The BioTector B3500ul TOC analyzer Process Tests November, 2017 Company Confidential

This presentation should be viewed with the following document available: Manual appropriate to the BioTector B3500ul.

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.

Pressure Test Purpose: Frequency of activation: Operation: Note: To detect a leak or partial leak in the BioTector. Frequency of activation: Once per day, and when the BioTector B3500ul is started. 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. Note: 1: In addition to the Pressure Test detailed above which operates once per day and each time the BioTector B3500ul is started, a Pressure Check is carried out as part of the Reactor Purge sequence. The Pressure Check only has pass /fail settings, it cannot generate any warning of a small leak in the BioTector B3500ul. 2: Pressure Tests are carried out at 400mbar, while the BioTector B3500ul runs typically at 4mbar, making the Pressure Tests a sensitive leak detection system.

Typical Pressure Test Menu.   T 9 : 1 7 2 8 - <  * I Z A C O M 6 s F N 4 . l / h L W 3 G B H Two test modes are available: Pressure Test: This simulates the pressure test in the same time as the BioTector allows (60s). Pressurize Reactor: This simulate the pressure test with long time limit, useful for detecting a leak.

Mixer Reactor leaking through diaphragm? PRESSURE TEST. CO2 ANALYZER ACID PUMP P3 DESTRUCTOR OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 O2 Pressure correct? MFC reading correctly? Air Pressure correct? Pump leaking? Leak in component? Fitting leaking? Valve Mixer Reactor leaking through diaphragm? STREAM / MANUAL VALVES STREAM 1 MANUAL STREAM 2 As part of every Reactor Purge sequence, a Pressure Check is carried out, which detects a major leak in the analysis system. In addition, every time the BioTector B3500ul is started up and once per day thereafter, a separate Pressure Test is carried out. The Pressure Test has the facility to give an early warning of a small leak, and also can stop the BioTector B3500ul should major leak be detected.

PRESSURE TEST. CO2 ANALYZER ACID PUMP P3 DESTRUCTOR OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 3. Is the MFC reading correctly? 1. Is the air pressure correct? 2. Is the O2 pressure correct? 5. Disconnect tube over cooler. Seal tube. Test. 4. Disconnect tube at TEE. 6. Seal exhaust valve. STREAM / MANUAL VALVES STREAM 1 MANUAL STREAM 2 Always follow a structured approach when looking for a leak. CAUTION: Traces of chemicals may be in tubes when they are opened.

Flow Test Purpose: Frequency of activation: Operation: Note: To detect a blockage or partial blockage in a gas flow path BioTector. Frequency of activation: Once per day, and when the BioTector B3500ul is started. Operation: The microcontroller activates the MFC with a gas flow of 60 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 45 LPH, the flow test passes. If the gas flow drops below 45 LPH but remains above 30LPH within the 30 second flow test time, a flow warning is logged. If the gas flow drops below 30LPH, a flow fault is logged and the BioTector stops. Note: In addition to the Flow Test detailed above which operates once per day and each time the BioTector B3500ul is started, the gas flow is continuously monitored as the analyzer runs. If the flow falls below 50% of its set-point for >12 seconds, a fault is generated and the BioTector B3500ul stops.

Typical Flow Test Menu. Two modes available for each valve:   T E S 9 : 1 7 2 8 - <  * X H A U 3 M P 4 I s C N 6 . l / h 5 G R B 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.

Tube or fitting blocked? Tube blocked outside BioTector? FLOW TEST: EXHAUST. CO2 ANALYZER ACID PUMP P3 DESTRUCTO R OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 MFC reading correctly? Air pressure correct? O2 pressure correct? Reactor blocked? Tube or fitting blocked? Valve blocked? Tube blocked outside BioTector? STREAM / MANUAL VALVES STREAM 1 MANUAL STREAM 2 The gas flow is continuously monitored as the analyzer runs. If the flow falls below 50% of its set-point for >12 seconds, a fault is generated and the BioTector System-C stops. In addition, every time the BioTector System-C is started up and once per day thereafter, a separate Flow Test is carried out. This test has the additional facility to give an early warning of a small leak.

FLOW TEST: EXHAUST. CO2 ANALYZER ACID PUMP P3 DESTRUCTO R OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 3. Is the MFC reading correctly? 1. Is the air pressure correct? 2. Is the O2 pressure correct? 5. Disconnect tube over cooler. Test. 4. Disconnect tube at TEE. 6. Disconnect tube before ozone destructor. 7. Disconnect tube after ozone destructor. 8. Disconnect tube outside BioTector. STREAM / MANUAL VALVES STREAM 1 MANUAL STREAM 2 Always follow a structured approach when looking for a blockage in a tube. CAUTION: Traces of chemicals may be in tubes when they are opened.

Tube or fitting blocked? Tube blocked outside BioTector? FLOW TEST: SAMPLE OUT. CO2 ANALYZER ACID PUMP P3 DESTRUCTOR OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 MFC reading correctly? Air pressure correct? O2 pressure correct? Tube or fitting blocked? Valve blocked? Tube blocked outside BioTector? STREAM / MANUAL VALVES STREAM 1 MANUAL STREAM 2 The gas flow is continuously monitored as the analyzer runs. If the flow falls below 50% of its set-point for >12 seconds, a fault is generated and the BioTector System-C stops. In addition, every time the BioTector System-C is started up and once per day thereafter, a separate Flow Test is carried out. This test has the additional facility to give an early warning of a small leak.

FLOW TEST: SAMPLE OUT. CO2 ANALYZER ACID PUMP P3 DESTRUCTO R OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 3. Is the MFC reading correctly? 1. Is the air pressure correct? 2. Is the O2 pressure correct? 4. Disconnect tube at TEE. Test. 5. Disconnect tube after valve. Test. 6. Disconnect tube after valve. Test. STREAM / MANUAL VALVES 7. Disconnect tube outside BioTector. Test. STREAM 1 MANUAL STREAM 2 Always follow a structured approach when looking for a blockage in a tube. 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 T020 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 T020. 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 T020, 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 18s (or programmed level), the status of the ozone test is Pass. If the o-ring breaks in a time between 18 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.

OZONE GENERATOR TEST: General view. The ozone generator assembly, as installed in the BioTector B3500ul. Note the hole for adjusting the current (blue circle). The ozone generator assembly, inside view below.

OZONE GENERATOR TEST: Physical items to check. OXYGEN MODULE MFC Is the oxygen purity >95% oxygen, and free of water and oil? If an oxygen analyzer is not available, a comparison can be made with oxygen from a cylinder. Additionally, the level of CO2 in the oxygen can be checked. AIR Is there liquid In ozone Generator tube? Is the coil resistance ok? Low voltage side, 2.5 – 3 ohms. Low to High voltage side, 7-14 kohms. If in doubt, replace it. Are the connections tight on the coil? OZONE GENERATOR Are the connections tight on thermostat? Are the connections tight on the PCB? CAUTION: Ensure that any traces of ozone are purged through the ozone destructor before opening any tubes or fittings.

OZONE GENERATOR TEST: Electrical items to check. Current setting ok? Connections tight in terminals? Ozone PCB back view Ozone PCB front view Connections tight in terminals? Current and voltage (24V DC) ok when generator running? The current is measured by the microcontroller. Lockout relay activated? Check L49 Fuse ok? S I M U L A T E   9 : 1 7 2 8 - F C = . l / h O 3 5 p m <  * Z N G R , V 4 D P B 6 X H ▼ Upper section of the motherboard, showing ozone generator terminals.

Sample Pump Test Purpose: Operation: 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 out through the sample bypass port, and on for 1 additional meter, to ensure a fresh sample is injected. The sample should always be as near to the BioTector B3500ul as possible, and always be at atmospheric pressure. When running in reverse, the sample 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. The settings can be changed by following the link to the Sample Pump screen to determine the correct time. Different times are programmable for each stream or manual sample.

SAMPLE PUMP TEST: Forward. CO2 ANALYZER ACID PUMP P3 DESTRUCTO R OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 The sample should be pumped out the bypass port and run for an additional 10 seconds. STREAM 1 MANUAL STREAM 2 STREAM / MANUAL VALVES Run the SAMPLE PUMP forward (FWD) and measure the time (in seconds) required for a fresh sample to fill and flow out through the bypass port. Add 10 seconds to the measured time and enter this value as the FORWARD time in the Sample Pump menu. The sample pump REVERSE time will be automatically set as 10 seconds greater than the FORWARD time.

SAMPLE PUMP TEST: Reverse. CO2 ANALYZER ACID PUMP P3 DESTRUCTO R OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 The sample should be pumped back to the sample point and the sample line left empty. STREAM / MANUAL VALVES STREAM 1 MANUAL STREAM 2 When running in reverse, the sample should be pumped completely back to the sample point, and the sample line left empty.

pH Test Purpose: Operation: To check the pH in the reactor at different stages in the reaction. Operation: The pH in the reactor is checked using the sample from the sample stream. The TIC acid reagent and sample are first injected into the reactor and mixed together, then the process stops allowing the pH to be checked. The process is repeated for the Base reagent and the TOC acid reagent.

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.

pH TEST: Example TIC pH test. CO2 ANALYZER ACID PUMP P3 DESTRUCTOR OZONE COOLER OZONE GENERATOR REACTOR MIXER P2 BASE ACID SAMPLE BYPASS EXHAUST MFC OXYGEN MODULE AIR BASE PUMP P4 SAMPLE PUMP P1 SAMPLE VALVE MV4 VALVE MV1 MV3 pH paper With the reactor mixer stops, the liquid accumulates at the bottom of the reactor. Open the fitting at the TEE. Lower the tube until a few drops of liquid drip out, just enough to wet the pH paper. STREAM / MANUAL VALVES STREAM 1 MANUAL STREAM 2 Example of testing the pH in the TIC phase. The TIC acid reagent and sample are first injected into the reactor, and mixed with the reactor mixer. 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.

pH TEST: Common issues encountered. OXYGEN MODULE MFC CO2 ANALYZER AIR Acid, Base pump: pumped volume correct? ACID PUMP P3 Are the programmed settings for sample, acid and base correct? ACID COOLER OZONE GENERATOR Acid, Base reagents: Is the normality correct? DESTRUCTOR OZONE BASE PUMP P4 BASE Is the pH in the sample very high ~>11pH or very low ~<3pH? SAMPLE PUMP P1 EXHAUST VALVE MV1 STREAM / MANUAL VALVES REACTOR MIXER P2 STREAM 1 STREAM 2 Reactor mixer running? MANUAL REACTOR VALVE MV3 SAMPLE BYPASS SAMPLE VALVE MV4 EXHAUST Examples of where pH issues could occur.