1100 DAD & MWD Reference Manual
1100 DAD & MWD Reference Manual
1100 DAD & MWD Reference Manual
Reference Manual
s1
Notices
© Agilent Technologies, Inc. 2002 Warranty rights not conveyed under these terms, it
must negotiate with Agilent to establish
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to this manual and any information
Manual Part Number contained herein, including but not CAU TI O N
G1315-90004 limited to the implied warranties of
merchantability and fitness for a par- A CAUTION notice denotes a haz-
ticular purpose. Agilent shall not be ard. It calls attention to an operat-
liable for errors or for incidental or
Edition consequential damages in connec- ing procedure, practice, or the like
Edition 07/2002 tion with the furnishing, use, or per- that, if not correctly performed or
formance of this document or of any adhered to, could result in damage
Printed in Germany information contained herein. Should to the product or loss of important
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Hewlett-Packard-Strasse 8 written agreement with warranty data. Do not proceed beyond a
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arate agreement shall control.
8 Specifications
Performance specifications of the detector
8 Specifications
Performance Specifications 288
A Safety Information
General Safety Information 292
Lithium Batteries Information 295
Disposal of Mercury from Deuterium Lamp 296
Radio Interference 297
Sound Emission 298
UV-Radiation 299
Solvent Information 300
Declaration of Conformity for HOX2 Filter 302
Aligent Technologies on Internet 303
Index
1
Installing the Detector
Site Requirements 14
Physical Specifications 16
Unpacking the Detector 17
Optimizing the Stack Configuration 20
Installing the Detector 22
Flow Connections to the Detector 25
Agilent Technologies 13
1 Installing the Detector
Site Requirements
Power Consideration
The detector power supply has wide ranging capabilities and accepts any line
voltage in the range mentioned in Table 1. Consequently, there is no voltage
selector in the rear of the detector. There are also no externally accessible
fuses, because automatic electronic fuses are implemented in the power
supply.
To disconnect the detector from line, unplug the power cord. The power supply still
WA RN ING
uses some power, even if the power switch on the front panel is turned off.
Shock hazard or damage of your instrumentation can result, if the devices are
WA RN ING
connected to a line voltage higher than specified.
Power Cords
Different power cords are offered as options with the detector. The female end
of all power cords is identical. It plugs into the power-input socket at the rear
of the detector. The male end of each power cord is different and designed to
match the wall socket of a particular country or region.
Never operate your instrumentation from a power outlet that has no ground
WA RN ING
connection. Never use a power cord other than the Agilent Technologies power cord
designed for your region.
Never use cables other than the ones supplied by Agilent Technologies to ensure
WA RN ING
proper functionality and compliance with safety or EMC regulations.
Bench Space
The detector dimensions and weight (see Table 1) allows you to place the
detector on almost any desk or laboratory bench. It needs an additional 2.5 cm
(1.0 inches) of space on either side and approximately 8 cm (3.1 inches) in the
rear for air circulation and electric connections.
If the bench should carry a Agilent 1100 Series system, make sure that the
bench is designed to bear the weight of all modules.
The detector should be operated in a horizontal position.
Environment
Your detector will work within the specifications at ambient temperatures and
relative humidity described in Table 1.
ASTM drift tests require a temperature change below 2 ∞C/hour (3.6 ∞F/hour)
over one hour period. Our published drift specification (refer also to
“Performance Specifications" on page 288) is based on these conditions.
Larger ambient temperature changes will result in larger drift.
Better drift performance depends on better control of the temperature
fluctuations. To realize the highest performance, minimize the frequency and
the amplitude of the temperature changes to below 1 ∞C/hour (1.8 ∞F/hour).
Turbulences around one minute or less can be ignored.
Do not store, ship or use your detector under conditions where temperature
CAU TI O N
fluctuations could cause condensation within the detector. Condensation will damage
the system electronics. If your detector was shipped in cold weather, leave it in its box
and allow it to warm up slowly to room temperature to avoid condensation.
Physical Specifications
Line frequency 50 or 60 Hz ± 5 %
Safety standards: IEC, CSA, UL, EN Installation category II, pollution degree 2
Damaged Packaging
If the delivery packaging shows signs of external damage, please call your
Agilent Technologies sales and service office immediately. Inform your service
representative that the detector may have been damaged during shipment.
If there are signs of damage, please do not attempt to install the detector.
CAU TI O N
Delivery Checklist
Ensure all parts and materials have been delivered with the detector. The
delivery checklist is shown below. Please report missing or damaged parts to
your local Agilent Technologies sales and service office.
Description Quantity
Detector 1
Power cable 1
Reference Manual 1
Fitting male
PEEK
Tubing
Ferrule front
This side is
Ferrule back
preinstalled
Fitting male SST
Capillary
If your detector is part of a complete Agilent 1100 Series system, you can ensure
optimum performance by installing the following configuration. This configuration
optimizes the system flow path, ensuring minimum delay volume.
Solvent cabinet
Vacuum degasser
Pump
Control module
Autosampler
Column compartment
Detector
Remote cable
AC power
Analog
signal to
recorder
GPIB or LAN
to LC
ChemStation
1 Install the LAN interface board in the detector (if required), see “Replacing
the Interface Board" on page 177.
2 Install theUV-lamp into the DAD, see “Exchanging a Lamp" on page 101.
3 Place the detector in the stack or on the bench in a horizontal position.
4 Ensure the line power switch at the front of the detector is OFF.
Status indicator
green/yellow/red
5 Connect the power cable to the power connector at the rear of the detector.
6 Connect the CAN cable to other Agilent 1100 Series modules.
7 If a Agilent ChemStation is the controller, connect either
Security lever
Interface board
Analog signal
APG remote
RS-232C
The detector is turned on when the line power switch is pressed and the green indicator
NO TE lamp is illuminated. The detector is turned off when the line power switch is protruding and
the green light is off.
To disconnect the detector from line, unplug the power cord. The power supply still
WA RN ING
uses some power, even if the power switch at the front panel is turned off.
The detector was shipped with default configuration settings. To change these settings see
NO TE “Setting the 8-bit Configuration Switch" on page 254.
When working with solvents please observe appropriate safety procedures (for
WA RN ING
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.
The flow cell is shipped with a filling of isopropanol (also recommended when the
NO TE instrument and/or flow cell is shipped to another location). This is to avoid breakage due to
subambient conditions.
1 Press the release buttons and remove the front cover to 2 Press the release button and open the flow cell door.
gain access to the flow cell area.
3 Insert the flow cell and install the capillaries to the 4 If another Agilent 1100 Series module is positioned on top
capillary holder (top is inlet, bottom is outlet). of the detector, route the tubing assembly waste from the
accessory kit behind the capillary holder and connect the
top end to the other module’s waste outlet.
To other module
To waste
5 Assemble the column-detector capillary from the 6 Connect the newly assembled fitting of the capillary to the
accessory kit. One side is already factory-assembled top fitting holder and the other end to the column.
Pre-assembled
7 Assemble the waste tubing from the accessory kit. 8 Connect the waste tubing to the bottom fitting holder and
a waste tubing to the leak outlet.
9 Remove the flow cell and establish a flow and observe for 10 Insert the flow cell, close the cover and replace the front
leaks. cover.
2
How to optmize the Detector
Optimizing the Detector Performance 30
Optimization Overview 31
Optimizing for Sensitivity, Selectivity, Linearity and Dispersion 33
Optimizing Selectivity 44
Agilent Technologies 29
2 How to optmize the Detector
The information in this chapter should be seen as a basic introduction to diode array
NO TE detector technics. Some of these technics may not be available in the instrument firmware
or the user interfaces (Control Module and/or Agilent Chemstation).
Optimization Overview
Parameter Impact
3 Setting the peak width (response time) • peak resolution versus sensitivity versus
• Use peak width according Figure 7 as starting point. disk space
• Set the peak-width close to the width of a narrow peak of interest in
your chromatogram.
4 Setting wavelength and bandwidth
• Sample wavelength:
• Never miss a peak by the use of a browser wavelength like 250 nm • sensitivity versus selectivity
with 100 nm bandwidth.
• Select specific wavelength with reduced bandwidth if you need
selectivity, e.g. 250,10 nm and 360,100 nm as reference wavelength.
• Set the sample wavelength to a peak or valley in the spectrum to get • sensitivity versus linearity
best linearity for high concentrations.
• Reference wavelength:
• Select the reference wavelength with broad bandwidth (30...100 nm) • baseline drift due to RI effects.
wavelength range where your analytes have little or no absorbance
(e.g. sample at 254 nm, reference at 320 nm).
Parameter Impact
Typical flow 0.01 ... 0.2 0.2 ... 0.4 0.4 ... 0.4 1 ... 2 ml/min 0.01 ... 5
rate ml/min ml/min ml/min ml/min
Time (min)
Please find below the details of the Agilent 1100 DAD/MWD flow cells:
Flow cell type Cell volume Part number Path length Path length Correction
(nominal) (actual) factor
500 Nanoliter flow cell kit 0.5 µl G1315-68714 10 mm 10.00 ± 0.02 mm 10/10
do not affect peak area nor peak symmetry. When set correctly, such filters
reduce baseline noise significantly (see Figure 9), but reduce peak height only
slightly. In addition, these filters reduce the data rate to allow optimum
integration and display of your peaks and to minimize disk space required to
store chromatograms and spectra.
Unfiltered
Figure 6 lists the filter choices of the detector. To get optimum results, set
peak width as close as possible to a narrow peak of interest in your
chromatogram. Response time will the be approximately 1/3 of the peak
width, resulting in less than 5 % peak-height reduction and less than 5 %
additional peak dispersion. Decreasing the peak width setting in the detector
will result in less than 5 % gain in peak height but baseline noise will increase
by a factor of 1.4 for a factor of 2 response-time reduction. Increasing peak
width (response time) by factor of two from the recommended setting
(over-filtering) will reduce peak height by about 20 % and reduce baseline
noise by a factor of 1.4. This gives you the best possible signal-to-noise ratio,
but may affect peak resolution.
Anisic acid
sample wavelength 252 nm
Absorbance (mAU)
30 nm
bandwidth
Reference wavelength 360
Wavelength (nm)
Bandwidth
30 nm
12 nm
4 nm
Because the detector averages absorbance values that are calculated for each
wavelength, using a wide bandwidth does not negatively impact linearity.
The use of a reference wavelength is highly recommended to further reduce
baseline drift and wander induced by room temperature fluctuations or
refractive index changes during a gradient.
An example of the reduction of baseline drifts is shown in Figure 12 for
PTH-amino acids. Without a reference wavelength, the chromatogram drifts
downwards due to refractive index changes induced by the gradient. This is
almost completely eliminated by using a reference wavelength. With this
technique, PTH-amino acids can be quantified in the low picomole range even
in a gradient analysis.
PTH-ASN
PTH-PHE
1 pmol each
PTH-PRO
PTH-ALA
PTH-ARG
Wavelength
267 nm
Reference 380 nm
Wavelength
267 nm
No reference
Time (min)
Grad.: 0.02 m KH2PO4/ACN from 12% ACN to 45% ACN in 12 min
Figure 12 Gradient Analysis of PTH-Amino Acids (1 pmol each), with and without Refer-
ence
Slit Width
The detector has a variable slit at the entrance of the spectrograph. This is an
effective tool to adapt the detector to changing demand of different analytical
problems.
A narrow slit provides spectral resolution for analytes with very fine
structures in the absorbance spectrum. An example of such a spectrum is
benzene. The five main absorbance bands (fingers) are only 2.5 nm wide and
just 6 nm apart from each other.
16 nm
4 nm
1 nm
A wide slit uses more of the light shining through the flow cell. This gives
lower baseline noise as shown in Figure 14.
Slit width 1 nm
Slit width 4 nm
Slit width 16 nm
However, with a wider slit, the spectrograph’s optical resolution (its ability to
distinguish between different wavelengths) diminishes. Any photodiode
receives light within a range of wavelength determined by the slit width. This
explains why the fine spectral structure of benzene disappears when using a
16-nm wide slit.
Furthermore, the absorbance is no longer strictly linear with concentration
for wavelengths at a steep slope of a compound’s spectrum.
Substances with fine structures and steep slopes like benzene are very rare.
In most cases the width of absorbance bands in the spectrum is more like
30 nm as with anisic acid (see Figure 10).
In most situations, a slit width of 4 nm will give the best results.
Use a narrow slit (1 or 2 nm) if you want to identify compounds with fine
spectral structures or if you need to quantify at high concentrations
(> 1000 mAU) with a wavelength at the slope of the spectrum. Signals with a
wide bandwidth can be used to reduce baseline noise. Because (digital)
bandwidth is computed as average of absorbance, there is no impact on
linearity.
Use a wide (8 or 16 nm) slit when your sample contains very small
concentrations. Always use signals with bandwidth at least as wide as the slit
width.
None Store signals only. No peak purity checks nor library search
features can be used for samples analyzed with this setting.
Apex Only one spectrum per peak is stored; a peak must be higher than
the value entered in Threshold (see below).
Apex + baseline Stores spectra for peaks > threshold at the top and at baseline
before and after each peak recommended minimum to do library
searches with baseline corrected spectra.
Apex + slope +baseline Add spectra at the up and down slope; required to do a minimum
peak purity check.
All in peak All spectra during all peak > Threshold are stored; required for a full
peak purity check.
Every 2nd spectrum Only every second spectrum is stored, occupying only half the disk
space.
All All spectra are stored.
Range
Only the wavelength range where the compounds in your sample absorb
contains information that is useful for purity checks and library searches.
Reducing the spectrum storage range saves disk space.
Step
Most substances have broad absorbance bands. Display of spectra, peak purity
and library search works best if a spectrum contains 5 to 10 data points per
width of the absorbance bands. For anisic acid (the example used before) a
step of 4 nm would be sufficient. However a step of 2 nm gives a better display
of the spectrum.
Threshold
Sets the peak detector. Only spectra from peaks higher than threshold will be
stored when a peak-controlled storage mode is selected.
Optimizing Selectivity
WL3 WL4
WL1 WL2
Wavelength (nm)
With a UV-visible detector based on a diode array and the correct choice of a
reference wavelength setting, quantitative detection is possible. To suppress
caffeine, the reference wavelength must be set to 282 nm. At this wavelength,
caffeine shows exactly the same absorbance as at 222 nm. When the
absorbance values are subtracted from each another, any indication of the
presence of caffeine is eliminated. In the same way, hydrochlorothiazide can
be suppressed if caffeine is to be quantified. In this case the wavelength is set
to 204 nm and the reference wavelength to 260 nm. Figure 16 shows the
chromatographic results of the peak suppression technique.
The trade-off for this procedure is a loss in sensitivity. The sample signal
decreases by the absorbance at the reference wavelength relative to the signal
wavelength. Sensitivity may be decreased by as much as 10–30 %.
Hydrochlorothiazide Hydrochlorothiazide
and caffeine and caffeine
Wavelength 204 nm Wavelength 222 nm
No reference No reference
user-specified ratio range. When the ratio falls within the range, the signal
output corresponds to the normal absorbance, giving single, clear peaks on a
flat baseline. An example is shown in Figure 17 and Figure 18.
Select 2 characteristic
wavelengths
Signal = WL1/WL2 20%
o-Terphenyl
Scaled
Biphenyl
WL2 WL1
Wavelength (nm)
Signals at 250 nm
Biphenyl
o-Terphenyl
No selectivity
Time (min)
The ratio range was set at 2 – 2.4 (2.2 ±10%). Only when the ratio between 249
and 224 nm was within this range, is the signal plotted. Of all four peaks, only
the third fulfilled the criterion (Figure 18). The others were not plotted.
3
Troubleshooting and Test Functions
Overview of the Detector’s Indicators and Test Functions 50
Status Indicators 51
Error Messages 53
Wavelength Recalibration 84
Test Functions 85
Agilent Technologies 49
3 Troubleshooting and Test Functions
Status Indicators
The detector is provided with two status indicators which indicate the
operational state (prerun, run, and error states) of the detector. The status
indicators provide a quick visual check of the operation of the detector (see
page 51).
Error Messages
In the event of an electronic, mechanical or hydraulic failure, the detector
generates an error message in the user interface. For each message, a short
description of the failure, a list of probable causes of the problem, and a list of
suggested actions to fix the problem are provided (see “Error Messages" on
page 53).
Wavelength Recalibration
Wavelength recalibration is recommended after repair of internal components,
and on a regular basis to ensure correct operation of the detector. The
detector uses the deuterium alpha and beta emission lines for wavelength
calibration (see “Wavelength Recalibration" on page 84).
Test Functions
A series of test functions are available for troubleshooting and operational
verification after exchanging internal components (see “Test Functions" on
page 85).
Status Indicators
Two status indicators are located on the front of the detector. The lower left
indicates the power supply status, the upper right indicates the detector
status.
Status indicator
green/yellow/red
Error Messages
Error messages are displayed in the user interface when an electronic,
mechanical, or hydraulic (flow path) failure occurs which requires attention
before the analysis can be continued (for example, repair, or exchange of
consumables is necessary). In the event of such a failure, the red status
indicator at the front of the detector is switched on, and an entry is written
into the detector logbook.
This section describes the meaning of detector error messages, and provides
information on probable causes and suggested actions how to recover from
error conditions.
Timeout
The timeout threshold was exceeded.
Probable Causes
• The analysis was completed successfully, and the timeout function switched
off the pump as requested.
• A not-ready state was present during a sequence or multiple-injection run
for a period longer than the timeout threshold.
Suggested Actions
✔ Check the logbook for the occurrence and source of a not-ready condition.
Restart the analysis where required.
Shutdown
An external instrument has generated a shut-down signal (through CAN or
REMOTE lines).
The detector continually monitors the remote input connectors for status
signals. A LOW signal input on pin 4 of the remote connector generates the
error message.
Probable Causes
• Leak detected in an external instrument with a remote connection to the
system.
• Shut-down in an external instrument with a remote connection to the
system.
• The degasser failed to generate sufficient vacuum for solvent degassing.
Suggested Actions
✔ Fix the leak in the external instrument before restarting the pump.
✔ Check external instruments for a shut-down condition.
✔ Check the degasser for an error condition. Refer to the Reference Manual
for the Aligent 1100 Series vacuum degasser.
Remote Timeout
A not-ready condition is still present on the remote input.
When an analysis is started, the system expects all not-ready conditions (e.g. a
not-ready condition during detector balance) to switch to run conditions
within one minute of starting the analysis. If a not-ready condition is still
present on the remote line after one minute the error message is generated.
Probable Causes
• Not-ready condition in one of the instruments connected to the remote line.
• Defective remote cable.
• Defective components in the instrument showing the not-ready condition.
Suggested Actions
✔ Ensure the instrument showing the not-ready condition is installed
correctly, and is set up correctly for analysis.
✔ Exchange the remote cable.
✔ Check the instrument for defects (refer to the instrument’s reference
documentation).
Synchronization Lost
During an analysis, the internal synchronization or communication between
one or more of the modules in the system has failed.
The system processors continually monitor the system configuration. If one or
more of the modules is no longer recognized as being connected to the system,
the error message is generated.
Probable Causes
• CAN cable disconnected.
• Defective CAN cable.
• Defective main board in another module.
Suggested Actions
✔ Ensure all the CAN cables are connected correctly.
✔ Switch off the system. Restart the system, and determine which module or
modules are not recognized by the system.
✔ Ensure all CAN cables are installed correctly.
Leak
A leak was detected in the detector.
The signals from the two temperature sensors (leak sensor and
board-mounted temperature-compensation sensor) are used by the leak
algorithm to determine whether a leak is present. When a leak occurs, the leak
sensor is cooled by the solvent. This changes the resistance of the leak sensor
which is sensed by the leak-sensor circuit on the detector main board.
Probable Causes
• Loose fittings.
• Broken capillary.
• Leaking flow cell.
Suggested Actions
✔ Ensure all fittings are tight.
✔ Exchange defective capillaries.
✔ Exchange flow cell components.
Additional Information
Detector leak error may be caused by the Aligent 1100 sampler. In each
sampler injection sequence, step# 2 ejects the mobile phase stored in the
metering head during the previous injection. This mobile phase is ejected
through the short plastic tube connected to port# 4 of the sampler switching
valve. The output of port# 4 is integrated into the sampler's contingency leak
drain system, which eventually terminates in the leak pan of the bottom
module of the stack - the detector. With normal injection volumes and run
times, the output of port# 4 is small, and evaporates right in the sampler leak
pan. However, the output of port# 4 is significant, and a substantial volume of
ejected mobile phase reaches the detector leak pan.
There are two possible fixes. Select the one which is most convenient.
1 The waste drain plumbing orientation, shown in step 4 on page 26,
eliminates the possibility of any leak drainage from above reaching the
detector leak pan. The leak drain for the detector can be connected to the
detector's leak drain fitting, and taken to waste separately.
2 If it is desired that the system has only one leak drain tube, then it's
possible in increase the length of the small plastic tube which is connected
to port# 4 of the sampler switching valve. This tube can then be taken to
waste separately. The tube which normally serves as the detector cell outlet
tube can be used for this purpose.
Fan Failed
The cooling fan in the detector has failed.
The hall sensor on the fan shaft is used by the detector main board to monitor
the fan speed. If the fan speed falls below two revolutions/second for more
than five seconds, the error message is generated.
Probable Causes
• Fan cable disconnected.
• Defective fan.
• Defective detector main board.
Suggested Actions
✔ Ensure the fan is connected correctly.
✔ Exchange fan.
✔ Exchange the detector main board.
Open Cover
The top foam has been removed.
The sensor on the detector main board detects when the top foam is in place.
If the foam is removed, the fan is switched off, and the error message is
generated.
Probable Causes
• The top foam was removed during operation.
• Foam not activating the sensor.
Suggested Actions
✔ Replace the top foam.
✔ Exchange the foam.
Cover Violation
The top foam has been removed.
The sensor on the detector main board detects when the top foam is in place.
If the foam is removed while the lamps are on (or if an attempt is made to
switch on the lamps with the foam removed), the lamps are switched off, and
the error message is generated.
Probable Causes
• The top foam was removed during operation.
• Foam not activating the sensor.
Suggested Actions
✔ Replace the top foam.
✔ Exchange the foam.
Communication Error
An internal communication error between the main processor and the
digital-signal processor has occurred.
Probable Causes
• Random communication error.
• Defective detector main board.
Suggested Actions
✔ Switch the detector off and on again at the power switch. If the error reoccurs,
exchange the detector main board.
UV Lamp Current
The UV lamp current is missing.
The processor continually monitors the anode current drawn by the lamp
during operation. If the anode current falls below the lower current limit, the
error message is generated.
Probable Causes
• UV lamp disconnected.
• Defective UV lamp.
• Defective detector main board.
• Defective power supply.
Suggested Actions
✔ Ensure the UV lamp connector is seated firmly.
✔ Exchange the UV lamp.
✔ Exchange the detector main board.
✔ Exchange the power supply.
UV Lamp Voltage
The UV lamp anode voltage is missing.
The processor continually monitors the anode voltage across the lamp during
operation. If the anode voltage falls below the lower limit, the error message is
generated.
Probable Causes
• Defective detector main board.
• Defective power supply.
Suggested Actions
✔ Exchange the detector main board.
✔ Exchange the power supply.
UV Ignition Failed
The UV lamp failed to ignite.
The processor monitors the UV lamp current during the ignition cycle. If the
lamp current does not rise above the lower limit within 2 – 5 seconds, the
error message is generated.
Probable Causes
• Lamp not connected.
• Defective UV lamp.
• Defective detector main board.
• Defective power supply.
Suggested Actions
✔ Ensure the lamp is connected.
✔ Exchange the UV lamp.
✔ Exchange the detector main board.
✔ Exchange the power supply.
UV Heater Current
The UV lamp heater current is missing.
During UV lamp ignition, the processor monitors the heater current. If the
current does not rise above the lower limit within one second, the error
message is generated.
Probable Causes
• UV Lamp not connected.
• Ignition started without the top foam in place.
• Defective UV lamp.
• Defective detector main board.
• Defective power supply.
Suggested Actions
✔ Ensure the UV lamp is connected.
✔ Replace the top foam, and turn on the lamp.
✔ Exchange the UV lamp.
✔ Exchange the detector main board.
✔ Exchange the power supply.
Type A, Parameter 0 or 2
Probable Causes
• Main board has been exchanged
Suggested Actions
✔ Power cycle the detector
Type B, Parameter 0 or 2
Probable Causes
• Defective or missing heater connector
Suggested Actions
✔ Ensure the connector to the detector main board is seated firmly and power
cycle the detector. At next switch-on you will get the same error message,
but with parameter 1 or 3 because the temperature hardware is detected
again (see below).
Type B, Parameter 1 or 3
Probable Causes
• Detector has recognized the hardware for temperature control. This is
because the detector didn't find the temperature hardware at last
switch-on.
Suggested Actions
✔ Power cycle the detector.
Heater Failed
Every time the deuterium lamp or the tungsten lamp is switched on or off a
heater self-test is performed. If the test fails an error event is created. As a
result the temperature control is switched off.
Probable Causes
• Defective connector or cable.
• Defective heater.
Suggested Actions
✔ Ensure the connector to the detector main board is seated firmly.
✔ Exchange heater assembly.
Wavelength Recalibration
The detector uses the alpha (656.1 nm) and beta (486 nm) emission lines of
the deuterium lamp for wavelength calibration. The sharp emission lines
enable more accurate calibration than is possible with holmium oxide. When
calibration is started, the 1-nm slit is moved into the light path automatically,
and the gain is set to zero. To eliminate effects due to absorbing solvents, the
test should be done with water in the flow cell. After calibration, the holmium
oxide test (see Figure “Holmium Oxide Test" on page 85) provides verification
of wavelength accuracy at three additional wavelengths. Wavelength
calibration should be done after maintenance of the flow cell, lamp exchange,
or after major repair, like processor board or optical unit exchange, see also
“Replacing the Detector’s Firmware" on page 178.
Test Functions
Intensity Test
The intensity test checks the lamp intensities (UV and visible lamps) over the
complete spectral range. The test evaluates the results automatically, and
provides an intensity spectrum.
Cell Test
The cell test compares the lamp intensities with and without flow cell
installed. The intensity ratio is an indicator of the amount of light absorbed by
the flow cell (e.g. contaminated or dirty cell windows).
Dark-Current Test
The dark-current test measures the leakage current from each optical diode.
The test evaluates the results automatically, and provides a graphical output
of the results.
Filter Test
The filter test checks the filter motor for correct movement, and checks the
absorbance of the holmium oxide filter in order to determine whether the
filter is dirty or contaminated.
Test Failed
Probable Causes
• Absorbing solvent or air bubble in flow cell.
• Incorrect calibration
• Dirty or contaminated flow cell.
• Dirty or contaminated optical components (achromat, windows).
Suggested Actions
✔ Ensure the flow cell is filled with water.
✔ Recalibrate (see “Wavelength Recalibration" on page 84) and repeat the test.
✔ Run the cell test (see “Cell Test" on page 90). If the test fails, exchange the
flow cell windows.
✔ Clean optical components with alcohol and lint-free cloth.
Intensity Test
The intensity test measures the intensity of the deuterium and tungsten lamps
over the full wavelength range (190 – 950 nm). Four spectral ranges are used
to evaluate the intensity spectrum. The test is used to determine the
performance of the lamps and optics (see also “Cell Test" on page 90). When
the test is started, the 1-nm slit is moved into the light path automatically, and
the gain is set to zero. To eliminate effects due to absorbing solvents, the test
should be done with water in the flow cell. The shape of the intensity
spectrum is primarily dependent on the lamp, grating, and diode array
characteristics. Therefore, intensity spectra will differ slightly between
instruments. Figure 23 shows a typical intensity test spectrum.
Test Failed
Probable Causes
• Absorbing solvent or air bubble in flow cell.
• Dirty or contaminated flow cell.
• Dirty or contaminated optical components (achromat, windows).
Suggested Actions
✔ Ensure the flow cell is filled with water, and free from air bubbles.
✔ Run the cell test (see “Cell Test" on page 90). If the test fails, exchange the
flow cell windows.
✔ Clean optical components with alcohol and lint-free cloth.
Cell Test
The cell test measures the intensity of the deuterium and tungsten lamps over
the full wavelength range (190 – 950 nm), once with the flow cell installed, and
once with the flow cell removed. The resulting intensity ratio is a measure of
the amount of light absorbed by the flow cell. The test can be used to check for
dirty or contaminated flow cell windows. When the test is started, the 1-nm
slit is moved into the light path automatically, and the gain is set to zero. To
eliminate effects due to absorbing solvents, the test should be done with water
in the flow cell.
Dark-Current Test
The dark-current test measures the leakage current from each diode. The test
is used to check for leaking diodes which may cause non-linearity at specific
wavelengths. During the test, the slit assembly moves to the dark position,
cutting off all light falling onto the diode array. Next, the leakage current from
each diode is measured, and displayed graphically (see Figure 26). The leakage
current (represented in counts) for each diode should fall within the limits
(red bands) shown in the plot (see Figure 26).
Test Failed
Probable Causes
• Defective optical unit.
Suggested Actions
✔ Exchange the optical unit.
Filter Test
The filter test checks the correct operation of the filter assembly. When the
test is started, the holmium oxide filter is moved into position. During filter
movement, the absorbance signal is monitored. As the edge of the filter passes
through the light path, an absorbance maximum is seen. Once the filter is in
position, the absorbance maximum (of holmium oxide) is determined. Finally,
the filter is moved out of the light path. During movement, an additional
absorbance maximum is expected as the edge of the filter passes through the
light path. The test passes successfully, if the two maxima resulting from the
edge of the filter assembly (during filter movement) are seen, and the
absorbance maximum of holmium oxide is within the limits.
Test Failed
Probable Causes
• Filter assembly (lever and filter) not installed.
• Defective filter motor.
Suggested Actions
✔ Install the filter assembly.
✔ Exchange the filter motor.
4
Repairing the Detector
Introduction into Repairing the Detector 96
Overview of the Repairing of the Detector 99
Simple Repairs 100
Exchanging Internal Parts 136
Agilent Technologies 95
4 Repairing the Detector
Simple Repairs
The detector is designed for easy repair. The most frequent repairs such as
lamp change and flow cell change can be done from the front of the detector
with the detector in place in the system stack. These repairs are described in
“Simple Repairs" on page 100.
To prevent personal injury, the power cable must be removed from the instrument
WA RN ING
before opening the detector cover. Do not connect the power cable to the detector
while the covers are removed.
When working with solvents 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.
Electronic boards and components are sensitive to electronic discharge (ESD). In order
CAU TI O N
to prevent damage always use an ESD protection (for example, the ESD wrist strap
from the accessory kit) when handling electronic boards and components (see “Using
the ESD Strap" on page 98).
Eye damage may result from directly viewing the light produced by the deuterium
WA RN ING
lamp used in this product. Always turn the deuterium lamp off before removing it.
Do not let liquid drip into the detector. It could cause shock hazard and it could
WA RN ING
damage the detector.
With the introduction of the G1315B/G1365B DAD/MWD some of the metal plates look
NO TE different (no air openings) compared to the G1315A/G1365A DAD/MWD. The figures have
changed for specific repairs only.
Interface board,
see page 177
Main Board,
Power supply, see page 141
see page 162
Fan,
see page 146
Tungsten
lamp,
see
page 101 Optical unit,
see page 152
Leak handling
system,
Deuterium lamp,
see page 129
see page 101
Flow cell,
see page 104 and page 107 Leak sensor,
see page 165
Simple Repairs
On the following pages repairs are described that can be carried out without
opening the main cover.
Deuterium lamp or If noise and/or drift exceeds your application limits or An intensity test should be performed
tungsten lamp lamp does not ignite. after replacement.
exchange
Flow cell exchange If application requires a different flow cell type. A holmium or wavelength calibration
test should be performed after
replacement.
Flow cell parts If leaking or if intensity drops due to contaminated flow A pressure tightness test should be
Cleaning or exchange cell windows. done after repair.
Coupling lens If light throughput is low due to contaminations. An intensity test should be performed
assembly cleaning or after replacement.
exchange
Cell support assembly If light throughput is low due to contaminations. An intensity test should be performed
after replacement.
Exchanging a Lamp
When required If noise or drift exceeds application limits or lamp does not ignite
Tools required Screwdriver POZI 1 PT3
Preparations for this procedure: 1 Press the release buttons and remove the front cover to
have access to the lamp area.
• Turn the lamp(s) off.
CAUTION:
If the detector has been in use, the lamp may be hot.
If so, wait five minutes until lamp cools off.
2 Disconnect lamp from the connector and unscrew the 3 Remove the lamp. Do not touch the glass bulb with your
lamp. fingers.
4 When replacing the vis-lamp, assure that the vis-lamp is 5 Insert the lamp. Fix the screws and reconnect the lamp to
inserted as shown (flat edge towards the deuterium lamp - connector.
opposite as in the figure).
When required If an application needs a different type of flow cell or the flow cell needs repair.
Tools required Two 1/4 inch wrenches for capillary connections
Parts required Standard flow cell, 10 mm, 13 µl, 120 bar, G1315-60012
Semi-micro flow cell, 6 mm, 5 µl, 120 bar, G1315-60011
High pressure flow cell, 6 mm, 1.7 µl, 400 bar, G1315-60015
500 nl flow cell, 10 mm, refer to “500 nl Flow Cell - Replacing or Cleaning" on
page 121
Preparations for this procedure: 1 Press the release buttons and remove the front cover to
have access to the flow cell area.
• Turn the lamp(s) off.
2 Press the release button and open the flow cell door. 3 Disconnect the cell inlet and the cell outlet capillary and
the waste capillary from the capillary holder.
4 Remove the flow cell by pressing the flow cell holder. Note:
The label attached to the flow cell provides
information on part number, path length and
maximum pressure.
If you want to replace flow cell parts, see “Repairing
the Standard or Semi-Micro Flow Cell" on page 107
or “Repairing the Standard or Semi-Micro Flow
Cell" on page 107.
5 Insert the flow cell into the cell compartment and close the 6 Reconnect the waste capillary and the cell inlet and the
cell door. cell outlet tubing to the capillary holder.
When required If the flow cell needs repair due to leaks or contaminations (reduced light
throughput)
Tools required Two 1/4 inch wrenches for capillary connections
hexagonal key 4 mm
Tooth picks
Parts required For parts, see “Standard Flow Cell" on page 184 and “Semi-Micro Flow
Cell" on page 186
The gaskets used in the standard and semi-micro flow cell are different.
NO TE
Preparations for this procedure: 1 Use a 4 mm hex key to unscrew the window assembly and
remove the gasket from the cell body.
• Turn off the flow.
• Remove the front cover.
• Remove the flow cell, see “Exchanging a Flow Cell" on
page 104.
gasket
windows
assembly
Note: 2 Use a tooth pick to remove the quartz window from the
window assembly.
If you want to replace the gasket only, continue with
step 8.
Do not mix the gasket #6 and # 7. They are different
for standard and semi-mirco flow cell.
3 If the washers fall out of the window assembly, they must be inserted in the correct order with the Teflon® ring to prevent
any leaks from the flow cell window.
4 Assemble the washers and the window assembly in 5 Correct orientation of spring washers [2] is required.
correct order.
6 Press the Teflon® ring into the window assembly. 7 Press the window assembly onto the new or cleaned
quartz window.
8 Insert a new gasket [6, 7] and the window assembly [1] 9 Using a 4-mm hex key, tighten the window screw hand
into the cell body. Assure, that the gasket is on the bottom. tight plus a quarter turn.
1
7
6
1
Next steps:
• Reconnect the capillaries, see “Exchanging a Flow Cell" on page 104.
• Perform a leak test.
• Insert the flow cell.
• Replace the front cover
• Perform a wavelength calibration, see “Wavelength Recalibration" on page 84 or holmium test, see “Holmium Oxide
Test" on page 85 to check the correct positioning of the flow cell.
When required If the flow cell needs repair due to leaks or contaminations (reduced light
throughput)
Tools required Two 1/4 inch wrenches for capillary connections
hexagonal key 4 mm
Tooth picks
Parts required Seal ring 79883-07101
Quartz windows 1000-0953
For other parts see “High Pressure Flow Cell" on page 188
Preparations for this procedure: 1 Remove the window assembly (1) and the gasket (2) from
the cell body.
• Turn off the flow.
• Remove the front cover.
• Remove the flow cell, see “Exchanging a Flow Cell" on
page 104. 1
2
2
1
If you want to replace the gasket only, continue with 2 Use a tooth pick to remove the quartz window from the
step 8. window assembly.
3 If the washers fall out of the window assembly, they must be inserted in the correct order with the Teflon® ring to prevent
any leaks from the flow cell window.
Follow the procedure “Repairing the Standard or Semi-Micro Flow Cell" on page 107 for reassembling.
Orientation of Flow Cell Parts
1 window screw 6
contains items 2, 3, 4, 5 5
and 6 4
2
2 seal ring 3
3 quartz window 2
7
4 compression washer
5 spring washers
4 window holder
1
6 window screw
7 flow cell
8 inlet capillary 8
9 outlet capillary
Preparations for this procedure: 1 Identify the inlet and outlet capillaries.
Outlet capillary
Outlet capillary
3 To replace the inlet capillary, use a 4-mm wrench for the 4 Unscrew the cell body from the heat exchanger and the
fitting. heat exchanger from the clamp unit.
Inlet capillary
5 Unscrew the fixing screw and unwrap the inlet capillary 6 Take the new inlet capillary and bend it 90° about 35 mm
from the grove in the flow cell body. from its end.
Screw
35 mm
90°
Inlet capillary
with heat
7 Bend the caillary again by 90° as shown below. 8 Insert the capillary into the hole between fixing screw and
the inlet fitting.
90°
9 The capillary lays in the grove and should be tied around 10 Insert the fixing screw, so that the capillary cannot leave
the body (in the grove) 5 times. the grove.
Screw
Inlet capillary
with heat
11 Fix the flow cell body to the heat exchanger. 12 Fix the inlet capillary to the flow cell body handtight first.
Then do a 1/4 turn with a 4-mm wrench.
IN IN
OUT OUT
13 Fix the new heat exchanger to the clamp unit. Next steps:
• Reconnect the capillaries, see “Exchanging a Flow
Cell" on page 104.
• Perform a leak test.
• Insert the flow cell.
• Replace the front cover.
• Perform a wavelength calibration, see “Wavelength
Recalibration" on page 84 or holmium test, see
“Holmium Oxide Test" on page 85 to check the correct
positioning of the flow cell.
Preparations for this procedure: 1 Identify the inlet and outlet capillaries.
Outlet capillary
Outlet capillary
3 To replace the inlet capillary, use a 4-mm wrench for the 4 Unscrew the cell body from the heat exchanger and the
fitting. heat exchanger from the clamp unit.
Inlet capillary
5 Fix the new heat exchanger to the clamp unit and the heat 6 Fix the inlet capillary to the flow cell body handtight first.
exchanger to the cell body. Then do a 1/4 turn with a 4-mm wrench.
Inlet capillary
Next steps:
• Reconnect the capillaries, see “Exchanging a Flow Cell" on page 104.
• Perform a leak test.
• Insert the flow cell.
• Replace the front cover.
• Perform a wavelength calibration, see “Wavelength Recalibration" on page 84 or holmium test, see “Holmium Oxide
Test" on page 85 to check the correct positioning of the flow cell.
The quartz block can be cleaned with alcohol. DO NOT touch the inlet and outlet windows
NO TE at the quartz block.
1 Disconnect the capillaries from the capillary holder and 2 Unscrew the cell body from the holder.
remove the flow cell.
3 Unscrew the capillaries from the flow cell. DO NOT use the 4 Using for example a toothpick, press on the plastic part
adapter at this time! and slide the quartz body out of the cell housing.
5 The quartz body and the cell seal assembly can be 6 This figure shows the correct holding of the quartz body
separated for cleaning purpose. and the cell seal assembly.
7 Replace the cell seal assembly onto the quartz body. It is 8 Slide the quartz body completely into the cell body to the
recommended to use a new assembly. front stop (use for example a toothpick).
9 Insert the flow cell capillaries and tighten them 10 Reassemble the flow cell body to the holder.
fingertight. Use the wrench and torque adapter as
described on page 124 and tighten the fittings alternate.
11 Re-install the flow cell and connect the capillaries to the Remove the flow cell and perform a leak test.
union holder.
If no leak is observed, install the flow cell and you
are ready to work.
IN
OUT
With the instrument accessory kit comes a 4-mm wrench and with the Sealing Kit a special
NO TE adapter. Both together work as a torque wrench with pre-defined torque (maximum allowed
torque for the cell fittings is 0.7 Nm). It can be used to tight the capillary fittings at the flow
cell body. The wrench has to be plugged into the adapter as shown in Figure 30.
Adapter
Wrench
max
0.7 Nm
Preparations for this procedure: 1 Unscrew the six screws and remove the flow cell cover.
• Turn off the flow.
• Remove the front cover.
• Remove the flow cell, see “Exchanging a Flow Cell" on
page 104.
2 If not already in this position, move the filter up. 3 While releasing the holder with a screwdriver, carefully
remove the holmium oxide filter using a pair of tweezers
covered with lint-free cloth or tape.
5 Replace the flow cell cover and fix the six screws. Next steps:
• Perform a holmium oxide test, see “Holmium Oxide
Test" on page 85 to check the proper function of the
holmium oxide filter.
• Insert the flow cell, see “Exchanging a Flow Cell" on
page 104.
• Replace the front cover.
• Turn on the flow.
Correcting Leaks
When required If a leakage has occurred in the flow cell area or at the heat exchanger or at the
capillary connections
Tools required Tissue
Two 1/4 inch wrenches for capillary connections
Parts required None
Leak pan
k sensor assembly
Leak funnel
Leak tubing
When required The coupling lens assembly is located between the tungsten and the
deuterium lamp. It may be replaced when light transmission is reduced and a
lamp exchange or window cleaning does not improve the light throughput.
Tools required Screwdriver POZI 1 PT3
hexagonal key 1.5 mm
A pointed pair of pliers
Preparations for this procedure: 1 Use the 1.5-mm hex key to loosen the setscrew that
secures the lens assembly.
• Turn off the lamp(s).
2 Carefully slide the lens assembly to the right into the 3 Remove the lens assembly completely.
deuterium lamp area by pushing it from the tungsten lamp
side with the hex key.
4 The assembly may be disassembled using a pair of pliers 5 The lens may be cleaned or the complete assembly must
to remove the retainer ring. be exchanged.
Retainer ring
Washer
Lens support
Lens
Lens holder
6 Insert the rebuilt or new lens assembly and slide it into its 7 Align the lens assembly with the wall of the deuterium
holder. area. Fix the setscrew that secures the lens assembly.
Next steps:
• Replace both lamps.
• Perform an intensity test to check the proper function.
• Replace the front cover.
When required This window is located between the holmium oxide filter and the flow cell. It
may be replaced when the transmission of light is reduced and a lamp
exchange or a window cleaning does not improve the light throughput.
Tools required Screwdriver POZI 1 PT3
hexagonal key 1.5 mm
Pointed pair of pliers
Preparations for this procedure are: 1 Unscrew the six screws and remove the flow cell cover.
• Turn off the lamp(s).
2 If not already in this position, move the holmium oxide 3 Use the 1.5-mm hex key to loosen the setscrew that
filter down. secures the cell support assembly.
4 Carefully slide the assembly to the right into the flow cell 5 Remove the cell support assembly completely.
compartment by pushing it from the holmium oxide filter
side.
6 The assembly may be disassembled using a pair of pliers 7 Insert the rebuilt or new assembly and slide it in until it is
to remove the retainer ring. The window may be cleaned or stopped by the filter lever.
the complete assembly must be exchanged.
Retainer ring
Washer
Spectro window
Cell support
8 Leave slight clearance for movement of the filter lever Next steps:
between both, the lens assembly and the filter lever, and
• Perform a filter test to check the proper function.
fix the setscrew. • Replace the flow cell cover, see “Cleaning or
Exchanging the Holmium Oxide Filter" on page 125.
• Replace both lamps.
• Replace the front cover.
The following procedures require opening the main cover of the detector. Always
WA RN ING
ensure the detector is disconnected from the line power when the main cover is
removed. The security lever at the power input socket prevents that the detector
cover is taken off when line power is still connected.
To disconnect the detector from line, unplug the power cord. The power supply still
WA RN ING
uses some power, even if the switch on the front panel is turned off.
When working with solvents 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.
The electronics of the detector will not allow operation of the detector when the top cover
NO TE and the top foam are removed. A safety light switch on the main board will inhibit the
operation of the fan immediately. Voltages for the other electronic components will be
turned off after 30 seconds. The status lamp will lit red and an error will be logged into the
logbook of the user interface. Always operate the detector with the top covers in place.
Electronic boards and components are sensitive to electronic discharge (ESD). In order
CAU TI O N
to prevent damage always use an ESD protection (for example, the ESD wrist strap
from the accessory kit) when handling electronic boards and components, see “Using
the ESD Strap" on page 98.
Eye damage may result from directly viewing the light produced by the deuterium
WA RN ING
lamp used in this product. Always turn off the deuterium lamp before removing the
deuterium lamp.
With the introduction of the G1315B/G1365B DAD/MWD some of the metal plates look
NO TE different (no air openings) compared to the G1315A/G1365A DAD/MWD. The figures have
changed for specific repairs only.
Parts required Depends on the work inside and the following procedures
Preparations for this procedure: 1 Press the release buttons and remove the front cover.
Unclip the waste funnel assembly.
• Turn off the detector.
• Disconnect the power cable.
• Disconnect capillaries.
• Remove detector from stack and place it on the working
bench.
2 Install the ESD strap. If installed, unscrew and remove the 3 Move the power lock across the power inlet and lift the
interface board. Place the board on the ESD kit. clips of the cover.
4 Lift the cover up and slide it towards the rear. 5 Unscrew the screws at the rear of the top plate, slide the
plate towards the front and remove it.
6 Disconnect the lamps from their connectors. 7 Remove the two lamp connectors towards the back by
depressing their connector tabs with a screwdriver.
8 While removing the top foam section completely, route the Note:
lamp cables through the hole in the foam.
Do not connect a power plug to the detector module
after removing the top covers.
A safety light switch on the main board will turn off
fan (immediately) and electronics (after 30 s) to
avoid the operation with removed covers. An error
will be generated (status lamp will light red) and the
logbook will show an error message.
When required If detector main board is defective or for repair on other assemblies
Tools required Screwdriver POZI 1 PT3
Hexagonal wrenches 5 mm, 7 mm and 15 mm
Parts required Detector main board (DAM) G1315-69540 (exchange assembly) for G1315A DAD
Detector main board (DAM) G1315-69540 (exchange assembly) for G1315B DAD
Detector main board (MWM) G1365-69540 (exchange assembly) for G1365A MWD
Detector main board (MWM) G1365-69540 (exchange assembly) for G1365B MWD
Analog
connector nuts
Remote
GPIB
Board recesses
4 Remove the front cover, top cover and top foam section, see “Removing the
Top Cover and Foam" on page 138.
5 Use a 5-mm and 7-mm wrench to unscrew the REMOTE and the GPIB
connector and a 15-mm wrench to unscrew the nuts of the ANALOG
connectors.
6 Disconnect all connectors from the detector main board.
S1 J1 J6 J7 J2 J3 J4 J5
Description Connector
GPIB J1
RS-232C J2
REMOTE J3
CAN J6/7
Analog output J4/5
SIMM memory J8/9 J10
Power supply J10 J8 J9
Interface board J13
Fan assembly J16
Heater (B-version) J17
Temperature sensor J18
(B-version) J13
Holmium oxide filter J19
Leak sensor J21
Optical unit J22 J16 BT1
assembly
Battery BT1 J18
Configuration switchS1 J17
J19 J21
J22
7 Remove the detector main board. Place the board on the ESD kit.
8 In most cases the RFI spring plate remains on the interface connectors of
the board. Carefully remove the spring plate and place it back into its
position in the instrument before installing a new board.
9 On the new board check the switch setting of address switch S1, see
“Setting the 8-bit Configuration Switch" on page 254.
An incorrect switch setting (for example, TEST/BOOT) may cause the module to turn in a
NO TE basic mode (yellow or red flashing status light). In such a case turn off the module, reset
the address switches, and turn on the module again.
10 Install the new detector main board and reconnect the connectors. Assure
that the board is fitted correctly into the board recess in the rear panel.
11 Refit the screws at the REMOTE and GPIB connectors and the nuts of the
ANALOG connectors.
12 Reinstall the top foam section, top cover and front cover, see “Replacing the
Foam and the Top Cover" on page 173.
13 Replace detector into the stack and reconnect the cables.
If a new detector main board is installed, update the serial number information of the
NO TE detector in the user interface, see procedure below.
14 Check the firmware revision of the module. If the firmware revision is older
than the current firmware revision of the module, update the firmware
using the standard firmware update procedure, see “Replacing the
Detector’s Firmware" on page 178.
The G1315B DAD and the G1365B MWD require firmware revision 4.x or above (main and
NO TE resident).
For firmware revisions below A.02.00 it is important never to press Done if the Serial# box
NO TE is blank. In this case, the module can no longer be recognized by either the control module
or the Agilent ChemStation. The main board must then be replaced.
6 Turn the detector off, then on again. The Records screen should display the
correct serial number for this module.
7 If a Agilent ChemStation is also connected, restart the Agilent ChemStation
now as well.
The reply line will respond with RA 0000 SER followed by the module serial
number you just entered.
2 Turn off thedetector, then on again. Then, restart the Agilent ChemStation.
If the serial number you have just entered is different than the original
module serial number, you will be given the opportunity to edit the
configure 1100 access screen during the restart of the Agilent ChemStation.
3 After start up, the serial number you have just entered can be seen under
the Instrument menu of the main user interface screen. The serial number
of the detector can also be seen by typing the following command into the
command line (depends on the detector type, either DAD or MWD):
print sendmodule$ (ldad, "ser?")
print sendmodule$ (lmwd, "ser?")
The reply line will give the module serial number.
Use this procedure for the the G1315A/G1365A only. For G1315B/G1365B detectors refer
NO TE to “Replacing Fan Parts (G1315B/G1365B)" on page 148.
Preparations for this procedure: 1 Disconnect the connectors from the main board (fan J16)
and pull the fan assembly out of its location.
• Turn off the lamp.
• Switch off the detector, and disconnect the cables and
acpillaries.
• Remove detector from stack and place it on the working
bench.
• Remove front cover, top cover and top foam section, see
“Removing the Top Cover and Foam" on page 138.
The fan must be installed in the correct orientation The figure below shows the required air flow
(see arrow on the fan) to ensure optimum cooling direction.
and operation of the detector. The direction of air
flow is from the front towards the rear.
AIRFLOW
G1315/65A
G1315/65B
2 Insert the fan assembly into its location and Reconnect Next steps:
the connector to the main board (fan J16), see figure
below for location. • Reinstall the top foam section, top cover and front
cover, see “Replacing the Foam and the Top Cover" on
page 173.
• Replace the detector into the stack.
• Reconnect cables, capillaries and turn on detector
When required If the fan is defective or noisy, if the temperature sensor or the heater fails
Tools required Screwdriver POZI 1 PT3, a pair of pliers
Parts required Fan assembly 3160-1016,
Temperature sensor assembly G1315-60000,
Heater assembly G1315-60003
Preparations for this procedure: 1 Disconnect the connectors from the main board; fan (J16),
temperature sensor (J18) and heater (J17) and pull the fan
• Turn off the lamp. assembly out of its location.
• Switch off the detector, and disconnect the cables and
capillaries.
• Remove detector from stack and place it on the working
bench.
• Remove front cover, top cover and top foam section, see
“Removing the Top Cover and Foam" on page 138.
The heater and temperature sensor assemblies are 2 To unclip the heater from the fan, use a pair of pliers,
clipped into the fan assembly. In case the squeeze the clips and push them through the hole. Repeat
temperature sensor or the heater assembly fails, this with the three remaining clips.
they can be unclipped separately from the fan
assembly.
If the fan is defective, unclip both, the temperature
sensor assembly and the heater assembly from the
fan as described in the next steps.
3 If required, remove the sensor out of its holder. 4 To unclip the sensor holder from the fan, pull it carefully
from its position pushing into the direction the arrow
points to.
5 To re-install the sensor holder (here shown with the 6 Clip the sensor carefully into its holder and route the
sensor), bring the holder into its position and slide it cables as shown.
carefully across the fan cable. Assure, that the fan rotates smoothly without any
scraping noise. Otherwise correct the position of the
sensor holder.
7 Position the heater assembly as shown and clip the heater The fan must be installed in the correct orientation
onto the fan. The cables should be oriented towards the (see arrow on the fan) to ensure optimum cooling
left corner. and operation of the detector. The direction of air
flow is from the rear towards the front (see figure on
next page).
The figure below shows the required air flow 8 Insert the fan assembly into its location.
direction.
AIRFLOW
G1315/65A
G1315/65B
9 Reconnect the connectors to the main board (fan J16), Next Steps:
temperature sensor (J18) and heater (J17), see figure
below for location. • Reinstall the top foam section, top cover and front
cover, see “Replacing the Foam and the Top Cover" on
page 173.
• Turn on the detector and prove, that the fan rotates
smoothly without any scraping noise. Otherwise repeat
step 5 and step 6 on page 150.
• Replace the detector into the stack.
• Reconnect cables, capillaries and turn on detector
Use this procedure for the the G1315A/G1365A only. For G1315B/G1365B detectors refer
NO TE to “Removing the Optical Unit (G1315B/G1365B)" on page 154.
10 Remove the two rubber shock absorbers. 11 Disconnect the SCI cable (J23) and the holmium oxide
filter motor (J19) from the detector main board.
With the introduction of the G1315B/G1365B DAD/MWD the appearance of the z-plane
NO TE (front metal plane) has been changed (no holes any more) and an isolation seal between
the optical unit and the z-plane. Therefore, some of the figures may still show the old
appearance of the G1315A/G1365A. For G1315A/G1365A detectors refer to “Removing the
Optical Unit (G1315A/G1365A)" on page 152.
Preparations for this procedure: 1 .Loosen the screw on the left side of the z-plane and the
two screes near the hydraulic connection.
• Turn off the lamp.
• Switch off detector, and disconnect power cable.
• Remove detector from stack and place it on working
bench.
• Remove front cover, top cover and top foam section, see
“Removing the Top Cover and Foam" on page 138.
2 Remove the two rubber shock absorbers. 3 Slide the z-plane to the front and remove it from the
module.
4 Disconnect the SCI cable (J23) and the holmium oxide 5 Remove the optical unit from the instrument holding the
filter motor (J19) from the detector main board. one hand at back of the heat sink.
When required The source lens (achromat) assembly might be cleaned or replaced when the
transmission of light is reduced and a lamp exchange or new spectro windows
do not improve the light throughput
Tools required Screwdriver POZI 1 PT3
hexagonal key 1.5 mm
A pointed pair of pliers
Parts required Source lens (achromat) assembly G1315-65201(includes filter lever
G1315-45001)
Spectro window 79880-28111
Filter lever G1315-45001
If the filter motor was removed, the filter lever should not be reused. Always use a new
NO TE filter lever to assure correct fit on the filter motor shaft.
Preparations for this procedure: 1 Place the optical unit on your bench.
• Turn off the lamp.
• Switch off detector and disconnect the power cable.
• Remove detector from stack and place it on the working
bench.
• Remove the front cover, top cover and top foam section,
see “Removing the Top Cover and Foam" on page 138.
• Remove the optical unit, see “Removing the Optical Unit
(G1315A/G1365A)" on page 152 or “Removing the
Optical Unit (G1315B/G1365B)" on page 154.
2 Pull the filter motor off the shaft. Keep the spring and the 3 Use the 1.5-mm hexagonal key to loosen the setscrew that
lever fixture in a safe place. Remove the filter lever on the secures the source lens assembly.
other side.
4 Use the 1.5-mm hexagonal key to loosen the setscrew that 5 Carefully slide the assembly to the right by pushing it from
secures the cell support assembly. the deuterium lamp side with a hexagonal wrench.
6 Remove the achromat assembly. 7 Use a metal blade (12-mm width, 1-mm thick) to unscrew
the lens achromatic.
8 Remove the spring and the spectro window from the 11 Replace the achromat assembly, move it completely into
holder. the optical and fix the setscrew.
9 Clean (with alcohol and lint-free cloth) or replace the
spectro window.
Do not clean the achromatic lens with any liquid. To
clean use dry air only.
10 Replace all parts into the holder and tighten the lens
achromatic with the metal blade.
12 Before installing the filter motor, press the filter lever in 13 While counter-holding the filter lever, insert the filter
from the other side. motor onto the filter shaft until it clicks into the final
position.
14 Slide in the cell support assembly until it is stopped by the Next steps:
holmium filter. Leave about 0.2-mm clearance for
movement of the filter lever between both the lens • Check that the filter lever is moveable.
assembly and the filter lever, and fix the setscrew. • Reinstall the optical unit, see “Installing the Optical Unit
(G1315A/G1365A)" on page 169 or “Removing the
Optical Unit (G1315B/G1365B)" on page 154.
• Reinstall the flow cell, see “Exchanging a Flow Cell" on
page 104.
• Reinstall the front cover, top cover and top foam
section, see “Exchanging the Detector Main Board" on
page 141.
• Replace detector into the stack.
• Reconnect the cables and turn on the detector.
If the filter motor was removed, the filter lever should not be reused. Always use a new
NO TE filter lever to assure correct fit on the filter motor shaft.
Preparations for this procedure: 1 Place the optical unit on your bench.
2 Pull the filter motor off the shaft. Keep the spring in a safe 3 Before installing the filter motor, press the filter lever in
place. from the other side.
4 While counter-holding the filter lever, press the filter Next steps:
motor onto the filter shaft until it clicks into the final
position. • Check that the filter lever is moveable.
• Reinstall the optical unit, see “Installing the Optical Unit
(G1315A/G1365A)" on page 169 or “Removing the
Optical Unit (G1315B/G1365B)" on page 154.
• Reconnect the filter motor cable to connector J18
(G1315/65A) or J19 (G1315/65B) on the detector main
board.
• Reinstall the front cover, top cover and top foam
section, see “Replacing the Foam and the Top Cover" on
page 173.
• Replace the detector into the stack.
• Reconnect the power cable and turn on detector.
The repair level of the power supply assembly is exchanging the complete assembly. No
NO TE serviceable parts are inside.
5 Carefully remove the bottom foam part by sliding it out 6 Unscrew the power supply at the rear of the module.
towards the rear.
7 Press down the power switch light pipe to remove it from 8 Remove the power supply completely.
the coupler. Re-use the coupler on the new power supply.
Power
switch light
pipe
Coupler
The repair level of the power supply assembly is exchange of the complete assembly. No serviceable parts
inside.
9 Insert the power supply into its location and fix it with the 10 Press down and clip in the power switch light pipe into the
screws at the rear panel. power supply.
Power
switch light
pipe
11 Reinstall bottom foam part. Slide it in underneath the leak Next steps:
drain.
• Reinstall the processor board, see “Exchanging the
Detector Main Board" on page 141.
• Reinstall the fan assembly, see “Exchanging the Fan
(G1315A/G1365A)" on page 146 or “Replacing Fan
Parts (G1315B/G1365B)" on page 148.
• Reinstall the optical unit, see “Installing the Optical Unit
(G1315A/G1365A)" on page 169 or “Removing the
Optical Unit (G1315B/G1365B)" on page 154.
• Reinstall the front cover, top cover and top foam
section, see “Replacing the Foam and the Top Cover" on
page 173.
• Replace detector into the stack.
• Reconnect the power cable and turn on the detector.
Electronic boards and components are sensitive to electronic discharge (ESD). In order
CAU TI O N
to prevent damage always use an ESD protection (for example, the ESD wrist strap
from the accessory kit) when handling electronic boards and components, see “Using
the ESD Strap" on page 98.
On the G1315B DAD and G1365B MWD the leak sensor can be pulled out without the
NO TE removing the leak pan (the next steps describe the procedure for the G1315A/G1365A).
12 Remove the leak pan from the cabinet bottom. 13 Remove the leak sensor assembly from the leak pan.
14 Replace the leak sensor assembly into the leak pan. 15 Route the leak sensor cable through the z-plane.
16 Replace the leak pan into the cabinet bottom. Next steps:
• Reconnect the leak sensor cable to the processor board
(J21).
• Replace the optical unit, see “Installing the Optical Unit
(G1315A/G1365A)" on page 169 or “Installing the
Optical Unit (G1315B/G1365B)" on page 171.
• Replace the front cover, top cover and top foam section,
see “Replacing the Foam and the Top Cover" on
page 173.
• Replace the detector into the stack.
• Reconnect the cables.
• Turn on the detector.
Preparations for this procedure: 1 The status light pipe is clipped into the top cover.
Next steps:
• Replace the top cover, see “Replacing the Foam and the Top Cover" on page 173.
• Replace the detector into the stack and reconnect the cables and capillaries.
• Turn on the detector.
Use this procedure for the the G1315A/G1365A only. For G1315B/G1365B detectors refer
NO TE to “Installing the Optical Unit (G1315B/G1365B)" on page 171
The fan must be installed in the correct orientation to ensure correct cooling and
CAU TI O N
operation of the detector, see “Exchanging the Fan (G1315A/G1365A)" on page 146.
Preparations for this procedure: 1 Check that the shock absorbers and the leak sensor cable
is placed correctly.
• The power supply, the fan and the processor board are
already installed.
2 Carefully insert the optical unit into the instrument holding 3 Reconnect the SCI cable (J23) and the holmium oxide filter
the one hand at back of the heat sink. motor (J19) to the detector main board.
4 Replace the two rubber shock absorbers and reconnect Next steps:
the ground connector.
• Reinstall the fan assembly (J16). Ensure the correct
direction of air flow.
• Reinstall the flow cell cover, see “Cleaning or
Exchanging the Holmium Oxide Filter" on page 125.
• Reinstall the flow cell, see “Exchanging a Flow Cell" on
page 104.
• Reinstall the lamps, see “Exchanging a Lamp" on
page 101.
• Reinstall the front cover, top cover and top foam
section, see “Replacing the Foam and the Top Cover" on
page 173.
• Replace detector into the stack.
• Reconnect the power cable and turn on the detector.
Use this procedure for the the G1315B/G1365B only. For G1315A/G1365A detectors refer
NO TE to “Installing the Optical Unit (G1315A/G1365A)" on page 169.
The fan must be installed in the correct orientation to ensure correct cooling and
CAU TI O N
operation of the detector, see “Replacing Fan Parts (G1315B/G1365B)" on page 148.
Preparations for this procedure: 1 Check that the shock absorbers and the leak sensor cable
is placed correctly.
• The power supply, the fan and the processor board are
already installed.
2 Carefully insert the optical unit into the instrument holding 3 Reconnect the SCI cable (J23) and the holmium oxide filter
the one hand at back of the heat sink. motor (J19) to the detector main board.
4 Replace the two rubber shock absorbers and reconnect Next steps:
the ground connector.
• Reinstall the fan assembly (J16). Ensure the correct
direction of air flow.
• Reinstall the flow cell cover, see “Cleaning or
Exchanging the Holmium Oxide Filter" on page 125.
• Reinstall the flow cell, see “Exchanging a Flow Cell" on
page 104.
• Reinstall the lamps, see “Exchanging a Lamp" on
page 101.
• Reinstall the front cover, top cover and top foam
section, see “Replacing the Foam and the Top Cover" on
page 173.
• Replace detector into the stack.
• Reconnect the power cable and turn on the detector.
Prerequisites The detector is open and other procedures have been carried out
Preparations for this procedure: 1 Route the lamp connector cables through the hole in the
foam.
• All the work within the module should be completed.
2 Insert the foam and make sure that the foam is installed 3 Press the lamp cables into the foam channel and
correctly. reconnect the lamp connectors to the front panel.
4 Reconnect the lamps. 5 Slide the top plate towards the rear and fix the top plate
screws.
Ensure correct
fit with Z-plane
6 Replace the cover. 7 If required, insert the interface board and fix the screws.
8 Replace waste funnel assembly and the front panel. Next steps:
• Replace the detector into the stack.
• Reconnect the hydraulic connections
• Reconnect the power cable and turn on the detector.
In case you insert the left or right side in the opposite position, you may not be able
WA RN ING
to remove the side from the top part.
1 Place the top part on the bench and insert the left and right 2 Replace the cover.
side into the top part.
3 Replace the detector into the stack and reconnect the cables and capillaries.
4 Turn on the detector.
When required For all repairs inside the detector or for installation of the board
Part required Interface board (BCD) G1351-68701 with external contacts and BCD outputs
Interface board (LAN) see “LAN Board" on page 249.
Tools required None
1 Install the ESD strap. Move the power lock across the 2 If required, unscrew and remove the interface board. Place
power inlet. the board on the ESD kit.
ESD strap
power lock
3 If required, insert the interface board and fix the screws. Next steps:
• Remove the ESD strap.
• Reinstall the module into the stack.
The G1315B DAD and the G1365B MWD require firmware revision 4.x or above (main and
NO TE resident).
3 If detector main board was replaced, reenter the serial number information
of the module through the user interface, see “Entering the Serial Number
using the Control Module" on page 144 or “Entering the Serial Number
using the Agilent ChemStation" on page 145.
5
Identifying Parts and Materials
Overview of Main Assemblies 180
Optical Unit Assembly 182
Standard Flow Cell 184
Semi-Micro Flow Cell 186
High Pressure Flow Cell 188
500 nl Flow Cell 190
Fan Assembly Parts 192
Holmium Oxide Filter 193
Coupling Lens Assembly 194
Source Lens (Achromat) Assembly 195
Cell Support Assembly 196
Control Module 197
Sheet Metal Kit (G1315A/G1365A) 198
Sheet Metal Kit (G1315B/G1365B) 199
Plastic Parts 200
Foam Parts 201
Power and Status Light Pipes 202
Leak Parts 203
Accessory Kit 204
Cable Overview 206
RS-232 Cable Kit 221
LAN Cables 222
3 1
2 10 8 9 10 11 5 13 12
Figure 35 Overview of Main Assemblies
2 Power supply , for power and status light parts, see page 202 0950-2528
Fuse for BCD board, 250 mA (total of 4 are on the board) 2110-0004
4 Fan assembly, for G1315B/G1365B heater and sensor see page page 192 3160-1016
5 Optical unit (exchange assembly), for additional optical unit parts, see page 182 G1315-69002
8 For details see page 184 for standard flow cell, page 186 for semi-micro flow cell, or
page 188 for high-pressure flow cell
2 Semi-flow cell, 6 mm, 5 µl, maximum pressure 120 bar, see page 184 G1315-60011
2 Standard flow cell, 10 mm, 13 µl, maximum pressure 120 bar, see page 184 G1315-60012
2 High Pressure flow cell, 6 mm 1.7 µl, maximum pressure 400 bar, see page 188 G1315-60015
5 Inlet capillary, 380 mm lg, 0.17 mm i.d., 0.6 mm o.d., for details see page 204 G1315-87311
13 Spring, for other holmium oxide filter parts, see page 193 1460-1510
14 Coupling lens assembly, for other coupling lens assembly parts, see page 194 G1103-68001
15 Source lens (achromat) assembly, for other source lens assembly parts, see page 195 G1315-65201
16 Cell support assembly, for other cell support assembly parts, see page 196 G1315-65202
13
9
12
14
15 1
16
4
3
2
7
11 10
5
17
6 Gasket BACK (Teflon), 2.3 mm hole, outlet side See kits below
7 Gasket FRONT (Teflon), 1.3 mm hole, inlet side See kits below
Cell repair kit STD, includes window screw kit, 4mm kexagonal G1315-68712
wrench and seal kit
Seal kit BACK for STD flow cell, qty=12 of item 6 G1315-68711
Seal kit FRONT for STD flow cell, qty=12 of item 7 G1315-68710
NOTE
Gaskets # 6 and #7 have different hole
diameters.
8
7
6
5
4
3
2
1
9
10
11
1 - window screw
2 - spring washers
3 - compression washer
4 - window holder
5 - quartz window
6 - Gasket
6 Gasket BACK (Teflon), 1.8 mm hole, outlet side See kits below
7 Gasket FRONT (Teflon), 1.3 mm hole, inlet side See kits below
Seal kit BACK for semi-micro flow cell, qty=12 of item 6 79883-68702
Seal kit FRONT for semi-micro flow cell, qty=12 of item 7 G1315-68710
NOTE
Gaskets # 6 and #7 have different hole
diameters.
8
7
6
5
4
3
2
1
9
10
11
1 - window screw
2 - spring washers
3 - compression washer
4 - window holder
5 - quartz window
6 - Gasket
6
5
4
2
3
2
12 11 3, 4 2
3, 4
13
5
10
7
16 8 9
14 15
17
11 Cell Housing 10 mm
4 Spring 1460-1510
When the filter motor has been removed, the filter lever should not be reused. Use always a
NO TE new filter lever to assure correct fit on the filter motor shaft.
3 1
2
4
1 Retainer ring
2 Washer-spring wavy
3 Lens support
4 Lens
5 Lens holder
1
2
4 Holder
When the filter motor has been removed, the filter lever should not be reused. Use always a
NO TE new filter lever to assure correct fit on the filter motor shaft.
1
2
3
Control Module
For the information on the sheet metal kit for the G1315B and G1365B refer to “Sheet Metal
NO TE Kit (G1315B/G1365B)" on page 199.
2
1
5 1
3
4
For the information on the sheet metal kit for the G1315A and G1365A refer to “Sheet Metal
NO TE Kit (G1315A/G1365A)" on page 198.
1 Sheet metal kit includes case, top cover and front G1315-68721
2
1
3
4
1
Plastic Parts
For correct assembling of the top and sides, see “Assembling the Main Cover" on page 176.
NO TE
Foam Parts
4
AIRFLOW 1
G1315/65A
G1315/65B
Washer 2190-0409
3
2
Leak Parts
5 Clip 5041-8387
2
4
3
1
6
Accessory Kit
This kit contains some accessories and tools needed for the installation and
repair of the detector.
3 Capillary column – detector 380 mm lg, 0.17 i.d. includes items G1315-87311
4, 5 and 6 (not assembled)
4
5
6
This end is
3 pre-installed
Cable Overview
Never use cables other than the ones supplied by Aligent Technologies to ensure
WA RN ING
proper functionality and compliance with safety or EMC regulations.
LAN cable Twisted pair cross over LAN cable, 10 feet long 5183-4649
(for point to point connection)
Category 5 UTP cable, 8 m long G1530-61480
(for hub connections)
Analog Cables
1 Shield Ground
2 Not connected
3 Center Signal +
4 Connected to pin 6
5 Shield Analog -
6 Connected to pin 4
7 Key
8 Not connected
1 Not connected
2 Shield Analog -
3 Center Analog +
1 Not connected
2 Black Analog -
3 Red Analog +
Remote Cables
START and STOP are connected via diodes to pin 3 of the 3394 connector.
NO TE
BCD Cables
10 1 BCD 5 20
11 2 BCD 7 80
3 3 BCD 6 40
9 4 BCD 4 10
7 5 BCD0 1
5 6 BCD 3 8
12 7 BCD 2 4
6 - Key 4 8 BCD 1 2
1 9 Digital ground
2 15 +5V Low
1 1 BCD 5 20
2 2 BCD 7 80
3 3 BCD 6 40
4 4 BCD 4 10
5 5 BCD0 1
6 6 BCD 3 8
7 7 BCD 2 4
8 8 BCD 1 2
9 9 Digital ground
NC 15 +5V Low
Green 1 BCD 5 20
Violet 2 BCD 7 80
Blue 3 BCD 6 40
Yellow 4 BCD 4 10
Black 5 BCD0 1
Orange 6 BCD 3 8
Red 7 BCD 2 4
Brown 8 BCD 1 2
White 15 +5 Vt Low
Auxiliary Cable
White 1 Ground
Green 3
Yellow 4
Grey 5 DC + 5 V IN
Pink 6 Vent
CAN Cable
Both ends of this cable provide a modular plug to be connected to Agilent 1100
Series module’s CAN-bus connectors.
One end of this cable provides a 15-pin plug to be connected to Agilent 1100
Series module’s interface board. The other end is for general purpose.
White 1 EXT 1
Brown 2 EXT 1
Green 3 EXT 2
Yellow 4 EXT 2
Grey 5 EXT 3
Pink 6 EXT 3
Blue 7 EXT 4
Red 8 EXT 4
Instrument PC
DCD 1 1 DCD
RX 2 2 RX
TX 3 3 TX
DTR 4 4 DTR
GND 5 5 GND
DSR 6 6 DSR
RTS 7 7 RTS
CTS 8 8 CTS
RI 9 9 RI
DB9 DB9 DB9 DB9
Male Female Female Male
LAN Cables
Recommended Cables
For point to point connection (not using a network hub) use a twisted pair
cross over LAN cable (P/N 5183-4649, 10 feet long).
For standard network connections using a hub use category 5 UTP cables,
(P/N G1530-61480, 8 m long).
6
Introduction to the Detector
Introduction to the Detector 224
Optical System Overview 225
Electrical Connections 228
Instrument Layout 230
Early Maintenance Feedback (EMF) 231
Electronics 232
Detector Main Board (DAM/MWM) 233
Firmware Description 241
Raw Data Conversion to Absorbance 243
Optional Interface Boards 248
Interfaces 250
Setting the 8-bit Configuration Switch 254
The Main Power Supply Assembly 259
Optical System
The optical system of the detector is shown in Figure 57. Its illumination
source is a combination of a deuterium-arc-discharge lamp for the ultraviolet
(UV) wavelength range and a tungsten lamp for the visible (VIS) and
short-wave near-infrared (SWNIR) wavelength range. The image of the
filament of the tungsten lamp is focused on the discharge aperture of the
deuterium lamp by means of a special rear-access lamp design which allows
both light sources to be optically combined and share a common axis to the
source lens. The achromat (source lens) forms a single, focused beam of light
through the flow cell. Each cell room and lamp are separated by a quartz
window which can be cleaned or replaced. In the spectrograph, light is being
dispersed onto the diode array by a holographic grating. This allows
simultaneous access to all wavelength information
Cell suppor
window
Tungsten lamp Flow cell
Coupling lens
Spectro len
Deuterium lamp Slit
Grating
Lamps The light source for the UV-wavelength range is a deuterium lamp with a
shine-through aperture. As a result of plasma discharge in low-pressure
deuterium gas, the lamp emits light over the 190-nm to approximately 800-nm
wavelength range. The light source for the visible and SWNIR wavelength
range is a low noise tungsten lamp. This lamp emits light over the wavelength
range 470 – 950 nm.
Achromat The achromat receives the light from both lamps and focuses it so that the
(Source Lens) beam passes through the flow cell.
Holmium Oxide The holmium oxide filter is electromechanically actuated. During the holmium
Filter filter test it moves into the light path.
Cell Support Win- The cell support window assembly separates the holmium filter area from the
dow flow cell area.
Flow Cell Com- The optical unit has a flow cell compartment for easy access to flow cells. A
partment variety of optional flow cells can be inserted using the same quick, simple
mounting system. The flow cell can be removed to check the optical and
electronic performance of the detector without having influences from the
flow cell.
Spectrograph The spectrograph material is ceramic to reduce thermal effects to a minimum.
The spectrograph consists of the spectrograph lens, the variable entrance slit,
the grating and the photodiode array with front-end electronics. The
spectrograph lens refocuses the light beam after it has passed through the flow
cell. The sampling interval of the diode array is < 1 nm over the wavelength
range 190 – 950 nm. Depending on the wavelength this varies from 1.0 to 1.25
diodes per nanometer (for example a diode every 0.8 to 1 nm).
For a small wavelength range, the small non-linearity could be neglected. With
the wavelength range from 190 – 950 nm a new approach is required to
achieve wavelength accuracy over the full range. Each spectograph is
calibrated individually. The calibration data is stored in the spectrograph on
an EEPROM. Based on these data, the built-in processors calculate absorbance
data with linear intervals (1.0, 2.0, …) between data points. This results in an
excellent wavelength accuracy and instrument-to-instrument reproducibility.
Variable Entrance The micro-slit system makes use of the mechanical properties of silicon
Slit System combined with the precise structuring capabilities of bulk micro-machining. It
combines the required optical functions — slit and shutter — in a simple and
compact component. The slit width is directly controlled by the
micro-processor of the instrument and can be set as method parameter.
Grating The combination of dispersion and spectral imaging is accomplished by using
a concave holographic grating. The grating separates the light beam into all its
component wavelengths and reflects the light onto the photodiode array.
Diode Array The diode array is a series of 1024 individual photodiodes and control circuits
located on a ceramic carrier. With a wavelength range from 190 – 950 nm the
sampling interval is < 1 nm.
Electrical Connections
• The GPIB connector is used to connect the detector with a computer. The
address and control switch module next to the GPIB connector determines
the GPIB address of your detector. The switches are preset to a default
address (see “GPIB Default Addresses" on page 255) which is recognized
once after power is switched on.
• The CAN bus is a serial bus with high speed data transfer. The two
connectors for the CAN bus are used for internal Agilent 1100 Series
module data transfer and synchronization.
• Two independent analog outputs provide signals for integrators or data
handling systems.
• The interface board slot is used for external contacts and BCD bottle
number output or LAN connections.
• The REMOTE connector may be used in combination with other analytical
instruments from Aligent Technologies if you want to use features such as
start, stop, common shut down, prepare, and so on.
• With the appropriate software, the RS-232C connector may be used to
control the detector from a computer through a RS-232C connection. This
connector is activated and can be configured with the configuration switch
next to the GPIB connector (see “Communication Settings for RS-232C
Communication" on page 255). See your software documentation for
further information.
• The power input socket accepts a line voltage of 100 – 120 V or
220 – 240 V AC ± 10 % with a line frequency of 50 or 60 Hz. Maximum power
consumption is 300 VA/125 W. There is no voltage selector on your detector
because the power supply has a wide-ranging capability. There are no
externally accessible fuses, because automatic electronic fuses are
implemented in the power supply. The security lever at the power input
socket prevents that the detector cover is taken off when line power is still
connected.
Never use cables other than the ones supplied by Aligent Technologies to ensure
WA RN ING
proper functionality and compliance with safety or EMC regulations.
Analog signals
APG remote
RS-232C
Configuration switch
Instrument Layout
The industrial design of the detector incorporates several innovative features.
It uses Agilent’s E-PAC concept for the packaging of electronics and
mechanical assemblies. This concept is based upon the use of expanded
polypropylene (EPP) layers of foam plastic spacers in which the mechanical
and electronic boards components of the detector are placed. This pack is then
housed in a metal inner cabinet which is enclosed by a plastic external
cabinet. The advantages of this packaging technology are:
• virtual elimination of fixing screws, bolts or ties, reducing the number of
components and increasing the speed of assembly/disassembly,
• the plastic layers have air channels molded into them so that cooling air can
be guided exactly to the required locations,
• the plastic layers help cushion the electronic and mechanical parts from
physical shock, and
• the metal inner cabinet shields the internal electronics from
electromagnetic interference and also helps to reduce or eliminate radio
frequency emissions from the instrument itself.
EMF Counters
The detector provides two EMF counters for the lamps. The counters
increment increments with lamp use, and can be assigned a maximum limit
which provides visual feedback in the user interface when the limit is
exceeded. The counters can be reset to zero after the lamp is exchanged. The
detector provides the following EMF counters:
• Deuterium Lamp On-Time
• Tungsten Lamp On-Time
Electronics
The electronics are comprised of four main components:
• detector main board (DAM/MWM), see page 233.
• power supply, see page 259.
Optional:
• interface board (BCD/external contacts), see page 248.
• interface board (LAN), see page 249.
Main processor
The Motorola MC 68332 microprocessor acts as the main processor with a
clock frequency of 16 MHz. It exchanges data with the ASIC through the core
bus as well as with the PSRAM (pseudo-static random access memory) of
2 × 512 kilobyte, the flash EEPROM (electrically erasable programmable
read-only memory) of 1 MB and the 1 × 32 KB battery-backed
NV-RAM (non-volatile). Battery life is designed to last for more than 25 years
under normal operating conditions.
Control lines provide communication to the lamp supply section, which
controls the deuterium and tungsten lamps. The main processor is connected
to the SSP (signal and spectra processor) through an 8-bit parallel bus.
Firmware
For an outline of the firmware, see “Firmware Description" on page 241. In
case you require exact mathematical equations for the transformation, see the
Understanding Your Agilent ChemStation handbook.
Leak Sensor
This block consists of a PTC for the leak detection and a NTC for the ambient
temperature compensation. A leak would cool down the PTC and this change
in resistance would generate a leak signal.
Fan Drive
The operation of the fan is controlled by the main processor and runs with
constant revolution. The fan produces a sense signal which is derived from the
revolution. This sense signal is used for diagnostics.
On-board Battery
An on-board lithium battery buffers the electronic memory when the module
is turned off.
For safety information on lithium batteries see “Lithium Batteries
Information" on page 295.
“B”
8-bit Heater
switch PWM drivers
ASIC
CAN Holmium
Motor driver motor
driver
REMOTE
driver Interface
board
RS-232
Real time
C driver Main Memory
clock
processor
Deuterium
Safety Lamp
Control lines lamp
lock supply
block Tungsten
Diagnostic data
lamp
SSP
PWM signal and Serial bus
PFP
drivers spectra processor Array
function
Analo and slit
block
gout 1
Low pass SSP RAM
filters
and
signal
SSP ASIC
conditionin
Analog g
out 2
MPS main
SIMM power
supply
memory module
SCI Board
The SCI (spectrograph connector interface), located on the optical unit
assembly is the interface between micro-slit, PDA and detector main board. In
addition, wavelength calibration data and manufacturing data from the
manufacturing process (for example, serial number, dates, and so on) are
stored in the EEPROM.
A/D Converter
The output signal from the PDA signal conditioning electronics is directed to
the 16-bit /160-kHz A/D converter. Multiplexing is used to monitor test signals
for diagnostic purposes including GND, reference voltage (Vref), and a ramp
signal. These signals are used to verify the front end electronics separately
from the PDA. The signal from the PDA temperature sensor is used for
temperature compensation.
Analog Outputs
There are two independent analog outputs (0…1 V full scale). Digital data from
the ASIC is converted into a pulse-width modulated signal (PWM). The PWM
signal is then fed to an amplitude modulator, which precisely turns the
reference signal on and off. This signal then passes to a low-pass filter section.
DAM/MWM
PFP ASIC
DAM/MWM Control Function Block / SSP Processor
SCI board
PDA signal
Test signals, PDA
GND, Vref signal conditioning PDA temperature sensor
ramp electronics
Filament
Deuterium lamp
filament control
Shut down
Deuterium lamp Anode
current control
Control bus
Deuterium
DAM/MWM Control Function Block
lamp sense
Tungsten lamp
voltage control
Diagnostic
A/D converter
Control bus
Safety Switches
If the EPP foam is removed while the instrument is still on, the safety light
switches are activated and the deuterium lamp, the tungsten lamps and the
fan are switched off.
Interfaces
For detailed information on interfaces, see “Interfaces" on page 250.
Temperature Control
The G1315B/G165B detectors are equipped with a temperature control to
improve the baseline stability in unstable environments (e.g. strong variation
of the temperature due to air condition systems). A heater and a temperature
sensor assembly have been added and are controlled by the detector main
board and its firmware. The temperature at the fan is compared with a
temperature sensor on the main board. Depending on the difference the heater
in front of the fan is controlled. There are no parameters to be set for the
temperature control.
Firmware Description
The firmware of the instrument consists of two independent sections:
• a non-instrument specific section, called resident system,
• an instrument specific section, called main system.
Resident System
This resident section of the firmware is identical for all Agilent 1100 series
modules. Its properties are:
• the complete communication capabilities (GPIB, CAN and RS-232C),
• memory management,
• ability to update the firmware of the ‘main system’.
Main System
Its properties are:
• the complete communication capabilities (GPIB, CAN, LAN and RS-232C),
• memory management,
• ability to update the firmware of the resident system.
In addition the main system comprises the instrument functions that are
divided into common functions like
• run synchronization through APG remote
• error handling,
• diagnostic functions,
• or module specific functions like
• internal events such as lamp control, filter movements,
• raw data collection and conversion to absorbance (see “Raw Data
Conversion to Absorbance" on page 243.
Firmware Updates
Firmware updates can be done using your user interface:
• handheld control module with files from a PC-card or
• Agilent ChemStation with files from floppy disk
The file naming conventions are:
xxxx-vvv.DLB, where
xxxx is the product number, for example, 1315 for the G1315A DAD, and
vvv is the revision number, for example 104 is revision 1.04
For instructions refer to your user interface.
main FW update
Resident System Main System
resident FW update
Gain Correction
During a blank measurement every photodiode is assigned a gain value,
depending on the amount of light falling on the diode array. These gain values
are stored in a table. They are used to adjust the amplification factor in the
signal conditioning electronics. This process is used to adjust small signal
levels to the optimum range of the A/D converter.
The DSP firmware uses the gain table to adjust the dark signal corrected
intensity spectra.
Subtract
Raw data
dark signal
Temperature
Temperatur Gain
e filter correction
Temperatur
ecorrection
Absorbance
calculation
Filtering
Spectra
runbuffer Signal
DAD calculation
Deuterium
line data
Wavelength
axis
Wavelength linearization
calibration
table
Absorbance
LC signals
spectra
Temperature Correction
The quantum efficiency of the photodiode array depends on the temperature
and is different for each wavelength. The temperature dependency follows a
monotone increasing function over the wavelength scale, which means it
increases with longer wavelengths (above 600 nm).
To correct the intensity spectrum for temperature effects, the temperature on
the photodiode array is averaged. With the help of a function, correction
factors for each wavelength are calculated. The temperature factors are used
to correct the intensity spectrum.
Temperature Filter
The temperature filter determines whether the temperature has been changed
significantly. Only in this case, temperature correction is applied.
Rawdata File
The runbuffer within the detector is used for signal and spectra data only. If
the runbuffer is full, no further signal data are entered. This will guarantee
useful signal data but may cause loss of interesting spectral data. The
runbuffer can hold about 90 spectra depending on the settings and may be
expanded by additional memory on the detector main board (SIMM modules).
Peak Detector
The peak detector (PD) always uses signal A as the pilot signal. The PD is
adjusted by means of two setpoints: peakwidth and threshold. Both setpoints
are time-programmable. While the PD-threshold is a method parameter of its
own, the PD-peakwidth parameter is derived from the general peakwidth
(PKWD) parameter. At the start of the run, the value for the PD-peakwidth is
set equal to the PKWD setpoint. The peak detector recognizes changes in the
slope of this signal (upslope, apex, downslope and baseline) and stores spectra
according to the operator’s instructions. During the run the PD-peakwidth
parameter can be changed by time-programming.
Mode Description
apex + baselines last baseline spectrum before peak, top of peak spectrum and first
baseline spectrum after peak is stored.
apex + slopes spectrum in peak upslope, at top of peak and in peak downslope is
stored.
all in peak compared to storing all spectra periodically, only stores spectra
within a peak at doubled period. Starts with last baseline spectrum
before peak and ends with first baseline spectrum after peak. If
baseline spectra are not detected, the spectrum before the first
spectrum in peak or the spectrum after the last spectrum within the
peak is stored instead.
all periodically all spectra are stored. The period depends on the
peakwidth setting. For peakwidth setting=0 (narrowest peak), the
spectrum data rate would be 20 Hz.
all second periodically every 2nd spectra is stored (50 % of mode all).
BCD Board
The BCD board provides a BCD output for the bottle number of the
Agilent 1100 Series autosampler and four external contacts. The external
contact closure contacts are relay contacts. The maximum settings are: 30 V
(AC/DC); 250 mA (fused). There are general purpose cables available to
connect the BCD output, see “BCD Cables" on page 216 and the external
outputs, see “External Contact Cable" on page 220 to external devices.
Board
identification
RFI filter
+ 250 mA
External External contact
contacts 4x connector
LAN Board
The HP JetDirect cards are network interface cards used in HP printers.
One board is required per Agilent 1100 stack. It is recommended to add the LAN board to
NO TE the detector with highest data rate.
The following cards can be used with the Agilent 1100 modules.
Recommended Cables
For point to point connection (not using a network hub) use a twisted pair
cross over LAN cable (part number 5183-4649, 10 feet long).
For standard network connections using a hub use category 5 UTP cables,
(part number G1530-61480, 8 m long).
Interfaces
The Agilent 1100 Series modules provide the following interfaces:
* The vacuum degasser will have a special connector for specific use. For details see description of main board.
Never use cables other than the ones supplied by Aligent Technologies to ensure
WA RN ING
proper functionality and compliance with safety or EMC regulations, see “Cable
Overview" on page 206.
GPIB Interface
The GPIB connector is used to connect the module with a computer. The
address and control switches next to the GPIB connector determine the
GPIB address of your module. The switches are preset to a default address and
recognized by the operating software from Aligent Technologies.
Autosampler 28 Autosampler 28
Pump 22 RID 29
FLD 23
CAN Interface
The CAN is an intermodule communication interface. It is a 2-wire serial bus
system supporting high speed data communication and real-time requirement.
Remote Interface
The APG remote connector may be used in combination with other analytical
instruments from Aligent Technologies if you want to use features such as
common shut down, prepare, and so on.
Remote control allows easy connection between single instruments or systems
to ensure coordinated analysis with simple coupling requirements.
The subminiature D connector is used. The module provides one remote
connector which is inputs/outputs (wired-or technique).
4 SHUT DOWN (L) System has serious problem (for example, leak: stops pump).
Receiver is any module capable to reduce safety risk.
5 Not used
6 POWER ON (H) All modules connected to system are switched on. Receiver
is any module relying on operation of others.
7 READY (H) System is ready for next analysis. Receiver is any sequence
controller.
8 STOP (L) Request to reach system ready state as soon as possible (for
example, stop run, abort or finish and stop injection). Receiver is
any module performing run-time controlled activities.
9 START REQUEST (L) Request to start injection cycle (for example, by start key on
any module). Receiver is the autosampler.
RS-232C
The RS-232C connector is used to control the instrument from a computer
through RS-232C connection, using the appropriate software. This connector
can be activated by the configuration switch module next to the GPIB
connector.
The RS-232C is designed as DCE (Data Communication Equipment) with a
9-pin male SUB-D type connector. The pins are defined as follows:
1 In DCD
2 In RxD
3 Out TxD
4 Out DTR
5 Ground
6 In DSR
7 Out RTS
8 In CTS
9 In RI
Instrument PC
DCD 1 1 DCD
RX 2 2 RX
TX 3 3 TX
DTR 4 4 DTR
GND 5 5 GND
DSR 6 6 DSR
RTS 7 7 RTS
CTS 8 8 CTS
RI 9 9 RI
DB9 DB9 DB9 DB9
Male Female Female Male
Mode Select 1 2 3 4 5 6 7 8
Switches 1 and 2 define which set of parameters (for example, for GPIB,
RS-232C, and so on) will be changed. Once the change has been completed, the
instrument must be powered up again in order to store the values in the
non-volatile memory.
Pump 22 00010110
FLD 23 00010111
VWD 24 00011000
DAD/MWD 26 00011010
Autosampler 28 00011100
RID 29 00011101
where 0 means that the switch is down and 1 means that the switch is up.
Mode Select 1 2 3 4 5 6 7 8
Use the following tables for selecting the setting which you want to use for
RS-232C communication. The number 0 means that the switch is down and 1
means that the switch is up.
3 4 5 3 4 5
0 0 0 9600 1 0 0 9600
0 0 1 1200 1 0 1 14400
0 1 0 2400 1 1 0 19200
0 1 1 4800 1 1 1 38400
0 7 Bit Communication
1 8 Bit Communication
Switches Parity
7 8
0 0 No Parity
1 0 Odd Parity
1 1 Even Parity
One start bit and one stop bit are always used (not selectable).
Per default, the module will turn into 19200 baud, 8 data bit with no parity.
Forced cold start erases all methods and data stored in the non-volatile memory.
CAU TI O N
Exceptions are diagnose and repair log books which will not be erased.
If you use the following switch settings and power the instrument up again, a
forced cold start has been completed.
Mode Select 1 2 3 4 5 6 7 8
TEST/BOOT 1 1 0 0 0 0 0 1
Stay-Resident Settings
Firmware update procedures may require this mode in case of firmware
loading errors.
Switches 1 and 2 do not force storage of this set of parameters in non-volatile
memory. Returning switches 1 and 2 to other positions (other than being both
up) will allow for normal operation.
If you use the following switch settings and power the instrument up again,
the instrument firmware stays in the resident part, that is, it is not operable as
a detector. It only uses basic functions of the operating system for example, for
communication.
Mode Select 1 2 3 4 5 6 7 8
TEST/BOOT 1 1 0 0 1 0 0 0
M P S
+ 3 6 V + 3 6 V (n o t u s e d )
s u p p ly
+ 2 4 V
lin e p rim a ry s u p p ly
v o lta g e + 2 4 V / 4 .5 A
c irc u its
se n se + 5 V
s w itc h in g + 5 V / 3 A
re g u la to r
+ 1 5 V / .3 A
lin e a r v o lta g e
re g u la to rs
-1 5 V / .3 A
To disconnect the instrument from line, unplug the power cord. The power supply
WA RN ING
still uses some power, even if the power switch on the front panel is turned off.
No accessible hardware fuse is needed because the main power supply is safe
against any short circuits or overload conditions on the output lines. When
overload conditions occur, the power supply turns off all output voltages.
Turning the line power off and on again resets the power supply to normal
operation if the cause of the overload condition has been removed.
An over-temperature sensor in the main power supply is used to turn off
output voltages if the temperature exceeds the acceptable limit (for example, if
the cooling fan of the instrument fails). To reset the main power supply to
normal operating conditions, turn the instrument off, wait until it is
approximately at ambient temperature and turn the instrument on again.
The following table gives the specifications of the main power supply.
Output 3 +5V/3A
Output 4 + 15 V / 0.3 A
Output 5 - 15 V / 0.3 A
7
Control Module Screens for Agilent
1100 DAD and MWD
Major keys on the Agilent 1100 Control Module 262
Control Module - Unsupported Module 263
Screens available from the Analysis screen 264
Screens available from the System screen 274
Screens available from the Records screen 276
Diagnostics and Tests 282
Table 44
ESC Return to previous screen and scroll through top layer views (Analysis, Settings)
i Information/help
Enter Store changed parameters or execute the choice from a pull-down menu
For the operation of the G1315B DAD and G1365B MWD you require:
NO TE Minimum Control Module firmware revision B.01.04 (G1323B).
Minimum LC Module firmware revision 4.xx.
Some screens may differ slightly depending on the module type G1315A/B DAD or
G1365A/B MWD.
In case the control module’s display seems to be frozen (hang-up due to a communication
NO TE problem on the CAN bus, unplug the control module from the LC module and reconnect.
The m-key allows access to the context sensitive menu. Setup view leads you
to add sections for additional Agilent 1100 modules. Restart re-boots the
control module.
Lamp ON/OFF
Use the F8 key (On/Off) to turn on the lamp(s). If more than one module is
available, select the DAD or MWD from the pop-up menu.
Setup View
In the Setup view, e.g. another module can be added to the view.
Here, e.g. the column compartment parameters are shown on the display as
well. The number of parameters on the display are restricted as additional
modules are added. Maximum 4 modules are shown automatically. If more
modules are in the system, you have to chose in Setup view.
With the Settings key you open a pull-down menu where you can select the
DAD modules.
Settings
Within the Settings you can change the DAD or MWD parameters and with a
different set of parameters available through the F1-5 keys. F7 key resets the
DAD or MWD to default values. F8 opens a window to turn on the lamps.
Use the m-key for the context sensitive menu. The Status command pulls up a
monitor screen displaying signals and spectra as programmed. Reset will load
the DAD or MWD default parameters. Balance brings the baseline back to set
offset.
Selecting More and Settings pull down menu you can enter special DAD or
MWD setpoints.
Selecting More and Signals C-E on the pull down menu you can enter
additional DAD or MWD signal parameters.
Settings - Timetable
With the F2 key (Timetable) you can list the timetable for the DAD or MWD.
Press F7 key (Insert) to add entries or F6 key (Delete) to remove entries.
Press the F7 key (Insert) to add a timetable events. Use the F6 key (Done) to
view the entered lines of the timetable.
Use the m-key for the context sensitive menu. It gives you additional tools for
the timetable.
Settings - Analog
With the F3 key (Analog) you can change the settings for the analog outputs.
Status
This is an example if an Agilent 1100 DAD or MWD is configured standalone.
Signal plot
Press F6 key (Plot) to enter the plot screen (available also from the Analysis
and System screen). Here you can observe the online signal(s). To add
additional online signals (maximum 3), press F6 key (Select). If more than one
signal is configured (see next), use the 1-2-3 number key to switch between the
signals.
Press F6 key (Select). Here you can add additional online signals (maximum
are 3), press F6 key (Select). Additional signals could be also pressure or
temperature signals from other modules. Use the Right/Left arrows to switch
between Available and Selected Signals. Use the F8 key (Move) to enter
available signals into the box for selected signals or vice versa.
Method screens
Use ESC to return to the Analysis screen. Use the F3 key (Method) to view the
parameters in a method and F8 key (Save As) to save the method in the
module(s). The PC-Card key is only active when a PCMCIA card is inserted in
the control module.
Use F2 key (PC-Card) to save a method on a PCMCIA card. Use the Right/Left
arrows to switch between PC-Card and Instrument window. Use the UP/Down
arrows to select the method. Use the F7/F8 keys (Copy) to enter available
signals into the box for selected signals or vice versa.
System screen
Use the Esc key to receive Views on the F5 key. Choose System from the
pull-down menu. This screen shows the last activities in the system.
System - Control
Use the F1 key (Control) to select the FL-Detector. Here you receive
information about the not-ready conditions if needed. F2 key (Reset) does a
re-initialization of the DAD or MWD.
System - Configuration
Use the Esc key to receive Views on the F5 key. Choose System from the
pull-down menu. Use the F2 key (Configure) to select the DAD or MWD. Here
you define further special setpoints for the DAD or MWD operation.
Use the F1 key (Interfaces) to access the interface settings (if required).
Records screen
Use the Esc key to receive Views on the F5 key. Choose System from the
pull-down menu. Use the F4 key (Records) to select the DAD or MWD. Errors
are reported either into the System Log (F2) or Error Log (F3).
Info Log
Use the m-key to receive a pop-up menu, Select Info Log. A list of the last
events are listed. For troubleshooting reasons they can be printed or saved to a
file on the PCMCIA card.
If a set limit has been exceeded, a message box will pop up. This will not stop a
sequence or run (information only to plan maintenance activities). If you
press Reset, the limits will be removed. Ignore will continue to keep the EMF
flag set.
Firmware Update
Use the Esc key to receive Views on the F5 key. Choose System from the
pull-down menu. Use the F3 key (Records) to select the DAD or MWD. Use the
F5 key (FW Update) to enter the Update section. If you want to update the
resident firmware (together with specific main firmware revisions), select the
a file from the PCMCIA card (RES_n_nn.DLB) and press execute. If you want
to update the main firmware, press F7 key (Transfer) to turn the module into
the resident mode (LED on module should blink yellow).
Use the Esc key to receive Views on the F5 key. Choose System from the
pull-down menu. Use the F3 key (Records) to select the Generic module. In
this screen the resident firmware revision is shown.
Use the F5 key (FW Update) to enter the Update section. Select the file from
the PCMCIA card (1315-nnn.DLB for DAD or 1365-nnn.DLB for MWD) and
press execute. When the update has finished the update, press F7 key
(Transfer) to return the module into the normal mode (LED on module should
stay yellow).
If you have not saved your methods, please do it before continuing. Otherwise
they will be overwritten during the update process.
Maintenance activities
Use the Esc key to receive Views on the F5 key. Choose System from the
pull-down menu. Use the F3 key (Records) to select the DAD or MWD. Use the
F4 key (Maint log) to view and edit the maintenance logbook.
Use the F7 key (Add) to add new maintenance activities. If an activity is not
listed, you can type the activity into the line “Add” using the control modules
key pad.
Tests screen
Use the Esc key to receive Views on the F5 key. Choose System from the
pull-down menu. Use the F3 key (Tests) to select the DAD or MWD. Several
tests are available to test the Agilent 1100 DAD or MWD. Additional test are
listed in the function box. Refer to “Troubleshooting and Test Functions" on
page 49 for more information on the tests.
Intensity Test
Use the F5 key (Intensity) to get the instrument profile (example with UV and
Vis lamp on).
Wavelength Calibration
Use the F1 key (Calibrate) and then F8 key (Execute) to start the DAD or
MWD wavelength calibration (with water in the flow cell). If a deviation is
found, press Adjust.
Use the F6 key (Plot) to view the signal. A simulated chromatogram (4 peaks)
will repeat until the run is stopped. The signal is also available on the analog
output. A change of the peak width will change the retention times.
Slit Test
Use the F3 key (Slit Test) to test the movement of the electromechanical slit
assembly.
8
Specifications
Performance Specifications 288
Performance Specifications
Short term noise ± 1 × 10-5 AU at 254 and 750 nm See “” on page 289
(ASTM)
Single and
Multi-Wavelengt
Drift 2 × 10-3 AU/hr at 254 nm See “” on page 289
Table 45 Performance Specifications Agilent 1100 Series DAD and MWD, continued
ASTM: “Standard Practice for Variable Wavelength Photometric Detectors Used in Liquid
NO TE Chromatography”.
Reference conditions: cell path length 10 mm, response time 2 s, flow 1 ml/min LC-grade
Methanol, slit width 4 nm.
A
Safety Information
General Safety Information 292
Lithium Batteries Information 295
Disposal of Mercury from Deuterium Lamp 296
Radio Interference 297
Sound Emission 298
UV-Radiation 299
Solvent Information 300
Declaration of Conformity for HOX2 Filter 302
Aligent Technologies on Internet 303
General
This is a Safety Class I instrument (provided with terminal for protective
earthing) and has been manufactured and tested according to international
safety standards.
Operation
Before applying power, comply with the installation section. Additionally the
following must be observed.
Do not remove instrument covers when operating. Before the instrument is
switched on, all protective earth terminals, extension cords,
auto-transformers, and devices connected to it must be connected to a
protective earth via a ground socket. Any interruption of the protective earth
grounding will cause a potential shock hazard that could result in serious
personal injury. Whenever it is likely that the protection has been impaired,
the instrument must be made inoperative and be secured against any intended
operation.
Make sure that only fuses with the required rated current and of the specified
type (normal blow, time delay, and so on) are used for replacement. The use of
repaired fuses and the short-circuiting of fuseholders must be avoided.
Some adjustments described in the manual, are made with power supplied to
the instrument, and protective covers removed. Energy available at many
points may, if contacted, result in personal injury.
Any adjustment, maintenance, and repair of the opened instrument under
voltage should be avoided as much as possible. When inevitable, this should be
carried out by a skilled person who is aware of the hazard involved. Do not
Safety Symbols
Table 46 shows safety symbols used on the instrument and in the manuals.
Symbol Description
The apparatus is marked with this symbol when the user should refer to the instruction manual in order to
! protect the apparatus against damage.
A warning alerts you to situations that could cause physical injury or damage to the
WA RN ING
equipment. Do not proceed beyond a warning until you have fully understood and
met the indicated conditions.
A caution alerts you to situations that could cause a possible loss of data. Do not
CAU TI O N
proceed beyond a caution until you have fully understood and met the indicated
conditions.
Danger of explosion if battery is incorrectly replaced. Replace only with the same or
WA RN ING
equivalent type recommended by the equipment manufacturer. Lithium batteries
may not be disposed-off into the domestic waste.
Bij dit apparaat zijn batterijen geleverd. Wanneer deze leeg zijn, moet u ze niet weggooien
NO TE maar inleveren als KCA.
Radio Interference
Never use cables other than the ones supplied by Aligent Technologies to
ensure proper functionality and compliance with safety or EMC regulations.
Sound Emission
Manufacturer’s Declaration
This statement is provided to comply with the requirements of the German
Sound Emission Directive of 18 January 1991.
This product has a sound pressure emission (at the operator position) < 70 dB.
• Sound Pressure Lp < 70 dB (A)
• At Operator Position
• Normal Operation
• According to ISO 7779:1988/EN 27779/1991 (Type Test)
UV-Radiation
Emissions of ultraviolet radiation (200-315 nm) from this product is limited
such that radiant exposure incident upon the unprotected skin or eye of
operator or service personnel is limited to the following TLVs (Threshold Limit
Values) according to the American Conference of Governmental Industrial
Hygienists:
Typically the radiation values are much smaller than these limits:
Solvent Information
Observe the following recommendations on the use of solvents.
Flow Cell
Avoid the use of alkaline solutions (pH > 9.5) which can attack quartz and thus
impair the optical properties of the flow cell.
Prevent any crystallization of buffer solutions. This will lead into a
blockage/damage of the flow cell.
If the flow cell is transported while temperatures are below 5 degree C, it must
be assured that the cell is filled with alcohol.
Aqueous solvents in the flow cell can built up algea. Therefore do not leave
aqueous solvents sitting in the flow cell. Add small % of organic solvents (e.g.
Acetonitrile or Methanol ~5%).
Solvents
Brown glass ware can avoid growth of algae.
Always filter solvents, small particles can permanently block the capillaries.
Avoid the use of the following steel-corrosive solvents:
• Solutions of alkali halides and their respective acids (for example, lithium
iodide, potassium chloride, and so on).
• High concentrations of inorganic acids like nitric acid, sulfuric acid
especially at higher temperatures (replace, if your chromatography method
allows, by phosphoric acid or phosphate buffer which are less corrosive
against stainless steel).
• Halogenated solvents or mixtures which form radicals and/or acids, for
example:
2CHCl3 + O2 → 2COCl2 + 2HCl
This reaction, in which stainless steel probably acts as a catalyst, occurs
quickly with dried chloroform if the drying process removes the stabilizing
alcohol.
• Chromatographic grade ethers, which can contain peroxides (for example,
THF, dioxane, di-isopropylether) such ethers should be filtered through dry
aluminium oxide which adsorbs the peroxides.
• Solutions of organic acids (acetic acid, formic acid, and so on) in organic
solvents. For example, a 1-% solution of acetic acid in methanol will attack
steel.
• Solutions containing strong complexing agents (for example, EDTA,
ethylene diamine tetra-acetic acid).
• Mixtures of carbon tetrachloride with 2-propanol or THF.
Table 49
Wavelength Accuracy
G1600A ± 1 nm
__________________ _______________
Engineering Manager Quality Manager
margins for negative absorbance, 43 safety standards, 16 using the ESD strap, 98
of selectivity, 44 weight and dimensions, 16 warnings and cautions, 96
overview, 31 power considerations, 14 replacing interface board (ECB), 177
peak width, 34 power consumption, 16 Replacing the Fan Parts ("B"), 148
sample and reference wavelength, 36 power cords, 14 response time (peak width), 34
slit width, 39 power supply RS-232C
spectra acquisition, 42 description, 259 cable kit to PC, 221
theshold, 43 specifications, 260 communication settings, 255
programmable slit width, 288 interface, 253
P settings, 256
R
parts identification, 179 S
500 nl flow cell, 190 range, 42
accessory kit, 204 rawdata file, 246 safety information
achromat (source lens), 195 rear view of module, 23 on lithium batteries, 295
cable overview, 206 recalibration of wavelength, 50, 84, 283 standards, 16
cables - analog, 208 Repairing, 95 sample and reference wavelength, 36
cables - APG remote, 211 repairs sample, holmium and dark current
cables - auxiliary, 218 assembling main cover, 176 spectrum, 283
cables - BCD, 216 cleaning the instrument, 97 selectivity optimization, 44
cables - CAN, 219 correction leaks, 128 sensor for fan, 192
cables - external contact, 220 definition of, 96 serial number
cables - LAN cables, 222 exchanging a flow cell, 104 entered on ChemStation, 145
cell support, 196 exchanging a lamp, 101 entered on control module, 144, 280
control module, 197 exchanging holmium oxide filter, 125 serial number change with control
coupling lens, 194 exchanging internal parts, 136 module, 280
foams and dampers, 201 exchanging leak sensor, 165 site requirements, 14
high pressure (micro) flow cell, 188 exchanging main board (DAM), 141 slit width, 39
holmium oxide filter, 193 exchanging power supply, 162 specifications
leak panels, 203 exchanging the achromat, 156 analog outputs, 289
main assemblies, 181 exchanging the fan ("A"), 146 communications, 289
optical unit, 182 installing optical unit, 169, 171 diode width, 288
overview, 180 introduction, 96 flow cell, 288
plastics, 200 of the detector, 3, 95 GLP features, 289
power and status, 201, 202 removing the optical unit, 152, 154 linear range, 288
semi-micro flow cell, 186 removing top cover and foam, 138 noise and drift (ASTM), 288
sheet metal, 198, 199 replacing cell support window, 133 programmable slit width, 288
standard flow cell, 184 replacing coupling lens, 130 safety and maintenance, 289
union holder/ZDV, 198, 199 replacing filter motor, 160 wavelength accuracy/bunching, 288
peak detector, 246 replacing firmware, 178 wavelength range, 288
peak width (response time), 34 replacing foam and top cover, 173 spectra
performance replacing leak handling system, 129 acquisition, 42
optimization, 30 replacing semi-micro flow cell acquisition modes, 247
photometric accuracy, 34 capillaries, 118 acquisition range, 42
physical specifications, 16 replacing status light pipe, 168 acquisition step and threshold, 42
humidity, 16 replacing STD flow cell capillaries, 113 run buffer, 245
line voltage and frequency, 16 simple repairs overview, 99 spectrograph, 225, 226
operation temperature, 16 the high pressure flow cell, 111 diodes per nm, 226
power consumption, 16 the standard/semi-micro flow cell, 107 stack configuration, 20, 21
front view, 20
rear view, 21
steps, 42
T
temperature control, 240
test chromatogram on control module, 284
test functions, 50
tests
dark current, 85, 91
filter, 85, 93
flow cell, 85, 90
holmium oxide, 85
intensity, 85, 88
overview, 85
tests on control module, 282
threshold, 43
troubleshooting
error messages, 50, 53
status indicators, 50, 51
U
unpacking, 17
unsupported Module, 263
using EMF, 231
uv-radiation, 299
V
variable entrance slit, 226
W
wavelength
accuracy and bunching, 288
range, 288
recalibration, 50, 84, 283
weight and dimensions, 16
*G1315-90004*
*G1315-90004*
G1315-90004