Installing the Micro Vacuum Degasser

Installing the Micro Vacuum Degasser

Installing the Micro Vacuum Degasser

Parts required Micro Vacuum degasser

Power cable
Interface cable as ordered, see “Cable Overview” on page 70
Preparation Locate bench space
Provide power connections
Unpack the vacuum degasser module

1 Place the micro vacuum degasser on the bench.

2 Ensure the power switch on the front of the micro vacuum degasser is OFF
(switch stands out).
3 Connect the power cable to the power connector at the rear of the micro
vacuum degasser.
4 Connect the interface cable to the micro vacuum degasser. The interface cable
(remote cable) is a one way connection to send a not-ready signal from the
degasser to the other modules to shut down the whole system after an error
condition of the degasser.

NOTE In an Agilent 1100 Series system, the individual modules are connected
through a CAN cable. The Agilent 1100 Series micro vacuum degasser is an
exception. The micro vacuum degasser can be connected via the APG remote
connector to the other modules of the stack. The AUX output allows to
monitor the vacuum pressure in the degasser chamber. An Agilent 1100 Series
control module can be connected to the CAN bus at any of the modules in the
system except for the degasser. The Agilent ChemStation can be connected to
the system through one GPIB cable at any of the modules (except for the
degasser), preferably at the detector. For more information about connecting
the control module or Agilent ChemStation refer to the respective user
manual.

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 Installing the Micro Vacuum Degasser
Installing the Micro Vacuum Degasser

Figure 3 Rear of the Micro Vacuum Degasser

Power socket

Fuse holder

Figure 4 Front of the Micro Vacuum Degasser

Status indicator

Power switch

Waste outlet
Serial number

5 Press in the power switch to turn on the micro vacuum degasser.

NOTE The power switch stays pressed in and a green indicator lamp in the power
switch is on when the micro vacuum degasser is turned on. When the line
power switch stands out and the green light is off, the micro vacuum degasser
is turned off.

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 Installing the Micro Vacuum Degasser
Flow Connections to the Micro Vacuum Degasser

Flow Connections to the Micro Vacuum

Degasser

Parts required Solvent cabinet including solvent bottles (filled with solvent) and bottle head assemblies
Micro Vacuum degasser
Solvent outlet tubes
Syringe with adapter
Preparation Install the micro vacuum degasser

1 Place solvent cabinet with the bottle(s) on top of the micro vacuum degasser.
2 Remove the front cover by pressing the snap fasteners on both sides.

Figure 5 Removing the Front Cover

3 If the micro vacuum degasser is not used with an Agilent 1100 Series pump,
connect the waste tube from the accessory kit to the waste outlet and place
into your waste system.
4 Put the bottle head assemblies into solvent bottles containing your mobile
phase.

WAR NI N G When working on capillary or tube fittings solvents may leak out.
Please observe appropriate safety procedures (for example, goggles,
safety gloves and protective clothing) as described in the material
handling and safety data sheet supplied by the solvent vendor,
especially when toxic or hazardous solvents are used.

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 Installing the Micro Vacuum Degasser
Flow Connections to the Micro Vacuum Degasser

5 Connect the solvent tubes from the bottle head assemblies to the inlet
connectors A through D (typically the upper connection of the channel) of the
micro vacuum degasser. Use the mounting tool shown in Figure 6 to fix the
tube screw. Fix the tubes in the clips of the micro vacuum degasser.

Figure 6 Mounting Tool

6 Connect the outlet tubes to the output ports (typically under connection of the
channel) of the micro vacuum degasser. Use the mounting tool shown in
Figure 6 to fix the tube screw.
7 Prime the degasser before first use (see “Priming the Degasser” on page 29).

NOTE Atmospheric gases can diffuse through the tubing and dissolve in the mobile
phase solvents. For best chromatographic results, keep the length of tubing
between the micro vacuum degasser and your pump as short as possible.

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 Installing the Micro Vacuum Degasser
Flow Connections to the Micro Vacuum Degasser

Figure 7 Flow Connections to the Micro Vacuum Degasser

Bottle Head Assembly

Solvent cabinet

Vacuum Degasser

Inlet tube
Outlet tube

Tube clip

Purge valve
Pump head

Inlet adapter

Waste tubing

Outlet capillary to sampler

MCGV

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 Installing the Micro Vacuum Degasser
Transporting the Micro Vacuum Degasser

Transporting the Micro Vacuum Degasser

WAR NI N G Drain any remaining solvents from the degassing channels before
transporting the micro vacuum degasser.

1 Disconnect the solvent tubes from solvent inlets from front panel.
2 Disconnect one of the solvent tubes from your pump.
3 Connect syringe adapter to solvent tube of this solvent channel.
4 Push syringe adapter onto syringe.
5 Pull syringe plunger to draw solvent out of micro vacuum degasser and tubing.
Continue to draw solvent into syringe until the solvent channel is completely
empty.
6 Repeat step 2 through step 5 for the remaining solvent channels.

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Installing the Micro Vacuum Degasser
Transporting the Micro Vacuum Degasser

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 2

2 Optimizing Performance

How to optimize the micro vacuum degasser to

achieve best chromatographic results
 Optimizing Performance
Introduction to the Micro Vacuum Degasser

Introduction to the Micro Vacuum

Degasser

The micro vacuum degasser comprises a 4-channel vacuum container,

including 4 micro structured membranes, and a vacuum pump. When the
micro vacuum degasser is switched on, the control circuit turns on the
vacuum pump which generates a partial vacuum in the vacuum container.
The pressure is measured by a pressure sensor. The micro vacuum degasser
maintains the partial vacuum by turning on and off the vacuum pump
depending on the signal from the pressure sensor.
The LC pump draws the solvents from their bottles through the special
tubular plastic membranes of the vacuum container. As the solvents pass
through the vacuum tubes any dissolved gas in the solvents permeates
through the membranes into the vacuum container. The solvents will be
almost completely degassed when leaving the outlets of the micro vacuum
degasser.

Figure 8 Overview (only one of the four solvent channels is shown)

Sensor Control Vacuum

circuit pump
Pump

4 micro structured supported

membranes
Solvent

Vacuum container

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Optimizing Performance
When to Use a Micro Vacuum Degasser?

When to Use a Micro Vacuum Degasser?

For capillary LC application with our 1100 Series Capillary LC System

For high-pressure mixing pumps with low flow rates or when you have
following conditions:
• if your detector is used with maximum sensitivity in the low UV
wavelength range,
• if your application requires optimum injection precision
• if your application requires highest retention time reproducibility
(mandatory at flow rates below 0.5 ml/min)
• if your sample or detection is sensitive to dissolved oxygen in the mobile
phase (degradation).
• With a Fluorescence Detector.
Generally a degasser should be used when negative effects due to dissolved
gas in the mobile phase exceed the limits that are acceptable for the user.
Negative effects that can be caused by dissolved gas are:
• Unstable flow due to unstable pumping conditions. This may result in a
high ripple or high standard deviations of peak retention times and peak
areas especially at low flow rates.
• Baseline noise on detectors that are sensitive to changes in the refractive
index.
• Sample degradation.
• Fluorescence Quenching due to dissolved oxygen.
• Baseline drift in electrochemical detectors due to dissolved oxygen
especially in reduction mode.

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 Optimizing Performance
Operation Modes of the Micro Vacuum Degasser

Operation Modes of the Micro Vacuum

Degasser

The micro vacuum degasser allows various operation modes. Operation

mode 1 and 2 are the normal operation modes of the degasser:
• In operation mode 1 the vacuum degasser works at 115 Torr.
• In operation mode 2 the vacuum degasser works in the range between 115
to 190 Torr.
• The continuous mode can be selected for highest degassing efficiency of
the degasser. In this mode the vacuum level is below 115 Torr.
• The error mode is activated in case the degasser cannot achieve a vacuum
level of 190 Torr.
(1 Torr = 1.33x10-3 bar)

Table 4 Operation Modes of the Vacuum Degasser

Operation Mode 1 Operation Mode 2 Continuous Mode Error Mode

Pressure Range [Torr] 115 115 -190 Below 115 Above 190
DC Voltage Readings Lower Limit: 590 - 600 600 - 800 Below 600 Above 800
[mV] (rough values) Upper Limit: 600 - 610
Operation mode Pump switched on and Pump switched on every Pump permanently 8 Minutes of continuous
off at upper and lower 2 minutes for 30 seconds running pumping before
limit during operation shutdown
Status Indicator OFF - below 800 mV OFF - below 800 mV OFF - below 800 mV YELLOW
YELLOW - above 800 mV YELLOW - above 800 mV YELLOW - above 800 mV
Failure Actions Switch to Operation Switch to Error Mode Switch to Error Mode Shut down module,
Mode 2 switch status indicator to
RED

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 Optimizing Performance
Operation Modes of the Micro Vacuum Degasser

NOTE The voltage readings given for the various modes are approximate values. All
values are set in the factory according to the vacuum level. Depending on the
vacuum sensor batch variations this will result in different voltage readings.
Regardless of the readings of the various stages no adjustment should be
performed on the degasser electronics.

NOTE See “Preparing to Measure the Pressure Sensor Readings” on page 41 for
setting up test meter connections to the degasser for reading the pressure
sensor output.

Normal Operation Mode 1

When the degasser is turned on, the vacuum pump runs and is connected to
ambient through the solenoid valve. The solenoid valve activates about
15 seconds after turning on the degasser (you can hear it click). The vacuum
pump then begins to pull a vacuum on the vacuum chamber. The voltage
measurements begin to decrease rapidly.
The yellow status LED turns off when the vacuum level reaches 190 Torr (DC
voltage readings around 800 mV).
The normal operation mode vacuum level (115 Torr) is achieved when the DC
voltage measures approximately 590 to 600 mV.
After achieving the normal operation mode vacuum level, the solenoid valve
turns off. The vacuum pump continues to run for a few seconds, then it turns
off.
When the DC voltage measurement rises back to approximately 600 to
610 mV, the turn on process begins again.
If the vacuum level of normal operation mode one cannot be achieved within
8 minutes the instrument turns into normal operation mode 2.

Normal Operation Mode 2 (Timing Mode)

Under certain operational conditions (large amount of dissolved gas in
mobile phase, high flow rates) the 115 Torr trigger level for operation mode 1
cannot be reached. The vacuum degasser automatically turns into operation
mode 2.
Normal operation mode 2 is a fixed timing mode. Every 2 minutes the
degasser is turned on for 30 seconds. This assures a pressure level in the
range from 115 to 190 Torr. The pressure signal measured with the auxiliary
cable is in the range between 600 to 800 mV.

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 Optimizing Performance
Operation Modes of the Micro Vacuum Degasser

If the vacuum level of normal operation mode two cannot be achieved within
8 minutes the instrument turns into error mode.

Continuous Mode
The continuous mode is activated either by switching SW1 on the main board
to 1 (removal of cover is required, see “Removing and Refitting the Top
Cover” on page 50, for identifying SW1, see “Overview of Internal Parts” on
page 54), or by connecting pin 1 (white cable) and pin 3 (green cable) of the
auxiliary cable to each other.
When turning on the vacuum degasser the vacuum pump will run
continuously. This will establish a vacuum level that is below the trigger level
(600 mV / 115 Torr) of the normal operation mode 1.
If the vacuum level of normal operation mode 2 cannot be achieved within 8
minutes the instrument turns into error mode.

NOTE When set to continuous mode the life time of the vacuum pump will be
significantly reduced.

When to use Continuous Mode

In continuous mode the vacuum pump runs continuously thus generating the
highest degassing efficiency of the degasser. This mode is recommended for
very sensitive applications, which shows baseline disturbance due to
ON/OFF switching of the degasser.

Error Mode
The error level for the vacuum degasser is 190 Torr (approximately 800 mV).
This level cannot be achieved when there is a failure in the degasser (for
example, leaks, etc.). When the error level is exceeded the yellow status
indicator lamp is turned on and the vacuum pump runs continuously. If the
degasser cannot reach one of the normal operation modes within 8 minutes
the status indicator turns red and the vacuum pump is turned off.

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 Optimizing Performance
Operational Hints for the Micro Vacuum Degasser

Operational Hints for the Micro Vacuum

Degasser

Priming the Degasser

The micro micro vacuum degasser can be primed either by drawing solvent
through the degasser with a syringe or by pumping with the connected pump.
Priming the micro micro vacuum degasser with a syringe is recommended,
when:
• micro vacuum degasser is used for the first time, or vacuum tubes are
empty, or
• changing to solvents that are immiscible with the solvent currently in the
vacuum tubes.
Priming the micro vacuum degasser by using the pump is recommended,
when:
• pumping system was turned off for a length of time (for example,
overnight) and if volatile solvent mixtures are used, or
• if solvents have been changed.

WAR NI N G When opening capillary or tube fittings solvents may leak out. Please
observe appropriate safety procedures (for example, goggles, safety
gloves and protective clothing) as described in the material handling
and safety data sheet supplied by the solvent vendor, especially when
toxic or hazardous solvents are used.

Priming with a Syringe

Before using a new degasser or new tubings for the first time:
1 Prime all tubings with at least 5 ml of iso-propanol no matter whether the
channels will be used with organic mobile phase or with water.
If you are changing to a solvent that is immiscible with the solvent currently
in the tubing continue as follows:
2 Replace the current solvent with iso-propanol, if current solvent is organic or
with water, if current solvent is an inorganic buffer or contains salt.

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 Optimizing Performance
Operational Hints for the Micro Vacuum Degasser

3 Disconnect solvent outlet tube of the channel that is supposed to be primed

from your pump.
4 Connect syringe adapter to solvent outlet tube.
5 Push syringe adapter onto syringe.
6 Pull syringe plunger to draw at least 5 ml of solvent through degasser and
tubing.
7 Replace the priming solvent with the new solvent of your choice.
8 Pull syringe plunger to draw at least 5 ml of solvent through degasser and
tubing.
9 Disconnect syringe adapter from solvent tube.
10 Connect solvent tube to your pump.
11 Repeat step 3 to step 10 for the other solvent channels.

NOTE When priming the micro vacuum degasser with a syringe the solvent is drawn
through the degasser tubes very quickly. The solvent at the degasser outlet will
therefore not be fully degassed. Pump for approximately 5 minutes with your
selected flow rate before starting any application. This will allow the micro
vacuum degasser to properly degas the solvent in the degasser tubes.

NOTE The pump should never be used for priming empty tubings (never let the pump
run dry). Use the syringe to draw enough solvent for completely filling the
tubings to the pump inlet before continuing to prime with the pump.

Priming with the Pump

When the pumping system has been turned off for a certain time (for
example, overnight) oxygen will rediffuse into the solvent channels between
the micro vacuum degasser and the pump. Solvents containing volatile
ingredients will slightly lose these, if left in the degasser without flow for a
prolonged period of time. Therefore priming of the micro vacuum degasser
and the pumping system is required before starting an application.
1 Flush the micro vacuum degasser and all tubes with at least 5 ml of solvent.
2 Repeat step 3 through step 10 with other channels, where needed.

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