TIC – Total Inorganic Carbon

Using Shimadzu TOC-V with PC control

(Rev. B; 19Apr04)


TIC Standards

Use designated volumetric flasks found in the cold room

Stock TIC Standard (2000ppm): 1.75g Sodium Bicarbonate + 2.205g dried Sodium Carbonate

Q.S. to 250 mL total volume with Nanopure water

Use 2000 ppm IC Na Carbonate/Bicarbonate standard found in the cold room and nanopure water to prepare working standards below

Concentration (ppm) / Stock IC (2000ppm) / Total vol. w/ nanopure
10.00 / 250 L / 50 ml
20.00 / 500 L / 50 ml
50.00 / 1250 L / 50 ml
100.00 / 1250 L / 25 ml
50 ppm QC / 2.5 mL ERA Custom Std / 50 mL

IC Reagent: 44ml 85% Phosphoric Acid + 106 ml Nanopure water

General Instrument Conditions

Carrier gas cylinder pressure: 300 psi

Carrier gas tank regulator pressure: 80-100 psi

Instrument carrier gas flow: 150 mL/min

Instrument carrier gas pressure: 4-5 kg/cm2

Dehumidifier temp: 1C

Instrument Start-Up

  1. Open GEL Database and initiate Run Log. Complete required fields and click the command button to open the TOC Control program.
  2. Turn on carrier gas at tank and check pressures (see above).
  3. Check level of NaOH in humidifier vessel. Adjust to between lines with nanopure water if necessary.
  4. Check level of 25% Phosphoric Acid in IC reagent vessel. Refill if < ½ full
  5. Attach plastic tubing connected to needle where the sample line (clear) from the autosampler connects above the syringe. Be careful not to cross tread the soft plastic.

6. Normally, the instrument should remain on with the furnace hot. If it is not, or if communications between the instrument and computer have been lost, follow the instructions below.

To establish communications:

a) Make sure computer, instrument, and autosampler are on.

b) Open TOC Control program (double-click icon).

c) Enter your name at prompt.

d) Choose ‘Connect’ under ‘Measure’ menu.

7. Once communications have been established:

a) Check carrier gas flow rate (150 ml/min).

b)Check for leaks by pinching off tubes to and from soda-lime scrubber while watching for

backflow into the dehumidifier waste vessel.

c) Under ‘Options” select ‘Instrument Conditions’

-Click on ASI and turn ASI off

-Make sure autoregeneration of IC solution is turned on

-TC furnace may remain on

d) Regenerate IC solution

-Under ‘Options’ choose ‘Maintenance’

-Click on regeneration of IC solution; work silicone drain tubing (from side of IC Rxn Vessel)a bit to open any flat spots due to pinch valve

-Watch to see if IC solution empties and refills.

e) Wash sample line by placing needle in a beaker of nanopure water

Under ‘Options’ choose ‘Maintenance,’ select ‘Washing’

Click on IC. Wash at least 3 times (2 washes/each)

-Tap air bubbles out of sampling syringe if necessary

8. To monitor and adjust baseline:

a) ‘View’  ‘Background Monitor’

b) Confirm all parameters are ‘OK’.

c) Choose range at which analysis will be performed (30 for above range of standards)

d) Confirm baseline stability.

e) For range 1 adjust baseline to  -90%, For ranges 5 and 30, adjust to 0.

Creating A Sample Table

  1. Create a new calibration curve file:

a) ‘View’  ‘Cal Curve File List’

b) Open appropriate template to be used for run (example, 'iclterb.cal').

c)Enter title of run and change file name to run date.

d)Save as new file using date as file name; ‘Cancel’ to return to Sample Table. DO NOT save over template file!!

  1. If necessary, open new Sample Table; ‘File’  ‘New’, respond ‘No’ to “Overwrite current instrument conditions…?” prompt.
  2. Insert new calibration file into Sample Table:

a) ‘Edit’  ‘Insert Standard’

b) Choose file just created; ‘OK’

  1. Insert QC’s:

a)Put cursor on line to which QC’s will be inserted.

b)‘Edit’  ‘Insert Sample’

c)Choose “icqc.met”; ‘OK’

d)Repeat a-c once

  1. Insert samples:

a)‘Edit’  ‘Autogenerate’

b)Click ‘Edit Method’

c)Choose “ltertic.met” (or other appropriate file); ‘OK’

d)Type project name and date under ‘Sample Name’

e)Under ‘Sample ID’ select ‘Index counter start from’ and type “1” in box

f)Enter number of samples in appropriate box


  1. Insert 2 more QC’s as above.
  2. Insert Blank:

a)Put cursor on line to which blanks will be inserted.

b)‘Edit’  ‘Insert Sample’

c)Choose “icblank.met”; ‘OK’

d)Repeat a-c once

  1. Enter QC ID’s on Sample Table.
  2. Enter cal curve file name for samples, and QC’s (and standards if incorrect):

a)Highlight empty boxes in ‘Cal Curve’ column.

b)‘Edit’  ‘Replace’

c)Type in new cal curve file name.

d)Press “Esc” key at error message to enter new file name.

  1. If fewer than 3 injections are required, modify the number for each sample on sample table
  2. Save Sample Table as date.”toc”
  3. Record file name on log form.

Starting a Run

1. Under ‘View’ select ‘Background Monitor’

2. Check the baseline at range 30 (should be near 0), and adjust if necessary

3. When ready to start, close background monitor

4. Click on ‘Start’

5. Click OK for ‘normal’ measurement mode

6. When prompted if ready to sample:

a) Insert vent needle (with 3-way stop cock) into sample vial with valve closed

b) Insert sample needle into sample vial

c) Open valve to vent sample and click ‘OK’

7. After the TOC-5000 completes the sample injections, choose ‘Continue’

8. Repeat the Sample procedure until the run is complete

Monitoring injections

1. Under ‘View’ choose ‘Real time window’

2. To switch between the Real time window and the Sample table choose the desired

screen under ‘Window’ (Or tile to view both simultaneously)

To monitor the current injection any box along the row of the sample being

analyzed must be highlighted in the sample table when switching to the

Real time window

Printing a Report

To print a concise report in the form of the Sample Table, choose 'File'  'Print Table' ‘Print’

To print calibration curve(s)

-Under ‘File’ choose ‘Page Setup’

-Select/deselect appropriate boxes under the ‘Cal Curves’ tab. Clear all under the other tabs.

-Enter Title on ‘Page Setup’ tab.

-Click OK

-Click ‘File’ then ‘Print’ then ‘OK’


  1. Wash flowline as before ("Instrument Startup", 7e) .
  2. Disconnect manual sampling needle and reconnect autosampler sample line.

3 Complete Run Log.

4. Complete Billing Log

5. Shut off carrier gas cylinder valve; Do not turn off regulator valve!