Blank Procedure - Waters Corporation



Performance Maintenance Protocol

996/2996/2998 PDA Detector

|Serial Number/ |      |

|Firmware Version: | |

|Date: |      |

|Performer: |      |

Performance maintenance

Goal

This performance maintenance protocol is a guide to performing maintenance tasks on your system. Packaged as part of the performance maintenance kit, it is intended to ensure optimum performance and an uninterrupted period of trouble-free operation.

Schedule

Waters recommends that performance maintenance visits be performed once a year. Systems under heavy use or using aggressive solvents will need more frequent maintenance. For detailed maintenance schedules, refer to the appropriate operator’s guide(s) located on the Waters Web site. Failure to follow the maintenance schedules as described in the operators guides may result in unreliable operation and inaccurate laboratory results. For some protocols, optional tests can be performed by Waters field service engineers for added confidence and reliability.

Safety considerations

[pic] Caution: Always observe Good Laboratory Practice and, when handling Waters Critical Clean™ parts, refer to Controlling Contamination in UPLC/MS and HPLC/MS Systems, P/N 715001307.

[pic] Warning: To prevent personal contamination with biologically hazardous or toxic materials, carefully dispose of the replaced component in the appropriate waste container.

[pic] Warning: When performing maintenance, remove power to the unit by powering down and disconnecting the power cord.

[pic] Warning: Always use proper static protection when handling any printed circuit boards.

[pic] Warning: Dispose of components in accordance with local or customer regulations. If the component comes with a Waters Corporation return sheet, follow its instructions.

[pic] Warning: Avoid contact with solvents by wearing suitable gloves and safety glasses.

[pic]

Some protocols may involve removing instrument covers, exposing the performer to high voltages, high currents, and moving parts. This presents risks of electric shock and/or damage to the instrument. To reduce these risks, Waters recommends that these protocols be conducted by certified Waters field service engineers, who have access to the latest information on Waters products. Waters is not responsible for an unqualified performer initiating actions that they do not understand. If there is any doubt on the part of the performer, a Waters certified field service engineer should conduct the performance maintenance activity.

Waters Quality Parts

Waters designs and manufactures Waters Quality Parts® to the same strict regulatory standards as your high-performance Waters systems. Waters recommends using Waters Quality Parts for all maintenance activities. Failure to use Waters Quality Parts may compromise laboratory results and reliability.

Customer education

Waters offers several operation and maintenance courses for ACQUITY® UPLC®, Alliance® HPLC and MS systems as well as courses designed to help you maintain professional competency and further your knowledge in Chromatography, UPLC, Informatics and Mass Spectrometry. For more information on available training courses from Waters Educational Services please visit the Waters Web site.

Compliance services

Waters Compliance Services help you achieve and maintain the regulatory compliance of your LC and MS instruments and software with a combination of expertise, compliant-ready systems and software, and a portfolio of services to ensure that you have quality data, consistently. To learn more about Compliance Services, please visit the Waters Web site.

General tasks

Use the following guidelines when conducting performance maintenance visits. This information is intended to be a guide only. For example:

• If a particular module has been recently serviced, it may need only testing and replacement of fewer parts.

• Not all procedures apply to all instruments (specify NA in the Comments section if the procedure does not apply).

• If the instrument fails to perform adequately during pre-performance maintenance checks, further service may be required beyond the scope of this protocol. Such service may incur additional parts and labor charges.

The following table lists the general tasks to be performed during a performance maintenance visit. Perform and confirm the steps listed for each procedure and record any comments that you have about the results at the end of each section.

For detailed instructions and a list of the necessary tools, refer to the operator’s guide located on .

NOTE: Before starting the performance maintenance protocol, power the detector off and then on.

|Inspect |Maintenance tasks |Post-performance maintenance checks |Optional calibration tests1 |

|Firmware version2 |Lamp |Initialization diagnostics |Wavelength accuracy |

|Fan |Foam filter3 |Read lamp energy4 | |

|Flow cell | |Verify calibration5 | |

|Tubing and fittings | | | |

|Error logs | | | |

1 Optional tests performed by Waters field service engineers as part of a Total Assurance with Calibration Plan. For those without the plan, the tests can be performed for an additional charge. Some of these tests may require additional chemistry kits that are not supplied in the performance maintenance kit.

2 Firmware upgrades, if required, should be performed by a Waters field service engineer prior to beginning performance maintenance. Firmware upgrades may require re-qualification of the upgraded instrument if it is in a regulated environment. If using MassLynx, checking the firmware version for the 996/2996 can only be performed by a Waters field service engineer using RS-232.

3 Available only in the 996/2996 Performance Maintenance Kits. Not required for the 2998.

4 For MassLynx users with a 996/2996, read lamp energy is performed only by Waters field service engineers.

5 For MassLynx users with a 996/2996, verify calibration is performed only by Waters field service engineers.

Inspect

Firmware version

Confirm what firmware versions are installed. Update if required.

NOTE: Refer to Software Downloads section under the Services & Support tab on the home page for the latest firmware and driver pack release notes. These release notes detail software and data system requirements, and installation notes.

To identify the 2998 firmware version in MassLynx:

1. Click the Additional Information tab in the Inlet editor.

2. Right-click the 2998 control panel and then select Launch Instrument Console.

3. Select the PDA detector, and then select Configure > Module Information. The firmware version is displayed.

To identify the 2998 firmware version in Empower:

1. Right-click the 2998 control panel in the Run Samples window, and then select Launch Instrument Console.

2. Select the PDA detector, and then select Configure > Module Information. The firmware version is displayed.

To identify the 996/2996 firmware in Empower:

1. Click Configure System in the Empower Start Up window.

2. In the Configure System window, click Empower Nodes in the Empower Configuration tree.

3. Select the proper node from the table, and then right-click and choose Properties.

4. Select the Instruments tab in the Properties window.

5. Locate the 996/2996 from the list and record the firmware version on the cover page of this performance maintenance protocol.

Firmware check complete.

Yes No N/A

Comments:      

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| |

Fan

To inspect the fan:

1. Observe the fan on the rear of the instrument.

2. Ensure that the fan grate is clear of debris and dust. The fan should be blowing outward.

3. Clean if necessary.

Fan inspection complete.

Yes No N/A

Comments:      

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Flow cell

Check flow cell for leaks.

Flow cell inspection complete.

Yes No N/A

Comments:      

| |

     

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| |

Tubing and fittings

Check tubing and fittings for leaks.

Tubing and fittings inspection complete.

Yes No N/A

Comments:      

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| |

     

| |

Error logs

Review error logs complete.

Yes No N/A

Comments:      

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Maintenance tasks

The following procedures are routinely performed as part of the performance maintenance. Waters Quality Parts have been used to replace/rebuild all parts.

• Lamp

• Foam filter

Yes No N/A

Comments:      

| |

     

| |

     

| |

Post-performance maintenance checks

Perform the post-performance maintenance checks only in the order listed.

Initialization diagnostics

Turn on power, allow instrument to complete and pass on-board software checks.

Initialization diagnostics check complete.

Yes No N/A

Comments:      

| |

     

| |

     

| |

Read lamp energy

1. Ensure that the flow cell is clean before reading the lamp energy.

2. For the 2998, use the read energy utility in Console to read the lamp enegy spectrum between 190 – 800 nm.

a. Click Maintain > Read energy > Read.

3. For the 996/2996, view the reference energy spectrum between 190 – 800 nm in Empower.

a. Click Diagnostics > PDA Calibration.

b. Click Run in the PDA Calibration window.

c. Click Stop.

4. Read the lamp energy at 230 nm.

5. Record the results.

|Wavelength (nm) |Exposure time (msecs) |Energy counts |

|230 |21 (996/2996 only) |      |

|230 |5 (2998 only) |      |

Read lamp energy complete.

Yes No N/A

Comments:      

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| |

Verify calibration

1. Fill the flow cell with a solvent compatible with the samples and mobile phases that you have been using. Waters recommends methanol.

2. For the 2998, use the verify calibration utility in the Console.

a. Maintain > Verify calibration > Start.

3. For the 996/2996, in the menu bar of the Run Samples window in Empower:

a. Click Diagnostics > PDA Calibration.

b. Click Run in the PDA Calibration window.

c. Click Stop to display a spectrum.

d. Click Calibration > Calibration Accuracy.

4. Record the results.

* The maximum deviation must be within +/- 1 nm of the standard calibration to pass.

|Verify calibration results |

|Calibration | Pass Fail |

|Maximum deviation |       nm |

Verify calibration complete.

Yes No N/A

Comments:      

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| |

Performance maintenance confirmation

|I confirm on behalf of | |      | |

| |Company Name |

|that this performance maintenance |      |

|procedure has been satisfactorily completed on: | |

| | | | |

| | |Serial No. |

| Signed: | | Date:       |

| | | | | | |

|Customer | |

|      | |

| | | | | | |

|Type Name | |

|I certify that the maintenance procedure has been successfully completed. | |

| Signed: | | Date:       |

| | | | | | |

|Waters Engineer | |

|      | |

| | | | | | |

|Type Name | |

|Comments:      |

| | | |

|      |

| | | |

| | |

|Waters Corporation |[pic] |

|34 Maple Street | |

|Milford, Massachusetts | |

|01757 USA | |

|Waters, MassLynx, The Science of What’s Possible and Waters Quality Parts are registered trademarks of Waters Corporation. All other trademarks are |

|property of their respective owners. |

|©2014 Waters Corporation. Printed in the U.S.A. |

Optional calibration tests

Optional calibration tests are performed by Waters field service engineers as part of a Total Assurance with Calibration Plan. For customers without this plan, these tests can be performed for an additional charge. Some of these tests may require additional chemistry kits that are not supplied in the performance maintenance kit.

Tools/materials required

* UV/Visible Absorbance Detector Wavelength Accuracy Calibration Solution (part number WAT042885)

* 10 mL priming syringe

* 100% HPLC-grade water

* 2 mL vial

* Powder-free nitrile gloves and safety glasses

[pic] Caution: Never change directly between immiscible solvents, or between buffered solutions and organic solvents. Immiscible solvents form emulsions in the fluid pathways. Buffered solutions and organic solvents in combination can result in salt precipitation in the gradient proportioning valves, pump heads, check valves, and other parts of the system. Confirm that all fluids in the system are miscible with methanol.

Wavelength accuracy

Testing the wavelength accuracy confirms that programmed wavelengths are within accuracy specifications. This test requires the Waters UV/Visible Absorbance Detector Wavelength Accuracy Calibration Solution (part number WAT042885).

* To ensure maximum testing accuracy, power-on the detector at least 60 minutes before you perform this test. Also, note that no column is required.

Testing for wavelength accuracy using Millennium32 or Empower

Creating the methods

1. Flush the flow cell with water at 1 mL/min for 20 minutes. Use an intermediate solvent to ensure miscibility if required.

2. Create a system in Millennium32 or Empower that is comprised of only the detector to be tested.

3. Double-click Run Samples, select the system that you created, and a project that has the PDA option enabled, then click OK.

4. In the Run Samples window, click the Single tab.

5. Click Develop Methods.

6. In the New Method Set, select the Instrument Method wizard, and then click Create New.

7. In the Instrument Method Editor, create and save an instrument method using the following parameters:

|Parameter |Setting |

|3D data collection (2996/2998 only) |Selected |

|Start wavelength |230 nm |

|End wavelength |700 nm |

|Resolution |1.2 nm |

|Sampling rate |2.0 spectra/sec |

|Auto exposure |Selected |

|Interpolate 656 nm |Selected |

|Filter response (Millennium32 version |0 sec |

|3.2) | |

|Filter response (Millennium32 version |1 sec |

|4.0 or Empower) | |

6. Select File > Save.

7. Enter a name for the instrument method and then click Save.

8. Select File > Exit.

9. Click Next.

10. In the Select Default Methods window, accept the defaults, and then click Next.

11. Name the method set, then click Finish.

12. On the Single Tab of Run Samples, enter the sample name.

13. From the Method Set drop-down list:

a. Select the name of the new method set that you created.

b. Enter a vial identification number.

c. Enter an injection volume of 0 µL.

d. Enter a run time of 5 minutes.

e. Accept the defaults for all other parameters.

Preparing the sample and making the injection

1. Rinse the 10 mL syringe twice with HPLC-grade water, and then flush the flow cell twice with HPLC-grade water.

2. From the Instrument Method toolbar, select the instrument method you created.

3. Click Setup and wait for the status to change to Idle.

4. Click the Prepare icon.

5. If prompted, select a printer for reporting, and then click OK.

6. Select Customize > Channels.

7. Enter 254 nm for the wavelength.

8. Click the Spectra tab, and then select View PDA Spectrum.

9. Click OK.

14. Click the Inject icon

15. Allow the baseline to stabilize.

16. After the baseline is stable, inject 5 mL of the Wavelength Accuracy solution (erbium perchlorate) into the detector flow cell inlet line using the 10 mL syringe and priming syringe needle.

17. After a few seconds, the erbium perchlorate absorbance spectrum appears in the real-time spectrum plot. Allow the erbium perchlorate solution to remain in the flow cell for at least 2 minutes. The real-time plot updates automatically. Hold a constant pressure on the priming syringe to maintain a steady response.

18. When the run time has expired, exit Run Samples.

19. Flush the flow cell for at least 10 minutes with HPLC-grade water at 1 mL/min.

Reviewing the data

1. In the Login window, click Review Data.

2. Select your Project > Review > Channels, and then click OK.

3. Select the sample name that you just ran. Click Review.

4. At the bottom of the Main window, click the 3D Channels tab to select the sample you named.

5. From the View menu, select 3D Layout.

6. Enter 254 (255 for 996/2996) in the Extract Choices field (next to the Extract Chromatogram icon), and then, click the Extract Chromatogram icon.

7. Click the Extract Spectrum icon, or Select Process > Extract Spectrum.

8. In the Contour plot, extract the spectrum by entering the time, or by dragging the spectral marker over the erbium spectrum (to the time at which the detector recorded the presence of the erbium perchlorate in the flow cell). Be sure to place the spectral marker in the center of the extracted chromatogram plateau. Note the change to the Spectral plot.

9. Right-click the spectral plot, and then click Properties.

20. From the Spectra tab, click Label Spectra (default).

21. From the UV Labels pane, click Multiple Lambda Max.

22. From the UV Labels pane drop-dwon list, click Wavelength.

23. Enter 20.0 in the Lambda Max Window text-list box.

24. Click OK.

25. To print the spectrum, right-click the Spectral plot, select Print, and then click OK.

26. Record the wavelength values displayed for the indicated peaks. Each peak wavelength value has a tolerance of ±1.5 nm.

|Measured peak value (nm) |Expected peak value (nm) |Result |

|      |255 ± 1.5 nm | Pass Fail |

|      |379 ± 1.5 nm | Pass Fail |

|      |523 ± 1.5 nm | Pass Fail |

Wavelength accuracy test (Millennium32/Empower) complete.

Yes No N/A

Comments:      

| |

     

| |

     

| |

Testing for wavelength accuracy using MassLynx

Creating the methods

1. Flush the flow cell with water at 1 mL/min for 20 minutes. Use an intermediate solvent to ensure miscibility if required.

27. Create a new MassLynx project to contain the PDA qualification methods and data.

28. Create a sample list that includes these columns:

• File Name

• MS File

• Inlet File

• Bottle

• Inject Volume

29. Create an inlet method using the detector and solvent management system parameters in the following tables.

* If necessary, in the Inlet Method window, configure the inlet system by selecting Tools >Instrument Configuration.

|PDA detector parameters |

|Parameter |Setting |

|Start wavelength |230 nm |

|End wavelength |700 nm |

|Resolution |1.2 nm |

|Sampling rate |2.0 spectra/sec |

|Interpolate 656 nm |Selected |

|Run time (mins) |5.0 |

|Filter response |1 |

|Save to disk |Selected |

|Solvent management parameters |

|Parameter |Setting |

|Flow rate |0.5 mL/min |

|Run time (mins) |10.0 |

30. Click Configure, and then follow the on-screen instructions.

31. Save and load the inlet method.

32. If a mass spectrometer is configured as part of your system, create an MS method using the following parameters.

|MS method parameters |

|Parameter |Setting |

|Acquisition mode |Centroid |

|Start mass |50 |

|End mass |250 |

|Run time (mins) |5 |

|Ion mode |Select as required for the installed |

| |probe type |

|Scan time (sec) |10 |

|Inter scan time |0.05 |

Making the injection

1. Place a vial of HPLC-grade water in position 1 of the autosampler.

Note: This allows MassLynx to “see” a contact closure and start the acquisition.

2. Complete line 1 of the sample list using the filename, an injection volume of 0 μL, and the inlet and MS methods created earlier. If necessary, ensure that the bed layout, vial position, and injection volume are defined correctly for the autosampler configuration.

3. Press Start on the sample list page to start the acquisition.

4. After acquisition has started, allow one minute for the baseline to stabilize.

33. Disconnect the detector’s inlet and outlet lines, and direct the line from the pump to waste.

34. Inject 5 mL of the erbium perchlorate wavelength accuracy solution using the 10 mL priming syringe and needle. Allow the solution to remain in the flow cell for 1 to 2 minutes while continuing to apply positive pressure to the syringe.

Analyzing the data

1. While running the acquisition, analyze the data.

35. Display the spectrum by highlighting line 1 of the sample list and clicking Spectrum.

36. Enable real-time update by ensuring that the Stopwatch icon is selected.

37. Click the 4-way arrow to expand data to the full window.

38. Select Display > Peak Annotation. Ensure that only Wavelength is selected and Decimal Places is set to 0 to display values as integers, and then click OK.

39. Click the Stopwatch icon to disable real-time updating.

40. Click (text icon), and add a text string to the spectrum that contains the test name, PDA serial number, and date.

41. Print the spectrum by selecting File > Print, and clicking OK.

42. Record the wavelengths displayed on the spectrum printout. Each peak wavelength value has a pass/fail tolerance of ±2.0 nm.

43. Reconnect the solvent management system to the detector, and flush the flow cell with HPLC-grade water for 5 minutes at 1 mL/min.

|Measured peak value (nm) |Expected peak value (nm) |Result |

|      |255 ± 1.5 nm | Pass Fail |

|      |379 ± 1.5 nm | Pass Fail |

|      |523 ± 1.5 nm | Pass Fail |

Wavelength accuracy test (MassLynx) complete.

Yes No N/A

Comments:      

| |

     

| |

     

| |

Calibration confirmation

|I confirm on behalf of | |      | |

| |Company Name |

|that the calibration has been satisfactorily completed on: |      |

| | | | |

| | |Serial No. |

| Signed: | | Date:       |

| | | | | | |

|Customer | |

|      | |

| | | | | | |

|Type Name | |

|I certify that the calibration has been successfully completed. | |

| Signed: | | Date:       |

| | | | | | |

|Waters Engineer | |

|      | |

| | | | | | |

|Type Name | |

|Comments:       |

| | | |

|      |

| | | |

| | |

|Waters Corporation |[pic] |

|34 Maple Street | |

|Milford, Massachusetts | |

|01757 USA | |

|Waters, MassLynx, The Science of What’s Possible and Waters Quality Parts are registered trademarks of Waters Corporation. All other trademarks are |

|property of their respective owners. |

|©2014 Waters Corporation. Printed in the U.S.A. |

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