DLT-100 Liquid-Water Isotope Analyzer: Los Gatos Research
DLT-100 Liquid-Water Isotope Analyzer: Los Gatos Research
DLT-100 Liquid-Water Isotope Analyzer: Los Gatos Research
DLT-100
Liquid-Water Isotope Analyzer
Automated Injection
Table of Contents
Table of Contents .......................................................................................................... 2
Instrument Setup........................................................................................................... 3
AutoInjector Setup ................................................................................................. 3
LWIA Setup ............................................................................................................. 3
Measuring Samples....................................................................................................... 7
File Transfer................................................................................................................. 19
Instrument Setup
AutoInjector Setup
1. Assemble Injection Unit, Keypad terminal, Safety Shield, and Power Supply as per
instructions in Chapter 6 of the LC PAL User Manual. Place autoloader on the right
side of the DLT, and attach keypad to the left side of the autoloader.
2. Setup Trayholder reference position as per instructions in Chapter 7 of the LC PAL
User Manual. Do NOT have a syringe installed for this step (breakage is possible).
3. Setup septum reference position as per instructions in Chapter 7 of the LC PAL User
Manual. Use injector “LCVlv1” as the septum location and do NOT have a syringe
installed for this step (breakage is possible).
4. Insert syringe as per instructions in Chapter 8 of the LC PAL User Manual. Manual
priming is not necessary for this syringe. Confirm that the syringe has some resistance
when manually actuated. If there is little to no resistance, tighten the syringe nut slightly.
When inserting the syringe holder into the Autoinjector, extra caution is required to
assure that the syringe needle does not bend.
LWIA Setup
1. Connect the instrument power cord to switched power entry module and the pump power
cord to the slave outlet labeled “Ext. Pump Power” on the LWIA. Use the voltage
selection switch to select the line voltage (e.g. 115 VAC or 210 VAC).
2. Connect the 3/8” pump connection to labeled 3/8” Swagelok port labeled “To Ext. Pump”
on the LWIA via the provided Teflon tubing. The connection should be tightened to ¼ -
½ turn past finger-tight using a wrench and leave a gap of < 3.5 mm.
< 3.5 mm
3. Connect the Drietite Laboratory Gas Drying unit to the labeled ¼” Swagelok port on
LWIA labeled “Dry Gas Inlet” via the provided ¼” Teflon tubing. The connection
should be tightened to ¼ - ½ turn past finger-tight using a wrench and leave a gap of <
3.5 mm. Remove the plastic gas plug. (NOTE – if using dry gas from a cylinder or
house dry gas system, make sure that the inlet pressure is between 0 – 5 psig).
< 3.5 mm
Remove
Plug
4. Connect the septum heater plug and 1/8” Teflon tube with filter assembly from the
Autoinjector septum block to the back of the LWIA. The connection should be tightened
to ¼ - ½ turn past finger-tight using a wrench and leave a gap of < 3.5 mm.
5. Connect the serial communications cable from the Autoinjector to the LWIA serial
connector labeled “LC-PAL”.
1. Change the septum in the autoinjector septum block as described in the “Changing Septa”
section.
2. Remove the syringe from the autoinjector and manually rinse with de-ionized water to
remove any salt build-up or septum residue that has collected in the syringe. Confirm
that the syringe has some resistance when manually actuated. If there is little to no
resistance, tighten the syringe nut slightly. When inserting the syringe holder into the
Autoinjector, extra caution is required to assure that the syringe needle does not bend.
Every 3 – 6 days:
1. Adjust the Laser Offset, if necessary (as described in the “Adjusting Laser Offset”
section).
2. Clean the sample transfer line and filter assembly as described in the “Cleaning the
Sample Transfer Line and Filter Assembly” section.
Measuring Samples
NOTE: The below example outlines the measurement of 3 samples with 3 reference
standards interspersed between the samples. Each vial is injected 6 times.
1. Load Tray 1(lower left Tray) with the reference standards (“REF 1” – “REF 3”) in positions
1 – 3.
2. Load Tray 1 with the unknown samples (“SAMPLE 1” – “SAMPLE 3”) in positions 4 – 6.
4. Depress the “INSERT” button 5 times to add 5 additional samples to the SAMPLE LIST:
5. Using the mouse and keyboard, rename the first 3 samples as the references (“REF 1” –
“REF 3”) and last 3 samples appropriately (“SAMPLE 1” – “SAMPLE 3”):
6. Use the top set of arrow keys (“->”) to transfer samples from the SAMPLE LIST to the RUN
LIST. Alternate between the references (“REF 1” …) and the unknown samples (“SAMPLE
1” …). After populating the RUN LIST, use the back arrow key (“<-“) to remove the top
“NULL” entry. The resulting configuration screen is shown below:
8. The run is now fully configured. Depress the “RUN” button to transfer to the expanded run
screen. This screen shows the exact sequence of measurements that will be taking place.
9. Depress the PLAY button (play arrow) to start the measurements. The instrument will go
through a series of flush cycles (e.g. filling with dry air and then evacuating) for ~ 2 minutes
to purge residual water. The autoinjector will then move to position 1 on Tray 1 and transfer
~ 1 microliter of water into the injection port. The needle will remain in the port for 60
seconds, withdraw, and wait 10 seconds to assure complete sample evaporation. The
instrument will then start taking data. If the “SPECTRUM” button is depressed, the
measured spectrum will be shown. The observed spectrum should be similar to that shown
below. Note that the transmission (top panel) should be 0.3 – 3.0 Volts and show marked
dips due to the water injection. The absorption spectrum (bottom panel) should show
absorption on the order of 10 – 60 %. The large, central peak near -1.0 GHz should be
roughly centered in shaded grey box.
10. Over the course of the run, switching back to “RUN” mode will show the measurement list
being populated as subsequent samples are measured.
11. The sample run can be stopped or paused at any time via the indicated buttons in the RUN
Mode. Note that the current sample will be completed prior to pausing/stopping.
12. Once the run is complete (or prematurely stopped), the data will be saved to the file indicated
in the center of the control panel (“h2o_20070319_001.txt”). The data analysis procedure is
outlined in a separate section.
4. The only columns required for data analysis are “Sample_name”, “D_H” and
“O18_O16”. Example data is shown below for a run that consisted of 5 standards (“Std
10”, “TRIN”, “LGR”, “GSDI”, and “Std 7”) interspersed amongst 5 unknowns (“1”, “2”,
“3”, “4”, and “5”). There are 6 injections for each vial:
6. The D/H and 18O/16O values for the 4th – 6th injection for each sample will be averaged
together to yield:
7. Using the known isotope ratios for the standards, δD (‰) and δ18O (‰), determine the
actual D/H and 18O/16O atomic ratios for the standards:
D δD
= + 1 * 155.76 × 10 − 6
H 1000
18
O δ 18O
= + 1 * 2005.2 × 10 − 6
16
O 1000
8. Make a graph of “Actual D/H” versus “Measured D/H” for the standards and fit it to a
line. The equation for this line is the relationship between the D/H measured by the
instrument and the actual D/H.
9. Use this relationship to calculate the “Determined D/H” for all of the samples. This
determined D/H can be readily converted to δD (‰) for both the standards and samples:
D
H
δD = − 1 * 1000
155.76 × 10 −6
10. Make a graph of “Actual 18O/16O” versus “Measured 18O/16O” for the standards and fit it
to a line. The equation for this line is the relationship between the 18O/16O measured by
the instrument and the actual 18O/16O.
11. Use this relationship to calculate the “Determined 18O/16O” for all of the samples. This
determined 18O/16O can be readily converted to δ18O (‰) for both the standards and
samples:
18O
16
O
δ 18O = − 1 * 1000
2005.2 × 10
−6
Note that the deviation between the Determined 18Ο/16Ο (‰) and the Actual 18Ο/16Ο (‰)
for the standards is ± 0.16 ‰. This value should be < ± 0.25 ‰ for the known
standards.
File Transfer
As noted above in the data analysis section, the instrument saves the measured results into files
named “h2o_(date)_(file #).txt”, “h2o_(date)_(file #).lgr.txt”, and “h2o_(date)_(file
#).txt.spectrum.bz2”. The user may transfer these data files from the instrument hard disk to a
USB memory device by undertaking the file transfer process described below.
1. Upon instrument startup, the Run Configuration screen should be displayed. Select the “File
Transfer” button to initiate the file transfer process. The instrument will prompt the user to
insert a USB Memory Device.
2. Insert the USB memory device into the back of the instrument and depress “OK”. The
instrument will warn the user to keep the USB device in the instrument until appropriately
prompted. Depress “OK” to enter the file transfer screen.
3. The user will see two file directory windows. The directory windows default to the local
drive on the left screen and the USB memory device on the right. The directory windows can
be changed by clicking the “Local Drive” or “USB Key” radio buttons.
4. The user may use the left mouse button to highlight one or multiple files in the windows and
the arrow buttons to copy the files between the directories. The user may also navigate
through folders, create directories, and delete files and directories. Files may be managed
within the local drive by selecting the “Local Drive” radio button above both directory
windows. Files can then be organized into directories by creating a folder, copying the
desired files to that folder, then deleting the original files. In the example shown here,
“h2o_20061204_000.txt” and “h2o_20061204_000.lgr.txt” have been copied from the
instrument hard drive to the USB memory device.
5. Once the files have copied, select “Exit” to complete the file transfer process. Note that, if
many files are being copied, the instrument may take several seconds to finish the transfer.
Once complete, the instrument will prompt the user to remove the USB memory device.
Depress “OK” and remove the USB device.
6. Note that, if there is a problem loading the USB device, or the device is not inserted, the
instrument will display an error message and allow the user to retry the file transfer process.
Changing Septa
NOTE: Septa should be changed every 200 – 400 injections.
1. Upon instrument startup, the Run Configuration screen should be displayed. Select
“SETUP” to enter SETUP MODE.
3. Select the “INITIATE” button. The instrument will start venting and take 180 seconds to
come to pressure. Once the cavity has vented, the “READY FOR NEW SEPTUM” line will
flash:
4. Unscrew the septum nut. Note that, since the septum holder is heated to ~ 70 °C, appropriate
care should be taken in handling the septum hardware. Remove the septum from the septum
nut using the provided septum puller.
5. Slide the septum nut and new septum onto a blunt 22-gauge needle (e.g. Hamilton AS tip
style or similar) with the Teflon-coated side of the septum facing away from the septum
nut.
Teflon-coated
Side
6. Place the whole assembly onto the autoinjector septum block and hand-tighten the septum
nut firmly.
7. Manually actuate the blunt 2-gauge needle a few times to confirm that the septum is
adequately pre-drilled.
8. Once the septum change procedure is complete, select the “SEPTUM CHANGED” button.
The cell will then be evacuated for 120 seconds prior to the display of “SEPTUM CHANGE
COMPLETE”. Hit OK to exit back to SETUP MODE and then RETURN to exit back to the
Run Configuration screen.
NOTE: Do not adjust the laser offset, unless the central peak has drifted by more
than ½ division (0.25 GHz).
1. Assess if the laser offset needs to be changed. If the large, central peak shown in the
“SPECTRUM” mode is centered in the grey box, there is no need to adjust the laser
offset. Over several days, the spectrum will drift to the right. If the central peak has
drifted by more than ½ division (0.25 GHz), the laser offset needs to be adjusted. For
example, in the screenshot shown below, the central peak has drifted to the right by 1
division (0.50 GHz).
2. In order to adjust the laser offset, enter “SETUP” mode and select the “Laser Offset”
button to enter the Laser Offset Adjustment Screen.
3. Depress the “>” softkey to move the central peak left. Since the peak has drifted by 1
division (0.50 GHz) to the right, the softkey must be depressed twice to shift the peaks by
0.50 GHz to the left. Note that the depicted number (“857”) is not relevant.
4. Once the wavelength has been adjusted, exit back to the run configuration screen. Upon
injection of the next sample, the “SPECTRUM” mode should show a central peak that is
well-centered in the grey box.
1. Shut down the instrument by depressing the “Exit” button. Shutdown will take 3 minutes
and assures that the instrument is no longer at vacuum. Turn off the instrument power.
2. Remove the transfer line and filter assembly from the instrument by using a 9/16” wrench to
disconnect the ¼” Swagelok connection at the instrument back panel. Do NOT unscrew the
smaller Swagelok connection between the filter assembly and transfer line.
3. IMMEDEATELY cap the instrument using the provided ¼” Swagelok Cap and fingertighten
firmly. This step is critical in preventing dust from entering the instrument.
4. Unscrew the septum nut. Note that, since the septum holder is heated to ~ 70 °C, appropriate
care should be taken in handling the septum hardware. Remove the septum from the septum
nut using the provided septum puller.
5. Using a clean, dry air canister, puff a single pulse of air through the filter assembly and
transfer line.
6. This will remove the black septum support. Carefully place the septum support aside.
7. Once the support has been removed, repeatedly pulse dry air through the filter assembly and
transfer line to remove all visible septa pieces.
8. Using the dry air canister, blow septa pieces from the black carbon support and replace it into
the heated injector block.
9. Using the dry air canister, blow septa pieces from the septum nut.
11. Remove the ¼” Swagelok cap from the instrument back panel and IMMEDEATELY replace
the filter assembly and transfer line onto the instrument back panel.
12. Finger tighten the ¼” Swagelok nut firmly and then use a 9/16” wrench to further tighten by
¼ - ½ turn.
13. Confirm that the filter assembly and transfer line are securely attached to the back of the
analyzer. Confirm that a new septum has been placed into the injection block.
2. Adjust the Current Time, Date, and Time Zone and depress the “APPLY” button. Press
the “RETURN” button to return to the run configuration screen.
Note that these advanced settings have been optimized prior to the instrument’s delivery
and should only be adjusted by skilled users.
1. Upon instrument startup, the Run Configuration screen should be displayed. Depress the
“SETUP” button to enter SETUP MODE. Depress “Advanced Inj” to adjust the injection
settings.
Sample Volume: The injected volume (in nL) for sample vials.
Standard Volume: The injected volume (in nL) for reference standards.
Fill Speed: The rate (in nL/s) at which the syringe is actuated during filling.
Fill Strokes: The number of strokes used to help minimize air in the syringe.
Injection Speed: The rate (in nL/s) at which liquid is injected into the instrument.
Pre Injection Delay: The delay (in ms) prior to injecting the sample.
Post Injection Delay: The delay (in ms) during which the syringe is held in the sample
port. This period assures that the liquid sample is completely
transferred into the instrument.
Post Withdrawal Delay: The delay (in ms) after the syringe is withdrawn and before the
measurements begin. This short delay assures that the system has
adjusted to the rapid syringe removal.
Once the values have been appropriately adjusted, depress “OK” to exit back to the setup menu.
2. Depress “Adv Setup” to adjust the flush cycle and other miscellaneous settings.
Once the values have been appropriately adjusted, depress “OK” to exit back to the setup menu.
5. You may be able to access the shared analyzer data directory from computers running
operating systems other than Windows™. The analyzer uses a Samba server to share the
data directory, and it may be accessed by any appropriate Samba client application.