TOC-5000 With PC Control



TOC-V w/TN

Operating Procedures for Normal Sensitivity TC, VOC, NPOC, IC, and TN Analysis

(Rev.F; 30Nov06)

Background & Nomenclature

Total Carbon/Nitrogen consist of several components. The TOC-V is capable of measuring only the soluble (non-particulate) components. These can be categorized as follows:

TC: Total (dissolved) Carbon. Includes VOC, NPOC, & IC. Samples are collected in a sealed vial with no headspace and are injected directly onto the combustion tube without exposure to air. All carbon is converted to CO2 and measured via NDIR detection. Samples are NOT acidified.

VOC: Volatile Organic Carbon. The portion of carbon that can be purged from the sample by exposure to air and/or bubbling carrier gas through the non-acidified sample. Can be measured using IC mode without acid addition. Samples are collected as for TC.

NPOC: Non-Purgable Organic Carbon. The portion of carbon remaining in solution AFTER the sample is acidified with 2 N HCl to pH 300 psi

Breathable air cylinder pressure (used for TN only): > 500 psi

Carrier gas tank regulator pressure: 80-100 psi

Instrument carrier gas flow: 100 mL/min

Instrument carrier gas pressure: 4-5 kg/cm2

Furnace temp: 720°C

Dehumidifier temp: 1(C

TN Detector Temp: 50°C

Analysis Procedures

1. Turn on carrier gas (and breathable air if running TN) at tank and check pressures (see above).

2. Check liquid levels in moisturizer, dehumidifier trap, carboys, and 2N HCl if running IC. Adjust as necessary.

3. Turn on power to instrument.

4. Open “TOC-Control V” program from Windows desktop.

5. Open “Sample Table Editor”.

6. For C only analysis - Right-click on “TOCV-csn” icon in left window and select “connect”.

For TN only or C and TN analysis - Right-click on “TOCandTN” icon in left window and select “connect”.

7. Confirm “Furnace Temp (Deg C)” is set to 720. If OK Click “Use Settings On PC”. If adjustments must be made:

A). Click “Edit Settings On PC”

B). Click “TOC” tab

C). Select 720 in lower right of window, then “OK”

D). Click “Use Settings On PC”

8. Confirm the correct rack is selected: Intrument ( Properties ( ASI Tab. Set Tray Type to either 24mL or 40 mL rack.

9. Open the template sample table you wish to use or build a new table.

10. IMMEDIATELY click “File( Save As” then save with time-stamped file name.

11. On top menu under “Instrument” click “Connect” and then “Background Monitor”. TC Furnace and dehumidifier should be at 720 and 1 deg C respectfully and TN Detector at 50 deg C for at least 30 min before analysis. Confirm baseline conditions are OK before proceeding.

12. Modify sample table according to your sample set. Cut rows as necessary but make sure samples remain bracketed by blank and QC.

NOTE: If SALT (KCL, K2SO4, etc) samples are being analyzed, be sure to add a nanopure water sample using “cleaning” method to end of run. Only 60 salt samples may be run before changing the ceramic wool atop the catalyst bed.

13. Place samples, calibration standard(s), and QC(‘s) in rack positions according to sample table “Vial” column. To change positions, click “View( ASI/8port sampler vials”

14. For NPOC and IC, check Sparge to confirm tube is not blocked:

Instrument ( Mechanical Check ( Sparge ( Sparge Gas Open

Clear sparge line if blocked.

15. To start run click “Instrument( Start”. Select Standby option according to instrument use schedule then click “Standby”. If ceramic wool must be changed between consecutive runs, select the “Shutdown” option.

16. Verify vial positions then click “OK”.

17. De-Select “External Acid Addition” then click “Start”

18. To monitor progress, right-click sample name in left window then select “Sample Window”. If hidden, click “Window( Sample Window” from top menu.

Shutdown

1. Shut off carrier gas and breathable air tank valves

2. Complete database log

3. Clean all glassware

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