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Appendix C
5/20/2009
12
11
PROCEDURE
11.1
How to run the Shimadzu 5000
11.1.1
Turn on the gas.
11.1.2
Turn on instrument. The power switch is located on the
right side of the instrument.
11.1.3
Instrument checks when turning on: Check level of liquid
in the humidifier, located in the lower right corner inside.
The level should be between the two lines. If low—add
DHOH. Unscrew cap on the side and squirt in up to upper
line.
11.1.4
Turn on ASI. Press F5 to initialize the ASI. Make sure the
turntable is in place to avoid error messages. If the ASI is
turned on after opening the MAIN MENU, the instrument
will automatically initialize the ASI. Samples may be
loaded onto the carousel while the TOC-5000 is warming
up. Just make sure the turntable is in place before turning
on the ASI.
11.1.5
Use the F keys to navigate. Go to NEXT (F1) which opens
the MAIN MENU. Press 3 and Enter for General
Conditions.
11.1.6
Using arrow keys, scroll down to TOC furnace. Press 1
and Enter to turn on furnace. Return to MAIN MENU
(F2). Make sure liquid in the TIC chamber —plastic
reservoir inside in upper center— is bubbling. If not, there
is a leak.
11.1.7
Press 6 and Enter to get to MONITOR SCREEN. This
screen allows you to monitor instrument conditions. It
takes 20-30 minutes to come to temperature.
11.1.8
Loading Samples: Decide on standard curve.
11.1.8.1
NPOC conditioning curve: Place a std vial
of DHOH is position S1. (This vial may also be
used as the zero std of the calibration curve.)
Load at least 3 sample vials of DHOH in
positions 1-3. 100
µ
l injection, range 1, 9 max
10 injections, 3 minute sparge.
11.1.8.2
NPOC: I use 2 curves: Low — 0-10 ppm -
--- DHOH, 2.0, 5.0, 10.0 as calibration
standards, and adding 0.5, 1.0, and 7.5 as well
for stds as samples. 60 µL injection, range 1,
6 min sparge.
High----- 0-20 ppm ----- DHOH, 5.0, 10.0, 20.0
as calibrating stds and adding 1.0, 2.0, & 15.0 as
stds as samples. 30 µL injection, range 1, 6