Bio Tector COD TOC TN analyzer Process Tests

Bio. Tector COD TOC TN analyzer Process Tests

This presentation should be viewed with the following document available: • Manual appropriate to the Bio. Tector.

Safety: Wear appropriate PPE! The Bio. Tector runs on mains electricity, 115 V or 230 V. Some components may be hot. The Bio. Tector 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 Bio. Tector. Operation: • • • The microcontroller activates the MFC with a gas flow of 40 LPH. If there is no leak in the Bio. Tector, 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 4 LPH but below 6 LPH, a pressure test warning is logged. If the gas flow remains above 6 LPH at the end of the pressure test, then the pressure test fails, a fault is logged and the Bio. Tector stops.

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

PRESSURE TEST MFC reading correctly? Pressure correct? MFC Mass Flow Controller MV 51 Purge Sample in (ARS) valve leaking, (around valve ball into the sample drain line)? OXYGEN O 2 Regulator Leak in analyzer? MV 7 Injection CO 2 Analyzer Ozone Destructor Circulation pump leaking? Through diaphragm in diaphragm pump? Through piston into water line in heavy duty pump? MV 1 Exhaust MV 4 Sample In EXHAUST Valve leaking? SAMPLE OUT Oxidized Fluid Catch-pot Cooler Fitting leaking? Glass beads P 2 Circulation Pump Ozone Generator TN Module MCR Reactor Cleaning DRAIN Pump leaking? P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero MV 5 Sample Out Valve leaking? Examples of some potential leak points in the Bio. Tector P 1 Sample ACID Manual ZERO MANUAL SAMPLE IN

PRESSURE TEST: Structured fault finding 2. Disconnect MFC outlet tube. Seal MFC outlet. Test. 1. Pressure correct? MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer MV 4 Sample In EXHAUST 5. Seal exhaust valve. Test. SAMPLE OUT Oxidized Fluid Catch-pot Cooler Glass beads P 2 Circulation Pump Ozone Generator TN Module MCR Reactor 4. Disconnect reactor outlet tube. Seal reactor tube. Seal sample out valve. Test. Cleaning DRAIN P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero MV 5 Sample Out 3. Disconnect Ozone outlet tube. Seal ozone outlet. Test. Always follow a structured approach when looking for a leak. P 1 Sample ACID Manual ZERO MANUAL SAMPLE IN

Flow Test Purpose: to detect a blockage or partial blockage in a tube in the Bio. Tector. 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 Bio. Tectors flow remains above 72 LPH, the flow test passes. • If the gas flow drops below 72 LPH but remains above 40 LPH within the 30 second flow test time, a flow warning is logged. • If the gas flow drops below 40 LPH, a flow fault is logged and the Bio. Tector 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 Bio. Tector allows (30 s). • Exhaust (or Sample Out) Flow: Simulate the flow test with long time limit, useful for detecting a blockage.

FLOW TEST: EXHAUST MFC reading correctly? Pressure correct? MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer Ozone Generator MV 4 Sample In Valve blocked? EXHAUST Line blocked outside Bio. Tector? SAMPLE OUT Cooler Glass beads P 2 Circulation Pump TN Module Oxidized Fluid Catch-pot Ozone destructor filter blocked? MCR Reactor Cleaning DRAIN Oxygen inlet to reactor blocked? Note, this enters the top of the HS reactor. P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero MV 5 Sample Out P 1 Sample Examples of some potential blockage points in the Bio. Tector. Note that the Exhaust valve and Purge/Sample out valve lines are tested independently. ACID Manual ZERO MANUAL SAMPLE IN

FLOW TEST: SAMPLE OUT MFC reading correctly? Pressure correct? MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator Valve blocked? MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer Ozone Generator MV 4 Sample In EXHAUST Line blocked outside Bio. Tector? SAMPLE OUT Oxidized Fluid Catch-pot Cooler MCR Reactor Glass beads P 2 Circulation Pump TN Module Cleaning DRAIN Valve blocked? P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero MV 5 Sample Out P 1 Sample Examples of some potential blockage points in the Bio. Tector. Note that the Exhaust valve and Purge/Sample out valve lines are tested independently. ACID Manual ZERO MANUAL SAMPLE IN

FLOW TEST: Structured fault finding 8. Disconnect MFC outlet tube, but only when system de-pressurized. Test. 1. Pressurecorrect? MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator 4. Disconnect exhaust tube. Test. MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer Ozone Generator MV 4 Sample In EXHAUST 3. Disconnect ozone destructor outlet. Test. SAMPLE OUT Oxidized Fluid Catch-pot 2. Disconnect ozone destructor inlet. Test. TN Module 6. Disconnect reactor outlet tube. Test. Glass beads P 2 Circulation Pump Cooler MCR Reactor 5. Disconnect sample out tube. Test. Cleaning DRAIN P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero MV 5 Sample Out 7. Disconnect Ozone outlet tube, but only when system de-pressurized. Test. P 1 Sample 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. ACID Manual ZERO MANUAL SAMPLE IN

Ozone Test Purpose: to check the level of ozone generated by the Bio. Tectors ozone generator. When the test kit has been installed in accordance with T 006 and the installation confirmed by the user, the Bio. Tector activates the ozone generator. The Bio. Tector 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 T 006. 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 T 006, 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 15 s (or programmed level), the status of the ozone test is Pass. • If the o-ring breaks in a time between 15 and 60 s, the status of the ozone test is Low Ozone. • If the o-ring does not break within 60 s, the status of the ozone test is Fail.

OZONE GENERATOR TEST Warning: Only work on ozone generator if mains power is isolated MFC Mass Flow Controller OXYGEN Oxygen purity >95% oxygen, and free of water and oil? Ozone Generator O 2 Regulator If PCB is suspected as being faulty, replace it. 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.

SAMPLE PUMP TEST: FORWARD MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer Ozone Generator MV 4 Sample In Oxidized Fluid Catch-pot EXHAUST SAMPLE OUT DRAIN Cooler The sample should be pumped out the drain. Glass beads P 2 Circulation Pump TN Module MCR Reactor Cleaning P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero MV 5 Sample Out P 1 Sample ACID Manual ZERO MANUAL SAMPLE IN

SAMPLE PUMP TEST: REVERSE MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer Ozone Generator MV 4 Sample In Oxidized Fluid Catch-pot EXHAUST SAMPLE OUT DRAIN Cooler Glass beads P 2 Circulation Pump TN Module MCR Reactor Sample and oxidized fluid should be completely pumped back to sample point. Cleaning P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero MV 5 Sample Out P 1 Sample ACID Manual ZERO MANUAL SAMPLE IN

p. H Test Purpose: to check the p. H in the reactor at different stages in the reaction. The Bio. Tector 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 Bio. Tector can be stopped at any time to allow the p. H be checked.

Typical p. H 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 p. H. Only a very small sample should be removed from the reactor, so as not to effect the p. H for the next test. It is important that the previous reaction finished normally to eliminate the possibility of any p. H influence from the previous reaction.

EXAMPLE: TIC p. H TEST, MCR REACTOR MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer MV 4 Sample In Ozone Generator EXHAUST SAMPLE OUT Oxidized Fluid Catch-pot Cooler MCR Reactor Cleaning DRAIN pe r P 4 Base Pump BASE pa MV 5 Sample Out p. H With the circulation pump stopped, the liquid accumulates at the bottom of the reactor. Glass beads P 2 Circulation Pump TN Module MV 6 Acid P 3 Acid Pump Zero P 1 Sample 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. ACID Manual ZERO MANUAL SAMPLE IN

EXAMPLE: TIC p. H TEST, HS REACTOR MFC Mass Flow Controller OXYGEN O 2 Regulator MV 7 Injection MV 1 Exhaust CO CO 22 Analyzer SAMPLE OUT MV 6 Acid Oxidized Fluid Catch-pot P 2 Circulation Pump Cooler With the circulation pump stopped, the liquid accumulates at the bottom of the reactor. HS Reactor Cleaning DRAIN P 4 Base Pump BASE P 3 Acid Pump p. H Manual pa EXHAUST Ozone Destructor Ozone Generator MV 4 Sample In pe r MV 5 Sample Out Option 1 is to slightly open the TEE fitting, just enough to wet the p. H paper. p. H p er ap P 1 Sample ACID Stream 2 MANUAL STREAM 2 STREAM 1 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

p. H ISSUES MFC Mass Flow Controller MV 51 Purge OXYGEN O 2 Regulator p. H in sample very high ~>12 p. H or very low ~<2 p. H? MV 7 Injection MV 1 Exhaust Ozone Destructor CO 2 Analyzer MV 4 Sample In Ozone Generator EXHAUST SAMPLE OUT Oxidized Fluid Catch-pot Circulation pump running? Injection settings for sample, acid and base correct? Glass beads P 2 Circulation Pump Cooler TN Module MCR Reactor Acid, Base reagents: normality correct? Cleaning DRAIN Acid, Base pump: pumped volume correct? MV 5 Sample Out P 4 Base Pump BASE MV 6 Acid P 3 Acid Pump Zero P 1 Sample ACID Manual 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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.

GENERAL OXIDIZED FLUID LAYOUT CATCH TN MODULE POT EMPTY N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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.

GENERAL OXIDIZED FLUID LAYOUT CATCH TN MODULE POT EMPTY N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 MEASURING LAYOUT CELL CLEAN TN MODULE N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 MEASURING LAYOUT CELL WASH TN MODULE N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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. • The cell is emptied.

MEASURING CELL EMPTY N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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) N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 217 nm, the through-cell reference is 265 nm.

DIW MEASURE (ZERO) N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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. • The cell is emptied.

MEASURING CELL EMPTY N Pump DRAIN LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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 NO 3 - is measured. The measuring frequency is 217 nm, the through-cell reference is 265 nm 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 LV 3 Cleaning 265 nm detector 217 nm detector LV 2 DIW CLEANING DIW LV 1 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).