Headspace Troubleshooting Made Easy. Presented today by: Susan Scheib Sr. Technical Support Specialist Joe Barta FSE Chicago & Escalation Engineer

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2 Headspace Troubleshooting Made Easy Presented today by: Susan Scheib Sr. Technical Support Specialist Joe Barta FSE Chicago & Escalation Engineer

3 Topics to cover 7000 Determining, setting and checking flow rates and pressures Leak checking unit Troubleshooting of motor, sensor and heater errors Mechanical obstructions Clearing memory Reproducibility and Sensitivity problems Preventative maintenance

4 HT3 Topics to cover Checking flow rates and settings with MFC Leak Checking Unit Software diagnostics Sample history logs Clearing Memory Part replacement Maintenance and Troubleshooting Preventative maintenance

5 Topics to cover Both GC runtime set correctly Schedule optimization based on varying method temps GC check out first FET technique M.O.M. Reproducibility/response issues related to loop fill Sample Matrix affects IQOQPQ options

6 7000 flows and pressures Standby flow rate Measured at line going to top of needle Set in standby/ready mode 1000/GC cycle time For a 20 min cycle time It would be set to 50 ml/min

7 7000 Static Vial Pressure Prepare sample vial as you normally would Set up method parameters for your application Turn vial needle flow controller all the way off Counterclockwise Allow sample to run as normal- do not Step When vial goes up on needle, record pressure on vial pressurization gauge This is your static vial pressure

8 7000 Vial Pressure Vial Pressurization is set 2-4psi above static vial pressure From Standby/Ready screen Press 3 on the keypad Open Vial Needle Flow Control knob (clockwise) Page Down until you get to PRESS Press Y/7 on the keypad to turn on valve Turn Vial Pressurization Control Knob to dial in setting Press N/9 when complete

9 VIPR VIPR Variable Injection Pressure Regulator Set typically at 2-3psi below vial pressure or at the same pressure as your static pressure Creates a constant backpressure in system during loop fill for increased reproducibility

10 Leak Checking 7000 Place empty capped vial in carrousel In Standby/Ready Mode Press 3 on keypad Press 1 for Leak check & follow instructions on screen Place cap nut on vent. Does press. gauge reach vial press. setting? NO- check fittings in valve oven and around valves YES check septa on vial, repeat. May need to check incoming gas supply

11 7000 Gas Flows

12 7000 Gas Flows (cont.)

13 7000 Motor/Sensor Errors Access to sensor screen Something should be highlighted for all motors, no??? At bottom. Motor test screen Press 2 on keypad Manually turn white gears to move motor Pull Platen motor Clean off sensors/flag

14 7000 Heaters/Thermocouples Self test Checking Fuse Check LED s on Logic Board Press Temps and. on keypad

15 Clearing Memory on 7000 Write down all method parameters Turn power off/remove right side panel Locate lever for ROM Chip behind keypad Note orientation of ROM Chip and raise lever to remove chip Turn power on to 7000 with chip removed for sec. Turn off power, replace ROM chip

16 7000 Reproducibility/Sensitivity Incorrect Flow rates and Pressures Blocked needle or sample loop Method not optimized More to come

17 7000 Preventative Maintenance Check gas flows/ leak check Clean off fans/boards Lubricate worm gears on motors Clean out platen chambers & carrousel Check temps of unit Run a check standard

18 HT3 Flows and Pressures Setting the Standby Flow Rate Locate the Standby Flow Rate parameter in the method. 1000/GC cycle time A GC cycle time of 20 min = a Standby Flow Rate of 50ml/min Enter this value into the method and save it.

19 HT3 Flows and Pressures Checking the static vial pressure When the vial is pushed up on the needle, the software will measure the static vial pressure in the unit status pane and record this value.

20 HT3 Flows and Pressures Vial Pressurization method parameter For most applications, setting the vial pressurization at 8 or 10psi will be fine. Depending on the static vial pressure, you may choose to set the vial pressurization to 2-4psi above the static vial pressure. Set the vial pressurization time to exceed the time it takes to reach the pressurization. If you choose to use a timing event instead, make sure you set the vial pressurization time to what you want and make sure the vial pressurization pressure parameter is set high enough to meet that time.

21 HT3 Flows and Pressures Loop Fill Pressure method parameter For most applications, setting the loop fill pressure at 3-5 psi below the vial pressurization will work well. If you choose to use a timing event instead, make sure you set the loop fill time to what you want and make sure the loop fill pressure parameter is set high enough to meet that time. The loop fill pressure setting has a direct impact on the compound recoveries you receive. If the pressure is higher, you will have greater sensitivity than if the pressures are lower.

22 HT3 Leak Checking Leak checking is easy using the software. Place a NEW capped empty vial in the #1 position of the carrousel. Click on the Leak Check icon on the top of the software. The unit will pressurize the vial until 15psi and then wait for the pressure to drop. If the unit passes the Leak Check, no further action is required. If the unit fails Leak Check, perform the Benchmark Test so that the valves can be tested individually for failure.

23 HT3 Leak Check Loop

24 HT3 Leak Check - Trap

25 HT3 Software Use the software to troubleshoot problems. Click on Tools, Diagnostics. Motors Valves Advanced Packets Firmware 21 CFR Part 11

26 HT3 Software Benchmark Test Running the Benchmark Test is a great diagnostic tool for troubleshooting problems. In the software, click on Tools, Diagnostics and the Benchmark tab. Follow the onscreen instructions. Pay special attention to the appropriate test. If you are having valve problems, look at the Valve Actuation Test results. If running in both loop and trap modes, the GC pressure should be greater than 25psi

27 HT3 Software Software has useful History Logs In the software, click on View > System History. Select a date range for the history filter. For HT3 errors, select the error box. This will show you instrument errors. For sample information, select the sample box. This will show you a run log of your samples. Note that the static and loop fill pressures, and the vial pressurization are all recorded.

28 HT3 Clearing Memory If the unit is doing strange things or is giving strange errors, consider clearing the memory. Turn the unit off, open from front covers. Remove the watch battery from the CPU/motor board. Wait 30 seconds and replace the battery. Turn the unit back on.

29 HT3 Maintenance If your HT3 has the dynamic trapping option, you can easily change the trap. Turn the unit off. Open the front cover to get access to the trap assembly. Loosen thumb nut off safety shield Remove the nuts on either side of the trap. Carefully remove the trap from the heater, replace the GV ferrule and the nuts. Perform a leak check on the unit to verify that the replacement trap is leak tight. Click on the Bake on the top of the software to Bake the trap out prior to use.

30 HT3 Maintenance Checking Flows Allow hot needle to cool Check flow to needle by removing line at top Removing Needle Allow to cool Remove nuts at top and side Remove kep nuts first Remove needle from unit Loosen allen screws and disassemble needle

31 HT3 Maintenance Lubricating the motor gears. Locate the worm gears on the platen, vial loader, needle loader, and carrousel motors. Soak a Q-tip in a light oil, like 3in1 Oil, sewing machine or gun oils. Do not use WD-40 or grease Wipe the Q-Tip on the worm gear and wipe off all the access. Using the software, work the oil into the gears. Refer to page of HT3 User Manual for further information.

32 If you are having flow problems: HT3 Troubleshooting Verify MFC Flow rate Check pressure of system Check incoming tank pressure Leak check system

33 HT3 Troubleshooting If vials get stuck as the carrousel indexes in/out: Grab the vial loader platform with pliers and adjust the platform accordingly until the vial s bottom sits flush with the roof of the chassis. Use the software diagnostics to verify the carrousel can move freely and vials don t get caught as the carrousel moves back and forth.

34 HT3 Troubleshooting If you determine a valve doesn t work using the software diagnostics, it can easily be replaced. All valves in unit are the same Trap valve (if applicable) is located inside the front panel of unit.

35 HT3 Troubleshooting If a vial breaks in the platen or the platen is getting stuck, removing the insulated cover is easy. Remove insulation around platen Clean out chambers See Page of HT3 User Manual for additional information

36 HT3 Heated Zones HT3 uses RTD s not Thermocouples Fuse for each heated zone Logic comes from CPU, then Temp to AC board

37 HT3 Preventative Maintenance Turn unit off and wait for heated zones to cool. Blow out dust from unit and off the fans. Lubricate the motor gears. Inspect the sample needle for damage. Turn the unit on and wait for the self-test to complete. Check the standby flow. Run the leak check and Benchmark tests. Run a check standard.

38 7000 and HT3 Set GC cycle time correctly to maximize sample throughput. GC cycle time is from ready to ready on the GC Schedule optimization based on varying method temperatures Run methods with cooler temperature zones first because it may take awhile for more insulated zones, like the platen, to cool down, extending run time.

39 Reproducibility/Response Issues? Check out GC first. Verify that the GC works correctly and the pressures and temperatures are what they should be. Perform the Full Evaporative Technique. Take 10ul of standard and inject it into an empty vial. Turn up the platen temperature to fully evaporate the 10ul in the vial, maybe 150C. Run the sample as usual and the standard should elute on the GC. Run this several times to establish headspace reproducibility. Compare the response of the FET to what you normally get.

40 Reproducibility/Response Issues? Use the Method Optimization Mode (M.O.M.) Program allows you to use a standard method of your choosing. Change one of the programmable settings (like platen temperature) a few degrees at a time. Run a series of standards to find out at what setting you get the best response/reproducibility. Can easily be done overnight so that downtime can be minimized.

41 Reproducibility/Response Issues? Make sure your loop fill time is correct. If your loop fill time is too short, the quick release of flow into the loop may cause inconsistent filling. If your loop fill time is too long, you might have low flow going through the loop which will cause inconsistent filling. Place a flow meter over the vent and record when the flow is 10-30ml/min, set the loop fill time accordingly. The shorter the loop fill time, the higher compound response you will have. Longer the loop fill time, the lower compound response you will have.

42 Sample Matrix Effects Depending on your sample matrix, you may have to make some adjustments to achieve the results you want. Partition coefficients (K) are impacted by matrix affects. Compounds with lower K values transfer from matrix to headspace easily. Compounds with higher K values are more likely to stay in the matrix instead of becoming gaseous and going into the headspace.

43 Sample Matrix Effects Adding salt to a liquid matrix forces polar compounds (like methanol) out of the liquid and into the gas phase, making for better compound recovery. Adjusting the ph can suppress biological growth in a sample and increase compound recovery. Some compounds will be seen better or suppressed depending on the ph of the sample.

44 Sample Matrix Effects Decreasing sample size will allow the compounds to go into the gaseous phase better (ten.10g pieces will allow better transference to the gas phase than one 1g piece.) Mixing the sample will help agitate compounds into the gas phase. Depending on the boiling point of the solvent, you may need to lengthen the Sample Equilibration Time or increase the Sample Equilibration Temperature.

45 IQ/OQ/PQ Teledyne Tekmar can provide Installation/Operational/Performance Qualifications for a 7000 or HT3 system. An existing system can have Qualifications performed on it in a timeline of your choosing by certified service engineers. If you receive a 7000 or HT3 that is new to you, we can install and qualify the headspace so that you know that it meets headspace standards of a new instrument.

46 Why upgrade from a 7000 to a HT3? Both headspaces utilize static headspace technology. The HT3 has dynamic headspace capability, with the use of an optional analytical trap. (increases sensitivity) The HT3 has 60 position sample carrousel, where the 7000 has 50 positions. The platen heater is designed better. The HT3 has one coiled heater and one RTD (Resistance Temperature Detector) to read the temperature. The 7000 has four heaters and four thermocouples, meaning four times the parts to breakdown. RTDs are more stable and accurate in their reading.

47 Why upgrade from a 7000 to a HT3? The HT3 has a mass-flow controller (MFC) that has a proven record in other Teledyne Tekmar products. Allows pressures and flows to be completely controlled by the software. Permits more reliable and consistent pressure functions and the ability to monitor pressures through the sampling process. Instead of using a VIPR on the 7000, using the MFC offers a tighter control loop fill in the HT3, so the VIPR is eliminated. Leak testing is more intuitive with the inline pressure sensor from the MFC.

48 Why upgrade from a 7000 to a HT3? Integrated software The 7000 was offered with a remote keypad or PC Teklink software. Some people considered the keypad to be limiting and cumbersome. The HT3 comes with software that utilizes the benefits and features of the Teklink software. Teklink can be run on same PC as GC software. (minimum OS required) Design and serviceability The HT3 has easily removed panels that allows easy access to all assemblies of the instrument

49 Why upgrade from a 7000 to a HT3? Upgradeability If you buy the static headspace HT3, then decide to upgrade to the optional dynamic mode, the trapping module can be installed. Easy transition between 7000 to HT3 Due to differences in technology (MFC) some method development may be needed.

50 Questions? Joe is on line to help answer your questions Later on Tekmar Technical Support (+1) outside the US Thank you! Please join us for our next webinar in this series UV/Persulfate TOC Troubleshooting Made Easy to be held Tues. October 4 th at 2pm EST.