Schambeck SDS 9414I User manual

SDS 9414I HPLC Pump

SDS 9414i HPLC Pump
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TABLE OF CONTENTS
1. Standard Accessories......................................................................................................... 5
1.1 Stainless Steel Version.................................................................................................................................... 5
1.2 PEEK Version.................................................................................................................................................. 5
2. Safety Instructions.............................................................................................................. 6
2.1 General Electrical Hazards.............................................................................................................................. 6
2.2 General Precautions........................................................................................................................................ 6
3. Technical Specifications .................................................................................................... 7
4. General Description ............................................................................................................ 8
4.1 Working Principle............................................................................................................................................. 8
4.2 Front Side View ............................................................................................................................................. 10
4.2.1 Pump Components ................................................................................................................................. 11
4.3 Rear Panel View............................................................................................................................................ 12
4.4 Function Connectors ..................................................................................................................................... 13
4.4.1 Remote Control (4) ................................................................................................................................. 13
4.4.2 RS232 Serial Interface (5) ...................................................................................................................... 13
4.4.3 Pressure Connector (6) .......................................................................................................................... 14
5. Menu Description.............................................................................................................. 15
5.1 Overview........................................................................................................................................................ 15
5.1.1 Input of Parameters ................................................................................................................................ 15
5.2 Flow Rate....................................................................................................................................................... 15
5.2.1 Constant Pressure .................................................................................................................................. 15
5.2.2 Maximum Flow........................................................................................................................................ 16
5.3 Minimum Pressure Threshold........................................................................................................................ 16
5.4 Maximum Pressure Threshold....................................................................................................................... 16
5.5 Compressibility .............................................................................................................................................. 17
5.6 Analyses Time............................................................................................................................................... 18
5.7 Delay Time..................................................................................................................................................... 18
5.8 Start Delay Time............................................................................................................................................ 18
5.9 Stop Delay Time............................................................................................................................................ 19
6. Instrument Setup............................................................................................................... 20
6.1 Check Voltage ............................................................................................................................................... 20
6.2 Capillary Connections.................................................................................................................................... 20
6.3 Priming the Pump.......................................................................................................................................... 20
7. Instrument Operation........................................................................................................ 22
7.1 Operation Conditions..................................................................................................................................... 22
7.1.1 Error Messages....................................................................................................................................... 22
7.2 Operation Modes ........................................................................................................................................... 24
7.2.1 Constant Flow Mode............................................................................................................................... 24
7.2.2 Constant Pressure Mode ........................................................................................................................ 25
7.3 Power Down Feature..................................................................................................................................... 26
8. Compressibility ................................................................................................................. 27
9. Service & Maintenance..................................................................................................... 30
9.1 Troubleshooting............................................................................................................................................. 30

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9.2 Exchange of Pump Head............................................................................................................................... 31
9.3 Pump Head Assembly................................................................................................................................... 32
9.3.1 Piston Back Flushing .............................................................................................................................. 33
9.3.2 Change of Piston Ring............................................................................................................................ 33
9.3.3 Replacing the Check Valves................................................................................................................... 33
9.3.4 Cleaning the Valve Cartridges................................................................................................................ 33
9.4 Software Initialization..................................................................................................................................... 36
9.4.1 Instrument Configuration Menu .............................................................................................................. 36
10. Serial Control Interface................................................................................................... 39
10.1 Hardware ..................................................................................................................................................... 39
10.1.1 Communication Parameters ................................................................................................................. 39
10.2 Command List.............................................................................................................................................. 39
10.2.1 Command Format................................................................................................................................. 39
10.2.2 Command Synchronization................................................................................................................... 42
10.2.3 Safety Feature ...................................................................................................................................... 42
11. Spare Parts & Accessories............................................................................................. 43
11.1 General Spare Parts.................................................................................................................................... 43
11.2 Pump Head Spare Parts.............................................................................................................................. 43
11.2.1 Analytical, General................................................................................................................................ 43
11.2.2 Analytical, Stainless Steel..................................................................................................................... 43
11.2.3 Analytical, PEEK................................................................................................................................... 44
11.2.4 Semi-Preparative, General ................................................................................................................... 44
11.2.5 Semi-Preparative, Stainless Steel........................................................................................................ 44
11.2.6 Semi-Preparative, PEEK ...................................................................................................................... 44
11.2.7 Micro, General ...................................................................................................................................... 45
11.2.8 Micro, Stainless Steel ........................................................................................................................... 45
11.2.9 Micro, PEEK.......................................................................................................................................... 45
11.3 Check Valve Parts ....................................................................................................................................... 45

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PICTURE INDEX
Picture 1: Working Principle...................................................................................................................................... 8
Picture 2: Front Side View....................................................................................................................................... 10
Picture 3: Pump Components ................................................................................................................................. 11
Picture 4: Rear Panel .............................................................................................................................................. 12
Picture 5: Status Display -Constant Flow Mode..................................................................................................... 24
Picture 6: Status Display -Constant Pressure Mode.............................................................................................. 25
Picture 7: Pump Head Assembly ............................................................................................................................ 32
Picture 8: Check Valve Assembly........................................................................................................................... 34
Picture 9: Check Valve Cross-Cut........................................................................................................................... 35
Picture 10: Checksum Formula............................................................................................................................... 40

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1. STANDARD ACCESSORIES
1.1 STAINLESS STEEL VERSION
§1 piece HPLC Pump SDS 9414I
§1 piece Operation Manual
§1 piece Power Cord
§2 pieces Fuses 0.5 A for 220 V; 1.0 A for 110 V
§1 piece Wrench ¼” x 5/16”
§1 piece Wrench 13 x 15 mm
§1 piece Allen Wrench 3 mm
§1 piece Allen Wrench 2.5 mm
§2 pieces Fittings with Ferrules (Stainless Steel)
§1 piece Plastic Syringe
§1 piece PTFE Tubing 1.6x3.2 mm I.D. for the pump suction capillary tube
§1 piece Capillary Tube (Stainless Steel)
1.2 PEEK VERSION
§1 piece HPLC Pump SDS 9414I
§1 piece Operation Manual
§1 piece Power Cord
§2 pieces Fuses 0.5 A for 220 V; 1.0 A for 110 V
§1 piece Wrench ¼” x 5/16”
§1 piece Wrench 13 x 15 mm
§1 piece Allen Wrench 3 mm
§1 piece Allen Wrench 2.5 mm
§2 pieces Hexagonal Fittings (PEEK)
§2 pieces Double Cone (PEEK)
§1 piece Plastic Syringe
§1 piece PTFE Tubing, 1.6 x 3.2 mm I.D. for the pump suction capillary tube
§1 piece Capillary Tube, 0.25 x 1.59 mm (PEEK)

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2. SAFETY INSTRUCTIONS
The manufacturer, does not warrant for any defects or damage resulting from incorrect
operation and maintenance, non-observance of the manual's instructions and negligence
during installation.
Before putting the instrument into operation, read the manual carefully and should there be
any further questions, please get in contact with your supplier.
2.1 GENERAL ELECTRICAL HAZARDS
§Check actual line voltage to confirm that the set voltage (on the rear side; voltage
selector and fuse carrier) of the instrument is correct.
§Before changing the instrument's voltage or before changing defect fuses, disconnect
the instrument from all power sources.
§The instrument has to be plugged into grounded wall sockets only.
§This instrument can be used only with other instruments which comply with the general
safety regulations.
§Connect all cable connections before switching on the instrument.
2.2 GENERAL PRECAUTIONS
§In order to avoid any damages, perform periodic leak checks on all installed supply
lines.
§The instrument is only allowed to be used for applications with specifications described
in this manual.
§For toxic solvents, follow a regulated and approved waste disposal program. Never
dispose of such products through the municipal sewage system.
§The instrument is suitable for operation between 10° C and 35° C surrounding
temperature.
§Flammable fluids are not to be used with this instrument.

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3. TECHNICAL SPECIFICATIONS
Flow Rate Micro:0.02–4.00 ml/min
Analytical:0.05 –9.95 ml/min
Semi-Preparative:0.20 –40.0 ml/min
Pump Head Material:Stainless Steel, PEEK, or Titanium
Pulsation:less than 1.0 %
Flow Accuracy:less than 0.1 %
Flow Precision:less than 1.0 %
Max. Pressure 40 MPa (400 bar)
Display:Alphanumeric, 2x20 characters LCD
Compressibility Factor: selectable from 0.7 to 1.0
Operation Mode: constant flow or constant pressure
Remote Control Analog: Flow Rate (0-10V); Start, Stop
Digital: RS232
Programmable Runtime: 00:01 to 99:59 h
Programmable Delay Time: 00:01 to 99:59 h
Safety Control: Min./Max. Pressure
Power Supply:220/110 Volt; 50/60 Hz
Dimensions:258 x 148 x 350 mm
Weight:8kg

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4. GENERAL DESCRIPTION
4.1 WORKING PRINCIPLE
The HPLC Pump SDS 9414I is a dual piston solvent delivery system. The mechanism is
designed with short piston stroke technology and only two check valves. This results in the low
pulsation of a dual piston pump combined with the reliability of a single piston pump.
Difficulties in solvent delivery systems caused mainly by malfunctioning of the valves.
The delivery piston of the standard analytical unit works with a 2 mm stroke length, the
compensation piston with 1 mm. The nearly pulse less solvent delivery of the SDS 9414I
results from the high stroke frequency and the use of the compensation piston. The two
pistons are contra rotating installed.
Picture 1: Working Principle

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While the delivery piston pushed the solvent volume out, the compensation piston, located on
the pressure side, collects half of the volume. During return movement of the delivery piston,
the collected volume is pumped from the compensation. The microprocessor controlled speed
regulation leads to a highly stable speed of the D.C. motor. Contrary to standard regulators,
the microprocessor is able to correct continuously the compressibility of the eluents through a
computerized program. This results in a constant volume delivery throughout the entire
delivery range.
The microprocessor technology also offers the possibility to handle the programming,
application and controlling of an instrument in a simple manner. Through the alphanumeric
display the instrument parameters are shown in clear letters. The user can easily control or
change the data. To simplify operation, the function keys are kept at a minimum.
There is basically the choice between two operation modes. The delivery with “constant flow”
and the delivery with “constant pressure”. According to the individual modes, the following
parameters can be programmed:
§Constant Flow in ml/min
§Constant pressure in MPa
§Min. Pressure Threshold
§Max. Pressure threshold
§Maximum Flow
§Compressibility Factor
§Max. Run Time
§Delay Time
§Programmable Start Delay
§Programmable Stop Delay
The HPLC pump is equipped with a built-in diagnostic system. This continuously controls the
following parameters:
§Power Failure
§Program Memory
§Max./Min. Pressure
§Max. Flow
§Motor Function
Illogical data entered by the operator will be ignored by the processor’s logic control and
signalized by flashing the display.

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4.2 FRONT SIDE VIEW
All parts necessary for the operation are positioned on the front side of the instrument.
Picture 2: Front Side View
1
2x20 Character LCD
2
Keyboard
3
Status Indicator Lights
4
Relief Valve
5
Pump Head

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4.2.1 PUMP COMPONENTS
Picture 3: Pump Components
1
Suction valve housing (connect from eluent reservoir)
2
Pump head (letter on pump head denotes type: a = analytical; m = micro;
p = preparative)
3
Mounting screws (4)
4
Pressure valve housing
5
Connecting capillary –damping piston
6
Connecting capillary –pressure sensor
7
Purge valve
8
Venting screw (PEEK)
9
Drain capillary (Purge valve)
10
Solvent outlet (connect to injector)

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4.3 REAR PANEL VIEW
Picture 4: Rear Panel
1
Main Switch
2
Power Cord Plug
3
Fuse Carrier w. Voltage Selector
4
REMOTE CONTROL connector (15 pins)
5
RS-232 Connector
6
PRESSURE OUT Connector

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4.4 FUNCTION CONNECTORS
4.4.1 REMOTE CONTROL (4)
PIN FUNCTION
1EXTERN -
2ERROR N.C.
3Internal use
4Internal use
5START /STOP
6RUN RELAY COM
7ERROR COM
8COM
9EXTERN +
10 RUN RELAY N.C.
11 INSTALLED-J
12 HIGH PRESSURE J.
13 REMOTE J.
14 RUN RELAY N.O.
15 ERROR N.O.
4.4.2 RS232 SERIAL INTERFACE (5)
PIN FUNCTION
1DCD
2RXD
3TXD
4DTR
5GND
6DSR
7RTS
8CTS
9RI

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4.4.3 PRESSURE CONNECTOR (6)
PIN FUNCTION
1Pressure -
2-
3Pressure + (10 mV / 1 MPa)

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5. MENU DESCRIPTION
5.1 OVERVIEW
The menu dialog can be activated if the pump is in the standby mode; indicated by the STOP
LED. To activate, push the [PROG]key. The program menu can be stepped through by using
the [PROG] key. The programming cycle can be terminated at any time by pushing the [STOP]
key.
5.1.1 INPUT OF PARAMETERS
The input and any change of existing parameters is done interactively.
If values have to be set or changed, this can be done by using the [p]key for increasing the
number and using the [q]key for decreasing the number. By pushing the [p]or [q]key for a
short time, the value will change with the smallest possible increment. By keeping the key
pressed, the numbers will increase more rapidly.
5.2 FLOW RATE
By pushing the [PROG]key the programming dialog is started. The display shows:
The value for the flow rate can be set to any wanted number by using the [p]or [q]key.
By pressing once for a short time the value will change in 0.05 increments for the analytical
head; in 0.01 increments for the micro head and in 0.2 increments for the preparative head.
By holding the [p]or [q]key pressed down the speed of changing the numbers will increase.
By reaching the maximum possible flow rate for a mounted head, the value will not increase
anymore and the display will start to twinkle.
When the flow rate is set to 0.0 ml/min, the pump is set to CONSTANT PRESSURE mode. In
this case, the next two menus can be switched through to set the CONSTANT PRESSURE
mode parameters.
After the correct flow rate is selected, the [PROG]key has to be pushed again. This fixes the
set value in the memory and switches the program to the next step.
5.2.1 CONSTANT PRESSURE
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:

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By pushing the [PROG]key this value will be fixed into the memory and the next program step is
called up.
5.2.2 MAXIMUM FLOW
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:
This step is built in as a safety feature to avoid any damage of the analyzer by reaching a too
high flow rate.
The desired maximum flow rate can be set by using the [p]or [q]key.
5.3 MINIMUM PRESSURE THRESHOLD
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:
At this step the minimum pressure level can be set. Any value from 0.0, but no higher than the
maximum level. A practical level is a value of about 20 % of the normal operation pressure.
After setting the wanted level by using the [p]or [q]key, the [PROG]key has to be used to
fix this value in the memory and to activate the next program step.
5.4 MAXIMUM PRESSURE THRESHOLD
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:

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These 40 MPa (400 bar or 6000 PSI) are indicating the pressure of the pump. The maximum
pressure level should be set to a level which ensures to avoid any damage of the whole
HPLC-system if a blockage of any part may occur. Always the weakest part has to be used for
selecting the correct level.
The selected maximum level has to be set by using the [p]or [q]key. The maximum level
cannot be set to a level below the low pressure level.
Activation of the [PROG]key stores the value into the memory and activates the next
programming step.
5.5 COMPRESSIBILITY
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:
The pump software contains a calculation program for correcting the pressure depending on
compressibility of solvents. The factor 1.0 has to be set when compressible solvents like water
are used. (For further details see 8. Compressibility). For changing the factor, which can be
set from 0.5 to 1.0, the [p]or [q]keys have to be used.
After selecting the correct factor, the [PROG]key has to be pushed to fix this value into the
memory and to call up the next programming step.

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5.6 ANALYSES TIME
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:
As the pump is able to count times, the requested run time can be selected in this step. If the
time is set to 0:0 the pump will start to run after pushing the [START]key and will stay under
this condition until the [STOP]key will be pushed.
If a time is selected, e.g. for a run time of 15 minutes "0:15", the display will show this value
after starting the pump by pushing the [START]key. The preset value will count down to "0:0".
After reaching zero the pump will stop automatically. A relay closure contact, available through
the interface connector can be used to stop also the peripheral equipment.
The analyses Time can be selected by using the [p]or [q]key for a time range from 00:01 to
99:59 h:min. The time will be fixed into the memory and the next program step is selected by
pushing the [PROG]key.
5.7 DELAY TIME
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:
Similar to the Analysis Time a Delay Time can be programmed. This Delay Time can be
selected from 00:01 to 99:59 h:min. The display will show the pre-selected value after
pushing the [START]key and will count down to 0:0. After reaching zero, the pump will start to
run. During the delay time the green LED within the [START]key will twinkle.
A relay closure contact, available through the interface connector, can be used to start also
the peripheral equipment. For setting the correct Delay Time the [p]or [q]key has to be
used, and the [PROG]key to fix the value into the memory and to activate the next
programming step.
5.8 START DELAY TIME
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:

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The HPLC pump SDS 9414I has a built-in start delay time function which protects and
therefore prolongs column's durability as a careful increase of pressure onto the column is
possible.
During the start delay time operation, the display shows the symbol “^” right before the RT.
The start delay time can be selected for a time range of up to 2 min 30 sec at a maximum.
The time value is selected by using the [p]or [q]key. The [PROG]key has to be pushed to
fix the value into the memory and to activate the next programming step.
5.9 STOP DELAY TIME
By pushing the [PROG]key the programming dialog is switched to the next menu. The display
shows:
The HPLC pump SDS 9414I has a built-in stop delay time function which protects and
therefore prolongs column's durability as a careful decrease of pressure onto the column is
possible.
During the stop delay time operation, the display shows the symbol “v” right before the RT.
The stop delay time can be selected for a time range of up to 2 min 30 sec at a maximum.
The time value is selected by using the [p]or [q]key. The [PROG]key has to be pushed to
fix the value into the memory and to leave the PROGRAMMING MODE.

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6. INSTRUMENT SETUP
6.1 CHECK VOLTAGE
Before connecting the pump to the mains, check the voltage shown on the type plate on the
rear of the instrument. This voltage should be identical with the voltage of the existing power
source. If the voltage is correct, connect the instrument with the enclosed power cord.
If necessary, the voltage has to be changed accordingly:
§pull out the voltage selector
§check the fuses inside the fuse carrier; if necessary exchange the fuses (the needed
fuse type is printed on the back panel of the instrument; 0.5A for 220V, 1.0A for 110V)
§Turn the voltage selector back in the power supply connector; make sure that the small
arrow points to the right voltage
6.2 CAPILLARY CONNECTIONS
§Connect the enclosed PTFE tubing (1.6 x 3.2 mm I.D.) to the pump’s suction inlet. Put
the end of the PTFE tubing into your eluent reservoir.
§Connect the relief valve outlet to the injection valve and/or autosampler with the
enclosed stainless steel/PEEK capillary.
§then the pump can be switched on
§connect the enclosed plastic syringe to the outlet capillary of the relief valve.
6.3 PRIMING THE PUMP
During the final quality control the pump is tested with Propanol. When setting up for operation
and later when changing solvents, care must be taken to ensure solvent miscibility to avoid
malfunctioning of the check valves. When changing immiscible solvents e.g. methanol-
hexane, the pump should be flushed with an intermediate solvent that is miscible with both,
e.g. chloroform.
The solvents should be degassed carefully before use, as air bubbles within the pump head
will create an unstable delivery of solvents by the pump. The most effective way of degassing
is by bubbling helium through the solvent. Storing the solvents at 0.5 to 1 bar after degassing,
a steady flow from the pump will be ensured. Under these conditions the solvents will be
delivered to the pump inlet better than by gravity alone. Sucking of eluents by the pump may
create air bubbles in the tubing. If helium is not available, heating of the solvent and stirring, as
well as ultrasonic treatment are also very well tested methods for solvent degassing. Many
problems associated with HPLC-systems arise from insufficiently degassed solvents.
Open the relief valve (one turn counter-clockwise). Then, with the help of the syringe, suck on
slowly approx. 10 ml solvent. Afterwards, remove the syringe and flush by using the purge