SSI BINARY SOLVENT DELIVERY MODULE 90-2581 REV B, BINARY SOLVENT DELIVERY MODULE Operator's Manual

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Binary Solvent Delivery Module

Dual Series-III Pumps with Serial PC and Voltage Control

Operator's Manual

90-2581 rev B

Scientific Systems, Inc. 349 N. Science Park Road State College,

6803

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1. INTRODUCTION

This operator's manual contains information needed to install, operate, and
perform minor maintenance on the Binary Solvent Delivery Module. The
figures below are for reference of items described in the manual.

Power

Switch

“T” With

Outlet

Left

Drawer

Control

ads

Ke

Prime Purge

alves

Cooling

Fan

Outlet
Filters

Right

Drawer

Power

Entr

Auxiliary I/O

oltage Control, etc.

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RS-232

Serial Ports

1.1 Description of the Binary Solvent Delivery Module

The system consists of two Series III high performance metering
pumps, in a compact package with pulse dampener and an off-line
pressure transducer. The pumps use a drawer system for easy access to
internal components for troubleshooting & service. These features
allow for:

f Fast & easy setup:

 Two inlet connection (from solvent reservoirs)
 One outlet connection (to injector)

All connections accessible from front panel

f Modular:

 Can be added to any system

f All Stainless steel or PEEK Fluid path, including pumps, valves

and fittings

f Modular pump bays for easy replacement and maintenance

f Self flushing pump heads for extended seal life and reduced

maintenance

f Pulse Dampener for reduced pulsation.

f Very high performance/price ratio

f Easily user adjustable process set points (flow rate, pressure. etc.)

via front key pads
f Digital readout of process parameters
f User settable upper/lower pressure and temperature limits
f RS-232 serial PC interface
f Compact size—Requires only 11 inches of bench space

The low pulsation flow produced by the reciprocating, single­piston pump is achieved by using an advanced rapid-refill cam design,
programmed stepper motor acceleration, and an internal pulse damper.

1.1.1 Pump Features

They include:

• Rapid refill mechanism to reduce pulsation

• Stainless Steel or PEEK™ pumps head

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• LED front panel readout of flow rate, pressure and upper/lower

pressure limits

• Flow adjustment in 0.001 ml increments, from 0.001 to 5.000

ml/min with a precision of 0.2% RSD (5mL/min heads)

Flow adjustment in 0.01 ml increments, from 0.01 to 10.00

ml/min with a precision of 0.2% RSD (10mL/min heads)

• Microprocessor advanced control

• Digital stepper motor design to prevent flow rate drift

over time and temperature

• Back panel RS232 serial communications port for

complete control and status monitoring

• Remote analog inputs (e.g. voltage) to control flow rate

1.1.2 Wetted Pump Materials

Pump heads, check valve bodies, and tubing are made out Stainless
Steel or PEEK™. Other materials are synthetic ruby and sapphire
(check valve internals and piston).

1.1.3 Self-Flushing Pump Head

Self-flushing pump heads provide continuous washing of the piston
surface without the inconvenience of a manual flush or gravity feed
arrangement. The self-flushing pump head uses a diaphragm and
secondary set of check valves to create a continuous and positive flow
in the area behind the high pressure pump seal. The flushing solution
washes away any buffer salts that have precipitated onto the piston.
If not removed, these precipitates can abrade the high pressure seal
and cause premature seal failure, leakage, and can possibly damage the
pump.

MOBILE

PHASE

SAPPHIRE

PISTON

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FLOW OF

FLUSH SOLUTION

HIGH-PRESSURE SEAL

PRIMARY

SECONDARY

SELF-FLUSH SEAL

Figure 1-1. Self-Flushing Pump Head

PISTON
MOVEMENT

1.1.4 Self-Flush and Seal Life

It is recommended that the Self Flush feature be used to improve
seal life in a number of applications. In particular, (as stated above) if
pumping Buffers, Acids/Bases or any inorganic solution near
saturation, the pump should utilize the Self Flush feature. With every
piston stroke, an extremely thin film of solution is pulled back past the
seal. If this zone is dry (without use of Self Flush), then crystals will
form with continuous operation, which will ultimately damage the
seal.

Another application where Self Flush is highly recommended is
when pumping Tetrahydrofuran (a.k.a. THR, Diethylene Oxide) or
other volatile solvents such as acetone (Note: THF and most solvents
are compatible only with all-Stainless Steel systems. THF will attack
PEEK). Volatile solvents will dry rapidly behind the seal (without the
use of Self Flush), which will dry and degrade the seal.

IPA, Methanol, 20% IPA/water mix or 20% Methanol/water mix
are good choices for the flush solution. Consult the factory for
specific recommendations.

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1.2 Specifications for the Binary Solvent Delivery Modules

Flow Rates ............0.000 to 5.000 mL/min for 5mL/min heads

0.00 to 10.00 mL/min for 10mL/min heads

Pressure ................ 0 to 6,000 p.s.i. for SS pump heads,

0 to 5,000 p.s.i. for PEEK™ heads,

Pressure Accuracy… .± 1% of full-scale pressure
Pressure Zero Offset. .± 2 p.s.i.

Flow Accuracy........± 2% for a flow rate of 0.20 mL/min and

above.

Flow Precision .......0.2% RSD

Dimensions ............9" high x 10.5" wide x 18.5" deep

Weight ...................34 lb

Power .................... 90-260 VAC, 50-60 Hz, 45W (The main

voltage supply shall not exceed ±10%)
Environmental……..Indoor use only
Altitude……………..2000 M
Temperature………10 to 30° C
Humidity……………20 to 90% Relative humidity

Remote Inputs . . . . RS-232, Voltage, Frequency

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2. INSTALLATION

2.1 Unpacking and Inspection

Prior to opening the shipping container, inspect it for damage or
evidence of mishandling. If it has been damaged or mishandled, notify
the carrier before opening the container. Once the container is opened,
inspect the contents for damage. Any damage should be reported to the
carrier immediately. Save the shipping container. Check the contents
against the packing list.

2.2 Location/Environment

The preferred environment for the Binary Solvent Delivery
Module is normal laboratory conditions. The area should be clean and
have a stable temperature and humidity. The specific temperature and
humidity conditions are 10 to 30 °C and 20% to 90% relative
humidity. The instrument should be located on a stable flat surface
with surrounding space for ventilation and the necessary electrical and
fluid connections.

2.3 Fluid Connections & Priming
There are only four connections to be made.

1. Connect left drawer pump solvent line supplied

2. Connect right drawer pump solvent line supplied

3. Connect line to injection valve from outlet “T”

4. Next, install the self flush. Connect the self flush inlet and
outlet (opaque) tubing as shown on the the next page.

Details on the proper installation of tubing and priming of the
pump and self flush is shown on the next page.

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SELF-FLUSH

PUMP

Connect wash solution inlet and
outlet tubing
(opaque) to the flush housing as

shown.

Make sure ferrule is in the correct
position.

Screw syringe on luer fitting.
Insert wash outlet tubing end
into clear adapter.

Connect pump inlet tubing as
shown.

Make sure ferrule is in the
correct
position.

Ensure inlet line filter is
submersed into solvent.

Attach syringe to Prime-Purge
valve.

Open Prime-Purge valve by
turning knob counterclockwise
two turns.

Draw syringe back to prime.
Draw on syringe until no

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2.4 Electrical Connection

The system utilizes Universal Switching Power Supply, and will
accept voltages from 90 – 260 VAC, 50-60 Hz.

WARNING: Do not bypass the safety ground connection as
a serious shock hazard could result.

2.5 Solvent Preparation

Proper solvent preparation will prevent a great number of pumping
problems. The most common problem is bubble formation, which may
affect the flow rate consistency. Aside from leaky fittings, the problem
of bubble formation arises from two sources: solvent out-gassing and
cavitation. Filtration of HPLC solvents is also required.

2.5.1 Solvent Out-gassing and Sparging

Solvent out-gassing occurs because the mobile phase contains
dissolved atmospheric gases, primarily N2 and O2. These dissolved
gases may lead to bubble formation and should be removed by
degassing the mobile phase before or during use. The best practical
technique for degassing is to sparge the solvent with standard
laboratory grade (99.9+%) helium. Helium is only sparingly soluble
in HPLC solvents, so other gases dissolved in the solvent diffuse into
the helium bubbles and are swept from the system. Solvent filtration is
not an effective alternative to helium degassing.

It is recommended that you sparge the solvent vigorously for 10 to
15 minutes before using it. Then maintain a trickle sparge during use
to keep atmospheric gases from dissolving back into the mobile phase.
The sparged solvent must be continually blanketed with helium at 2 to
3 psi. Non- blanketed, sparged solvents will allow atmospheric gases
to dissolve back into the mobile phase within four hours.

Solvent mixtures using water and organic solvents (like methanol or
acetonitrile) hold less dissolved gas than pure solvents. Sparging to
reduce the amount of dissolved gas is therefore particularly important
when utilizing solvent mixture.

Even with sparging some out-gassing may be occur. A back
pressure regulator installed after the detector flow cell will help
prevent bubbles from forming and thus limit baseline noise.

WARNING: Always release pressure from the pump slowly. A rapid
pressure release could cause the pulse damper diaphragm to rupture.

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2.5.2 Cavitation

Cavitation occurs when inlet conditions restrict the flow of solvent
and vapor bubbles are formed during the inlet stroke. The key to
preventing cavitation is to reduce inlet restrictions. The most common
causes of inlet restrictions are crimped inlet lines and plugged inlet
filters. Inlet lines with tubing longer than 48" (120 cm) or with tubing
of less than 0.085" (2 mm) ID may also cause cavitation.

Placing the solvent reservoirs below the pump level also promotes
cavitation. The optimal location of the reservoirs is slightly above the
pump level, but it is adequate to have them on the same level as the
pump.

2.5.3 Filtration

Solvent filtration is good practice for the reliability of the Binary
Solvent Delivery Module and other components in a HPLC system.
Solvents should always be filtered with a 0.5 micron filter prior to use.
This ensures that no particles will interfere with the reliable operation of
the piston seals and check valves. Solvents in which buffers or other salts
readily precipitate out will need to be filtered more often. After filtration,
the solvents should be stored in a closed, particulate-free bottle.

2.5.4 Initial system pressurization (Daily)

IMPORTANT: To maximize accuracy at all pressures and flows
this pump contains a pulse damper for each solvent used. It is
important that the pump be brought to pressure with both pumps
running to insure that each pulse damper has the correct solvent in it.
It is recommended that the flow be set to the operational flow with an
equal mixture of the two solvents. Once the system has reached a
constant pressure the composition should be set to the initial
conditions.

2.6 Instrument Installation

2.6.1 Mobile Phase Reservoirs

The mobile phase reservoir should be placed at the same level or
slightly higher than the pump, never below the pump, and the inlet
tubing should be as short as practical. These steps minimize pressure
losses on the inlet side of the pump during refill and help to avoid
bubble formation. These steps are particularly important when using
high vapor pressure solvents (hexane, methylene chloride, etc.).
Mobile phases should be degassed, filtered and covered. (See Section

2.4.)

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2.6.2 Self-Flush Solution

Self-flush heads require 250-500 mL of flushing solution. See
section 1.1.4 for self-flush solution recommendations. A pH indicator
that will indicate the concentration of salts in the solution is
recommended as a reminder to change the solution. This flush solution
should be replaced with a fresh solution weekly to avoid frequent
pump maintenance.

2.6.3 Inlet Tubing and Filters

The table below shows the inlet tubing and filter used in the Binary
Solvent Delivery Module. All inlet lines are supplied in a 30" (76 cm)
length and are made of a fluoropolymer material.

2.6.4 Priming the Pump and the Flushing Lines

Connect a syringe to the outlet tubing. Run the pump at a flowrate
of 3 to 5 ml/min. Prime the pump by pulling mobile phase and any air
bubbles through the system and into the syringe (a minimum of 20
ml).

To prime the flush lines for a self-flush head, simply place the inlet
line in the flush solution and connect a syringe to the outlet line and
apply suction until the line is filled with flush solution. Place the
outlet line in the flush solution. Secure both flush lines in the flush
solution container so they stay immersed during pump operation.

2.6.6 Long Term Pressure Calibration Accuracy

This note applies if your pump is equipped with an electronic
pressure transducer. The transducer has been zeroed and calibrated at
the factory. Over the life of the pump, some drift may occur. For
example, it is typical for the zero to drift < 10 p.s.i. after about 1 year
of operation (i.e., with no back pressure on the pump a reading of 1-9
p.s.i. may be displayed). A similar drift may also occur at higher
pressures, and are typically less than 1% (e.g. <50 p.s.i. at 6,000 p.s.i.
back pressure).

If pressure calibration and/or drift is a concern, consult the factory.
The pump can be shipped back to SSI for recalibration. Alternatively,
written calibration and zero-reset procedures are available. Consult the
factory to receive these instructions.

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2.7 Preparation for Storage or Shipping

2.7.1 Isopropanol Flush

Disconnect the outlet tubing from the pump. Place the inlet filter in
isopropanol. Use a syringe to draw a minimum of 50 ml through the
pump. Pump a minimum of 5 ml of isopropanol to exit. Leave the inlet
tubing connected to the pump. Place the inlet filter in a small plastic
bag and attach it to the tubing with a rubber band. Plug the outlet port
with the shipping plug or leave a length of outlet tubing on the pump
or cover the outlet port with plastic film.

2.7.2 Packaging for Shipping

CAUTION: Reship in the original carton, if possible. If the original carton is
not available, wrap the pump in several layers of bubble wrap and cushion the
bottom, top, and all four sides with 2" of packaging foam. Although heavy, an
HPLC pump is a delicate instrument and must be carefully packaged to
withstand the shocks and vibration of shipment.

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3. OPERATION

3.1 Pump Front Panel Controls and Indicators

3.1.1 Control Panel

3.1.1.1 Digital Display

The 3-digit display shows the pump flow rate (mL/min), system
pressure (psi), or the set upper or lower pressure limit (psi) when
operating. Choice of display is selected with the MODE key.

3.1.1.2 Digital Display Pump Keypad

∆

∇

MODE

RUN

STOP

Fast And Slow Button Repeat On The Up And Down Arrow Buttons:
If the UP-ARROW or DOWN-ARROW button is held down for more
than approximately one half of a second, the button press will repeat at
a slow rate of approximately 10 times a second. Once slow button
repeat has begun, fast button repeat can be initiated by using a second
finger to press down the second arrow button. During fast button
repeat, the button press will repeat at a rate of approximately 100
times a second. Switching back and forth between repeat speeds can
be accomplished by pressing and releasing the second arrow button
while keeping the first arrow button held down.

When pressed, this button increases the flow rate.

When pressed, this button decreases the flow rate.

Use this button to cycle through the four display modes: flow rate,
pressure, upper pressure limit, or lower pressure limit. A status LED
to the right of the digital display indicates which mode is active.

When pressed, this button alternately starts and stops the pump.

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3.1.1.3 Status LEDs

Q ml/min

Q PSI

Q HI PR

Q LO PR

Q RUN

Q FAULT

When lit, the digital display shows flow rate in mL/min.

When lit, the digital display shows system pressure in psi.

When lit, the display shows the user-set upper pressure limit in psi.

When lit, the display shows the user-set lower pressure limit in psi.

Lights to indicate that the pump is running.

Lights when a fault occurs and stops the pump.

3.1.1.2 Power-up Configuration

Non-volatile Memory Reset: If the pump is operating erratically,
there is the possibility that the memory has been corrupted. To reset
the memory and restore the pump to it's default parameters, press and
hold the UP-ARROW button when the power is switched on. Release
the button when the display reads "rES". The parameters stored in
non-volatile memory, i.e., the flowrate, the pressure compensation, the
voltage/frequency select, the lower pressure limit, and the upper
pressure limit will be set to the factory default values. The head type
setting is the only parameter not changed by the non-volatile memory
reset function. If the firmware is upgraded to a newer version, a non­volatile memory reset will automatically occur the first time the power
is switched on.

3.1.1.5 Power-Up Tests

Display Software Version Mode: The software version can be
displayed during power-up by pressing and holding the RUN/STOP
and the UP-ARROW buttons when the power is switched on. Release
the buttons when the display reads "UEr". The decimal point number
displayed on the display is the software version. To exit this mode,
press the RUN/STOP button.

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