The ESCSIS Instruments page...how to keep them running
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1. The MAT 253

1. 1. The GCC on the 253

1. 1. 1. Compound Specific dD

1. 1. 1. 1. Daily Tasks

1. 2. The Trace GC on the 253

1. 3. The H-device on the 253

2. The Delta XP

2. 1. The TC/EA and Conflo III on the Delta XP

2. 2. The Gasbench on the Delta XP

3. The Delta Advantage

3. 1. The Costech ECS (elemental analyzer) on the Delta Advantage

4. The Finnigan MAT 251

1. Make sure the furnace is at 1400°C (it is underneath the GC) and MS source is on (make sure all the green lights are on, below source on MS).

2. Check Gases in Back Flush Mode: in mass spec

In Isodat-NT Instrument Control:
Make sure you are in CO2 mode (bottom left, second pull down menu)
Set X-axis to “Magnetic Field” (top middle, second pull down, Icon: red arrow pointing to axis)
Make sure you are in Back Flush Mode with Open Split (should be set up already by last run, but to make sure check in the GC Interface graphic that the He and Back flush “knobs” are blue (ie on) and Open Split “bar” is out and off)

Run Scan:
Press green arrow (upper middle Panel)
Double (left) click on cup 2 (or right click and select “exclusive” to see only cup 2 voltage

Acceptable gas levels:
N2: 100 to 500 mV
H20: up to 1000 mV
Ar: 60 mV is standard operating conditions, but instrument can be run with Ar up to 100mV

Print Sheet
Use “print” icon near top middle panel (not under “print” at the top)
Be sure to date, indicate user, and scan conditions

3. Check Gases in Straight Mode: i.e. coming through GC and GCC

Instrument Control:
Same as above except that you want to be in “Straight Mode”
In GC Interface graphic turn He and Backflush “knobs” off and close Open Split “bar”)
Wait ~3 minutes to equilibrate system

Run Scan:
Press green arrow (upper middle Panel)
Double (left) click on cup 2 (or right click and select “exclusive”) to see only cup 2 voltage

Acceptable gas levels:
N2: up to 10-15V (mostly CO)
H20: up to 1000 mV
Ar: up to 100mV

Print Sheet
Use “print” icon near top middle panel (not under “print” at the top)
Be sure to date, indicate user, and scan conditions

4. Determine H3+ Factor

In Isodat-NT Acquisition
Select HD mode (it was in CO2 mode to check gases)
Turn Reference gas DOWN on GCC interface. The upper most knob controls the reference gas flow. Usually, the knob needs to be turned COUNTERCLOCKWISE 10+ full times to reach 1500 mV.
While the gas is falling, switch from “Trace GC?” mode (in lowest, furthest right pull-down menu) to “Std_GC.”

Turn reference gas on in GC Interface letting Mass 2 equilibrate at 1500 mV. Knob may need to be adjusted to increase or decrease reference gas level.

Open H3+ Factor Sequence
Select H3_GCC.seq.
Go to File Browser, open Sequence tab; select “Pagani” folder; “H3 Factor” folder; “H3_GCC.seq"

Turn reference gas off and let system equilibrate (~15 seconds)

Select line 1; select “Start”; erase “acquisition”; select “OK”

H3+ Factor Run controls when the reference gas is introduce to the MS, but you have to control the gas level using the Reference knob. H3+ Factor Run has an initial triplicate at 1500 mV followed by 8 doublets at higher voltages.
Increase gas pressure after initial 3 gas pulses (~240° clockwise turn), then after every 2 pulses (360° clockwise turn)

When run is complete:

Select H3+ icon (top left)
Select “DETERMINE” on popup screen
Look at H3+ factor; is it similar to the previous day? What is the SD?
If H3+ factor looks good, Select “OK” and “Save Changes”

5. Standard Run

Select Trace GC? mode (lower left panel)
Open dD Standard Sequence
Select dD Standard.seq.
Go to File Browser, open Sequence tab; select “Pagani” folder; “Standards” folder; “dD Standards”

Peak center should be selected only for first standard run
Select first run; Select Start: select “OK”

Use Standard 4 and Mix A (0.8 ul Mix A and 0.3 ul Std 4)
Pull up Mix A first so not to contaminate it with Std 4.

After run (1 hour, 20 minutes), determine if Std run is good and instrument is ready to run.
Open “Shortcut to Shared Docs?” on desktop: Select Pagani/nikolai/May 2006?
Open “Shortcut to Stuff” on desktop; Select “Data” and select file (presently in pagani/Nikolai/DH standards/May 2006?.

Drag file from Stuff to Shared Docs?

NOW, on data processing computer
Open Isodat Workspace (Isodat NT/Workspace)
Select Results tab
Right click “select path” select “OK”
Select Pagani/nikolai/May 2006?
Open file
Tag peaks to Androstane (isotope value -256.4‰ @ 1790 sec)
Re-evaluate
Input data into spreadsheet
Right click on peak data file
Select “WK1 export”
Name file and put on desktop
Open file on desktop, select “OK”
Select column 3/2 data; copy data
Open file Mix A?_Std 4?.excel, if not open already, it is on the desktop.
Right click, Paste special “transpose” below last raw data (column D)
Copy columns A, B, and C and paste below, then copy calculations from file above.
Run is good if the values are within ±5‰ or so of expected value.
Run samples….