BioTector COD TOC TN analyzer Process Tests

This presentation should be viewed with the following document available: Manual appropriate to the BioTector.

Safety: Wear appropriate PPE! The BioTector runs on mains electricity, 115V or 230V. Some components may be hot. The BioTector uses acidic and basic reagents. Electrostatic devices may be present on some PCB’s. Always wear a grounding strap.

Oxidation Phase Process Tests

Pressure Test Purpose: to detect a leak in the BioTector. Operation: The microcontroller activates the MFC with a gas flow of 40 LPH. If there is no leak in the BioTector, the gas flow will drop eventually to 0 LPH. If the gas flow drops below 4 LPH within 60 seconds, the pressure test passes. If the gas flow is above 4LPH but below 6LPH, a pressure test warning is logged. If the gas flow remains above 6LPH at the end of the pressure test, then the pressure test fails, a fault is logged and the BioTector stops.

Typical Pressure Test Menu. Two modes available: Pressure Test: Simulate the pressure test in the same time as the BioTector allows (60s). Pressurize Reactor: Simulate the pressure test with long time limit, useful for detecting a leak.

PRESSURE TEST P2 Circulation Pump Glass beads MFC reading correctly? Pressure correct? MFC Mass Flow Controller Sample in (ARS) valve leaking, (around valve ball into the sample drain line)? MV51 Purge OXYGEN Leak in analyzer? O2 Regulator MV7 Injection EXHAUST MV1 Exhaust Circulation pump leaking? Through diaphragm in diaphragm pump? Through piston into water line in heavy duty pump? CO2 Analyzer Ozone Destructor Valve leaking? MV4 Sample In SAMPLE OUT Cooler Oxidized Fluid Catch-pot TN Module Fitting leaking? MCR Reactor Ozone Generator P2 Circulation Pump Glass beads Cleaning DRAIN Pump leaking? P4 Base Pump BASE MV6 Acid P3 Acid Pump ACID MV5 Sample Out Zero Manual Valve leaking? P1 Sample ZERO MANUAL SAMPLE IN Examples of some potential leak points in the BioTector

PRESSURE TEST: Structured fault finding 1. Pressure correct? MFC Mass Flow Controller 2. Disconnect MFC outlet tube. Seal MFC outlet. Test. MV51 Purge OXYGEN O2 Regulator MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor 5. Seal exhaust valve. Test. MV4 Sample In SAMPLE OUT Cooler Oxidized Fluid Catch-pot TN Module 4. Disconnect reactor outlet tube. Seal reactor tube. Seal sample out valve. Test. MCR Reactor Ozone Generator P2 Circulation Pump Glass beads Cleaning DRAIN P4 Base Pump BASE MV6 Acid P3 Acid Pump ACID MV5 Sample Out Zero Manual P1 Sample ZERO 3. Disconnect Ozone outlet tube. Seal ozone outlet. Test. MANUAL SAMPLE IN Always follow a structured approach when looking for a leak.

Flow Test Purpose: to detect a blockage or partial blockage in a tube in the BioTector. Operation: The microcontroller activates the MFC with a gas flow of 80 LPH. The gas flow through the exhaust and sample out valves / lines are tested independently. If there is no blockage in either of the lines, and the BioTectors flow remains above 72 LPH, the flow test passes. If the gas flow drops below 72 LPH but remains above 40LPH within the 30 second flow test time, a flow warning is logged. If the gas flow drops below 40LPH, a flow fault is logged and the BioTector stops.

Typical Flow Test Menu. Two modes available for each valve: Exhaust (or Sample Out) Test: Simulate the flow test in the same time as the BioTector allows (30s). Exhaust (or Sample Out) Flow: Simulate the flow test with long time limit, useful for detecting a blockage.

FLOW TEST: EXHAUST P2 Circulation Pump Glass beads MFC reading correctly? Pressure correct? MFC Mass Flow Controller MV51 Purge OXYGEN O2 Regulator MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor Line blocked outside BioTector? Valve blocked? MV4 Sample In SAMPLE OUT Cooler Ozone Generator Ozone destructor filter blocked? Oxidized Fluid Catch-pot TN Module MCR Reactor P2 Circulation Pump Glass beads Cleaning DRAIN Oxygen inlet to reactor blocked? Note, this enters the top of the HS reactor. P4 Base Pump BASE MV6 Acid P3 Acid Pump ACID MV5 Sample Out Zero Manual P1 Sample ZERO MANUAL SAMPLE IN Examples of some potential blockage points in the BioTector. Note that the Exhaust valve and Purge/Sample out valve lines are tested independently.

FLOW TEST: SAMPLE OUT P2 Circulation Pump Glass beads MFC reading correctly? Pressure correct? MFC Mass Flow Controller MV51 Purge OXYGEN Valve blocked? O2 Regulator MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor Line blocked outside BioTector? MV4 Sample In SAMPLE OUT Cooler Ozone Generator Oxidized Fluid Catch-pot TN Module MCR Reactor P2 Circulation Pump Glass beads Cleaning DRAIN Valve blocked? P4 Base Pump BASE MV6 Acid P3 Acid Pump ACID MV5 Sample Out Zero Manual P1 Sample ZERO MANUAL SAMPLE IN Examples of some potential blockage points in the BioTector. Note that the Exhaust valve and Purge/Sample out valve lines are tested independently.

FLOW TEST: Structured fault finding 1. Pressure correct? Pressure correct? MFC Mass Flow Controller 8. Disconnect MFC outlet tube, but only when system de-pressurized. Test. MV51 Purge OXYGEN O2 Regulator 4. Disconnect exhaust tube. Test. MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor 3. Disconnect ozone destructor outlet. Test. MV4 Sample In SAMPLE OUT Cooler Ozone Generator Oxidized Fluid Catch-pot 2. Disconnect ozone destructor inlet. Test. TN Module 6. Disconnect reactor outlet tube. Test. MCR Reactor 5. Disconnect sample out tube. Test. P2 Circulation Pump Glass beads Cleaning DRAIN P4 Base Pump BASE MV6 Acid P3 Acid Pump ACID MV5 Sample Out Zero Manual 7. Disconnect Ozone outlet tube, but only when system de-pressurized. Test. P1 Sample ZERO MANUAL SAMPLE IN Always follow a structured approach when looking for a blockage. Always allow 1 minute for each test, as oxygen gas will flow until the system is pressurized. CAUTION: Traces of chemicals may be in tubes when they are opened.

Ozone Test Purpose: to check the level of ozone generated by the BioTectors ozone generator. When the test kit has been installed in accordance with T006 and the installation confirmed by the user, the BioTector activates the ozone generator. The BioTector calculates Pass, Low Ozone or Fail against its programmed criteria. The user can also check the time required for the o-ring to break against the graph in T006. This provides an indication as to how well the ozone generator is operating. NOTE: Always use a new o-ring for each test, and do not carryout the test with an o-ring which has been fitted to the test bar for some time. This o-ring will have stretched and so give a false result.

Typical Ozone Generator Test Menu. When the ozone generator test has been installed in accordance with T006, the user activates the Start Test menu item. When the o-ring breaks, the user activates the Stop Test menu item. If the o-ring breaks within 15s (or programmed level), the status of the ozone test is Pass. If the o-ring breaks in a time between 15 and 60s, the status of the ozone test is Low Ozone. If the o-ring does not break within 60s, the status of the ozone test is Fail.

Only work on ozone generator if mains power is isolated OZONE GENERATOR TEST Warning: Only work on ozone generator if mains power is isolated MFC Mass Flow Controller Oxygen purity >95% oxygen, and free of water and oil? OXYGEN O2 Regulator If PCB is suspected as being faulty, replace it. Ozone Generator Liquid In ozone generator? Coil resistance ok? If in doubt, replace it. Connections tight on coil? Connections tight on thermostat (if fitted)? Connections tight in terminals? Fuse ok?

Sample Pump Test Purpose: to simulate the operation of the sample pump. Operation: The microcontroller turns the sample pump on in the forward or reverse direction. When running forward, the sample should be pumped through the tube as far as the cleaning cycle valve, or out the sample line drain if the line equalization feature is not used. When running in reverse, the fluid from the oxidized fluid catch pot should be pumped completely back to the sample point, and the sample line left empty. When the pump is stopped by the user, the run time is displayed on the screen.

Typical Sample Pump Test Menu. The stream valve as well as the sample pump forward and reverse times can be checked. When the correct time has been determined, the settings can be changed by following the link to the Sample Pump screen. Different times are programmable for each stream or manual sample.

The sample should be pumped out the drain. SAMPLE PUMP TEST: FORWARD MFC Mass Flow Controller MV51 Purge OXYGEN O2 Regulator MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor SAMPLE OUT MV4 Sample In Oxidized Fluid Catch-pot DRAIN Cooler Ozone Generator TN Module The sample should be pumped out the drain. MCR Reactor P2 Circulation Pump Glass beads Cleaning P4 Base Pump BASE MV6 Acid P3 Acid Pump ACID MV5 Sample Out Zero Manual P1 Sample ZERO MANUAL SAMPLE IN

SAMPLE PUMP TEST: REVERSE MFC Mass Flow Controller MV51 Purge OXYGEN O2 Regulator MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor SAMPLE OUT MV4 Sample In Oxidized Fluid Catch-pot DRAIN Cooler Ozone Generator TN Module MCR Reactor Sample and oxidized fluid should be completely pumped back to sample point. P2 Circulation Pump Glass beads Cleaning P4 Base Pump BASE MV6 Acid P3 Acid Pump ACID MV5 Sample Out Zero Manual P1 Sample ZERO MANUAL SAMPLE IN

pH Test Purpose: to check the pH in the reactor at different stages in the reaction. The BioTector takes a sample from the sample stream and injects this into the reactor. This is followed by (for example in the TIC&TOC mode) TIC acid, Base and TOC acid. The BioTector can be stopped at any time to allow the pH be checked.

Typical pH Test Menu. Any range or sample stream can be checked, and any operating mode (for example, TIC&TOC or TC). When the fluid has been mixed in the reaction, the process stops to allow the user check the pH. Only a very small sample should be removed from the reactor, so as not to effect the pH for the next test. It is important that the previous reaction finished normally to eliminate the possibility of any pH influence from the previous reaction.

EXAMPLE: TIC pH TEST, MCR REACTOR MFC Mass Flow Controller MV51 Purge OXYGEN O2 Regulator MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor MV4 Sample In SAMPLE OUT Cooler Ozone Generator Oxidized Fluid Catch-pot TN Module MCR Reactor P2 Circulation Pump Glass beads Cleaning With the circulation pump stopped, the liquid accumulates at the bottom of the reactor. DRAIN P4 Base Pump BASE MV5 Sample Out pH paper MV6 Acid P3 Acid Pump ACID Zero Manual P1 Sample ZERO MANUAL SAMPLE IN To take a sample from the MCR reactor (as shown) it is necessary to open the fitting after the sample out valve and activate the TAKE SAMPLE function in the menu, which pulses the sample out valve, and allows a few drops of fluid out.

EXAMPLE: TIC pH TEST, HS REACTOR MFC Mass Flow Controller OXYGEN O2 Regulator MV7 Injection EXHAUST MV4 Sample In MV1 Exhaust CO2 Analyzer CO2 Analyzer Ozone Destructor MV6 Acid SAMPLE OUT Cooler Ozone Generator Oxidized Fluid Catch-pot HS Reactor With the circulation pump stopped, the liquid accumulates at the bottom of the reactor. Cleaning P2 Circulation Pump DRAIN P4 Base Pump BASE P3 Acid Pump ACID Manual Stream 2 pH paper P1 Sample MANUAL pH paper MV5 Sample Out STREAM 2 STREAM 1 Option 1 is to slightly open the TEE fitting, just enough to wet the pH paper. If there is sufficient liquid in the reactor, Option 2 is to open the fitting after the sample out valve and activate the TAKE SAMPLE function in the menu, which pulses the sample out valve

pH ISSUES P2 Circulation Pump Glass beads Mass Flow Controller MFC Mass Flow Controller MV51 Purge OXYGEN O2 Regulator pH in sample very high ~>12pH or very low ~<2pH? MV7 Injection EXHAUST MV1 Exhaust CO2 Analyzer Ozone Destructor MV4 Sample In SAMPLE OUT Cooler Ozone Generator Oxidized Fluid Catch-pot Injection settings for sample, acid and base correct? TN Module MCR Reactor Acid, Base reagents: normality correct? P2 Circulation Pump Glass beads Cleaning DRAIN Acid, Base pump: pumped volume correct? Circulation pump running? P4 Base Pump BASE MV5 Sample Out MV6 Acid P3 Acid Pump ACID Zero Manual P1 Sample ZERO MANUAL SAMPLE IN

Liquid Phase Process Tests

Typical Purge Cell Test Menu. The Purge Cell Test operates as follows: The cell and oxidized fluid catch pot are emptied.

OXIDIZED FLUID CATCH POT EMPTY N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs, pumping the oxidized fluid from the catch-pot through the cell to drain.

OXIDIZED FLUID CATCH POT EMPTY GENERAL LAYOUT TN MODULE N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The OXP Sample Pump runs reverse for 2 second to empty the Oxidized Fluid Catch-pot completely. Note that as it is difficult to completely empty the cell in an upwards direction, some liquid may remain in the cell.

MEASURING CELL EMPTY N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, and any traces of liquid remaining in the cell are pumped to drain.

Typical Clean Cell Test Menu. The Clean Cell Test operates as follows: The cell and oxidized fluid catch pot are emptied. The cell is cleaned with cleaning fluid Any residue from cleaning fluid is washed out with DIW.

OXIDIZED FLUID CATCH POT EMPTY N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs, pumping the oxidized fluid from the catch-pot through the cell to drain.

OXIDIZED FLUID CATCH POT EMPTY GENERAL LAYOUT TN MODULE N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The OXP Sample Pump runs reverse for 2 second to empty the Oxidized Fluid Catch-pot completely.

MEASURING CELL EMPTY N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, and any traces of liquid remaining in the cell are pumped to drain.

MEASURING CELL CLEAN N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs, bringing cleaning fluid into the cell. This is typically carried out every 50-100 reactions, to clean the cell and guarantee that the cell and tubes will never require any physical cleaning or maintenance.

MEASURING CELL CLEAN N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, cleaning the tube to the catch-pot, and additionally puts a few drops of cleaning fluid into the catch-pot to clean the base of the catch-pot. This is later removed by the OXP sample pump.

MEASURING CELL CLEAN N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs, bringing cleaning fluid back out of the catch-pot tube.

MEASURING CELL CLEAN N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, pumping the cleaning fluid to drain.

GENERAL LAYOUT TN MODULE MEASURING CELL CLEAN GENERAL LAYOUT TN MODULE N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The OXP Sample Pump runs reverse for 2 second to empty the Oxidized Fluid Catch-pot.

MEASURING CELL WASH N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The DIW wash is carried out after every cleaning reaction. Typically there are two consecutive washing cycles after each cleaning. The N pump runs, bringing DIW into the cell.

MEASURING CELL WASH N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, washing the tube to the catch-pot, and additionally puts a few drops of DIW into the catch-pot to wash the base of the catch-pot. This is later removed by the OXP sample pump.

MEASURING CELL WASH N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs, bringing DIW back out of the catch-pot tube.

MEASURING CELL WASH N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, pumping the cleaning fluid to drain.

GENERAL LAYOUT TN MODULE MEASURING CELL WASH GENERAL LAYOUT TN MODULE N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The OXP Sample Pump runs reverse for 2 second to empty the Oxidized Fluid Catch-pot. The process is now repeated for a second wash cycle.

Typical Read DIW REF Test Menu. The Read DIW REF Test operates as follows: The cell is emptied. The cell is filled with DIW, and the readings taken.

MEASURING CELL EMPTY N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, and any traces of liquid remaining in the cell are pumped to drain.

DIW MEASURE (ZERO) The N pump runs, bringing DIW into the cell. N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs, bringing DIW into the cell.

DIW MEASURE (ZERO) N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The Flash Lamp is activated, and the cell zero is measured. The measuring frequency is 217nm, the through-cell reference is 265nm.

DIW MEASURE (ZERO) N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, pumping the DIW to drain.

Typical Read Sample Test Menu. The Read Sample Test operates as follows: The cell is emptied. The cell is filled with Sample from the oxidized fluid catch pot, and the readings taken.

MEASURING CELL EMPTY N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, and any traces of liquid remaining in the cell are pumped to drain.

MEASURING CELL FILL N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs, pumping the oxidized fluid from the catch-pot into the cell.

TN MEASURE N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The Flash Lamp is activated, and the TN in the form of NO3- is measured. The measuring frequency is 217nm, the through-cell reference is 265nm and this data is used with the cell zero readings to calculate the TN result. Typically, three separate measurements are carried out, with the N pump running for 2 seconds between each measurement.

MEASURING CELL EMPTY N Pump DRAIN DRAIN LV3 Cleaning 217nm detector CLEANING LV2 DIW DIW 265nm detector LV1 Sample in SAMPLE OUT Detector module. Oxidized Fluid Catch-pot To OXP Cleaning valve To OXP Sample out valve The N pump runs in reverse, returning the oxidized fluid from the cell to the catch-pot. The OXP sample pump then uses the oxidized fluid in its reverse cleaning process, emptying the oxidized fluid catch pot. Note: If the OXP sample pump reverse time is not set, for example if a span calibration is run, then the oxidized fluid is pumped to drain by the N pump, not into the oxidized fluid catch pot (not shown on presentation).