figure: Start method writing
Secondly, the operator has to write a loop method. In the loop method inject the dissolved and
filtered crude with the gradient box C line. Thereafter pumping mobile phase around the same
volume, then the rotor total volume. This called elution. If the main component come down during
the elution, then collect it in the fraction bottles. See in the position column collect fraction from 2
to 10. After the elution pumping stationary phase. It is necessary to refresh the column with fresh
clean solvent and push down the all components from the sample what stayed in the stationary
phase. This called extrusion.
Table of contents
