PERFORMANCE VERIFICATION: IONSCAN LS with Autosampler Module

Transcription

1 Version 5.0 Page 1 of 8 PERFORMANCE VERIFICATION: IONSCAN LS Smiths Detection 30 Technology Dr. Warren, NJ Copyright Smiths Detection 007 All rights reserved. Reproduction, adaptation or translation without prior written permission is prohibited, except as allowed by copyright laws. Warranty The information contained in this document is subject to change without notice. Smiths Detection makes no warranty of any kind with regards to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Smiths Detection shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.

2 Version 5.0 Page of 8 PRE EXECUTION PROTOCOL APPROVAL SMITHS DETECTION - PROTOCOL APPROVAL I agree that the Performance Verification (PV) procedures, assembled by Smiths Detection, are appropriate for the equipment defined in the table of contents. Name Signature Date CUSTOMER PROTOCOL APPROVAL I agree that the PV procedures in this document are applicable to the equipment defined in the table of contents. Name Signature Date QUALITY PROTOCOL APPROVAL I agree that the PV procedures in this document are applicable to the equipment defined in the table of contents. Name Signature Date POST EXECUTION PROTOCOL APPROVAL SMITHS DETECTION - PROTOCOL APPROVAL I agree that the PV procedures, assembled by Smiths Detection, are appropriate for the equipment defined in the table of contents. Name Signature Date CUSTOMER PROTOCOL APPROVAL I agree that the PV procedures in this document are applicable to the equipment defined in the table of contents. Name Signature Date QUALITY PROTOCOL APPROVAL I agree that the PV procedures in this document are applicable to the equipment defined in the table of contents. Name Signature Date

3 Version 5.0 Page 3 of 8 TABLE OF CONTENTS PRE EXECUTION PROTOCOL APPROVAL... SMITHS DETECTION - PROTOCOL APPROVAL... CUSTOMER PROTOCOL APPROVAL... QUALITY PROTOCOL APPROVAL... POST EXECUTION PROTOCOL APPROVAL... SMITHS DETECTION - PROTOCOL APPROVAL... CUSTOMER PROTOCOL APPROVAL... QUALITY PROTOCOL APPROVAL... TABLE OF CONTENTS...3 GENERAL INSTRUCTIONS...6 SIGNATURE PROTOCOL...6 ERROR CORRECTION...6 NO-ENTRY SPACES...6 USER REQUIREMENTS...6 PARTS AND MATERIALS...7 REQUIRED TEST PARTS AND MATERIALS...7 REQUIRED TEST STANDARDS...7 INSTRUMENT TO BE VERIFIED...8 TEST PROCEDURE...8 TEST LOCATION...9 DESORBER SEAL CHECK...10 PURPOSE...10 BACKGROUND...10 TEST EQUIPMENT LIST...10 PROCEDURE...10 RESULTS...10 AUTOSAMPLER ALIGNMENT CHECK...11 PURPOSE...11 BACKGROUND...11 TEST EQUIPMENT LIST...11 PROCEDURE...11 RESULTS...11 AUTOSAMPLER SYRINGE VOLUME CALIBRATION CHECK...1 PURPOSE...1 BACKGROUND...1 TEST EQUIPMENT LIST...1 PROCEDURE...1 RESULTS...1 AUTOSAMPLER SLIDE TRAY CHECK...13 PURPOSE...13

4 Version 5.0 Page 4 of 8 BACKGROUND...13 TEST EQUIPMENT LIST...13 PROCEDURE...13 RESULTS...13 NOISE CHECK...14 PURPOSE...14 BACKGROUND...14 TEST EQUIPMENT LIST...14 PROCEDURE...14 RESULTS...14 CALIBRANT ION CHECK...15 PURPOSE...15 BACKGROUND...15 PROCEDURE...15 RESULTS...16 REACTANT ION CHECK...17 PURPOSE...17 BACKGROUND...17 PROCEDURE...17 CARRYOVER CHECK...18 PURPOSE...18 BACKGROUND...18 TEST EQUIPMENT LIST...18 PROCEDURE...18 RESULTS...18 LIMIT OF DETECTION CHECK...19 PURPOSE...19 BACKGROUND...19 TEST EQUIPMENT LIST...19 PROCEDURE...19 RESULTS...19 DETECTOR LINEARITY CHECK...0 PURPOSE...0 BACKGROUND...0 TEST EQUIPMENT LIST...0 PROCEDURE...0 RESULTS...0 PEAK PROFILE CHECK...1 PURPOSE...1 BACKGROUND...1 TEST EQUIPMENT LIST...1 PROCEDURE...1 RESULTS...1 INJECTION REPEATABILITY CHECK... PURPOSE... BACKGROUND... TEST EQUIPMENT LIST...

5 Version 5.0 Page 5 of 8 PROCEDURE... RESULTS... SUMMARY OF PERFORMANCE VERIFICATION...3 FINAL CONCLUSION...3 NOISE ANALYSIS...4 REGRESSION ANALYSIS...4 DETERMINATION OF INJECTION REPEATABILITY...4 QUALIFICATION CONTROL PARAMETERS...4 AUTOSAMPLER MODULE...4 HIGH PERFORMANCE INJECTOR, AUTOSAMPLER ONLY...4 CRITICAL IONSCAN PARAMETERS, NEGATIVE AND POSITIVE ION MODES...4

6 Version 5.0 Page 6 of 8 GENERAL INSTRUCTIONS SIGNATURE PROTOCOL TESTED BY: Signature and/or initials of Smiths Detection Field Service Engineer, or other personnel performing tests. Date indicates the date test was executed. ACCEPTED BY: Signature and/or initials of customer representative. QA ACCEPTED: Signature and/or initials of customer QA department responsible for reviewing data. ERROR CORRECTION In the event of an entry error, cross out the incorrect value with a single line and write the correct entry. Initial and date the error. If space does not allow, footnote the error, and correction at the bottom of the page. eg. 0FEB04 NO-ENTRY SPACES Any entry that is not filled in (ie. test not necessary, space for comments not needed, etc.) should be crossed out with one diagonal line. Write a short reason, or N/A on the line along with initials and date. USER REQUIREMENTS The IONSCAN-LS detection system is a trace chemical detection tool that utilizes the analytical technique of Ion Mobility Spectrometry. Ion Mobility Spectrometry measures the movement of ions created via atmospheric pressure chemical ionization. Movement of ions is through a counter flow gas phase. Characteristic mobilities are automatically compared to user-generated libraries. Quantitative reports are generated by a custom 1CFR11 compliant software package. A dedicated liquid autosampler increases reproducibility ofthe compounds analyzed by this analytical tool. Analysis times are typically seconds. The timeliness of the data provides faster overall data turnaround for any analytical laboratory. It requires standard power, and a PC, for automated analysis, 1CFR11 compliance, and quantitation. The features of the IONSCAN-LS system are testable as documented in the Operation Qualification procedures, unless they are functionally assumed as inherent to the system, ie. Ni63 ionization source, or a constraint by design, ie maximum temperature limitations. The IONSCAN-LS analytical system has demonstrated it applicability in the areas of pharmaceutical cleaning validation, raw material analysis, illegal/counterfeit drug detection and interdiction, industrial hygiene and more

7 Version 5.0 Page 7 of 8 PARTS AND MATERIALS The following parts and materials are required for running the installation qualification. REQUIRED TEST PARTS AND MATERIALS Quantity Item 1 10-µL syringe, SGE or compatible 1 Solution standards kit 1 pk Teflon substrates p/n pk Teflon substrates p/n Teflon card, ring assembly 1 Personal computer running Windows 000 or XP 1 Excel software package 100 ml Hexane Pesticide grade or comparable 100 ml Acetone Pesticide grade or comparable 1pk -ml, 1-mm amber autosampler vials 1pk Caps with silicone/teflon septa REQUIRED TEST STANDARDS Quantity Solution 1 ml 5 pg/µl TNT in hexane 1 ml 50 pg/µl TNT in hexane 1 ml 100 pg/µl TNT in hexane 1 ml 150 pg/µl TNT in hexane 1 ml 00 pg/µl TNT in hexane 1 ml 50 pg/µl TNT in hexane 1 ml 500 pg/µl TNT in hexane 1 ml 50 pg/µl diazepam in acetone 1 ml 100 pg/µl diazepam in acetone 1 ml 150 pg/µl diazepam in acetone 1 ml 00 pg/µl diazepam in acetone 1 ml 50 pg/µl diazepam in acetone 1 ml 1000 pg/µl diazepam in acetone Solutions prepared by Smiths Detection using certified analytical standards. Analyte IUPAC Name CAS # Concentration Supplier Lot No.,4,6-TNT Diazepam 1-Methyl-,4,6- trinitrobenzene 1-Methyl-5-phenyl-7- chloro-1,3-dihydro- H-1,4-benzodiazepin- -one mg/mL 1mg/mL Cerilliant Cerilliant

8 Version 5.0 Page 8 of 8 INSTRUMENT TO BE VERIFIED IONSCAN MODEL# IM-Station Software Ver. or Serial Number PROCLAIMS Software Ver. Firmware Version Operational Time Negative Mode Positive Mode Autosampler s/n Sample Count A/S Firmware Version TEST PROCEDURE 1. Verify that the IONSCAN-LS with Autosampler module has been assembled correctly.. Turn instrument on and put into negative ion mode. 3. Verify communication between IONSCAN-LS, Autosampler and operating software. 4. Verify appropriate control parameters for the detection of TNT. Refer to Appendix 5. Allow instrument to come ready and stabilize for approximately 1 hour before proceeding with test. 6. Perform all checks in negative ion mode. 7. Switch instrument to positive ion mode. 8. Verify appropriate control parameters for the detection of diazepam. Refer to Appendix 9. Allow instrument to come ready and stabilize for approximately 1 hour before proceeding with test

9 Version 5.0 Page 9 of 8 TEST LOCATION Instrument underwent Performance Verification as of the date this protocol was performed. Company Name Address Department Building Number Room Date Performance Verification performed Performance Verification Performed by (Name and Signature): Verified PV is Complete by(name and Signature): Date

10 Version 5.0 Page 10 of 8 DESORBER SEAL CHECK PURPOSE To verify that when the IONSCAN-LS performs an analysis and the desorber stage moves up and seals the sample substrate between the desorber and the inlet, a proper seal is obtained. BACKGROUND To analyze a sample, the sample substrate is inserted into the tray on the front of instrument and the slide is moved to the right to introduce the sample into the analyzer. When the analysis cycle starts, the desorber moves up and seals the sample between the desorber heater and the IMS inlet. As the sample is heated the sample carrier gas (clean dry air) sweeps the desorbed vapors into the IMS detector. To provide efficient sample transfer the sample should be properly sealed between the desorber and inlet to ensure that no vapors escape out the side. TEST EQUIPMENT LIST 1. Teflon substrate card assembly with standard Teflon substrate (p/n ) inch calibration tool PROCEDURE This test is performed in negative ion mode only. 1. Remover Inlet cover. CAUTION! INLET IS HOT!. In STANDBY mode, initiate ANVIL CYCLE and select UP position. 3. Using the calibration tool, check gap between desorber and inlet flange. There should be a moderate amount of resistance; however, the bar should still be able to be moved. If an adjustment is needed, turn set screw to the right of desorber, and recycle the ANVIL and place it in the UP position. 4. Repeat until calibration is correct. 5. Allow IONSCAN-LS unit to come ready. 6. Assemble a new Teflon substrate, card and ring. 7. Insert substrate card into IONSCAN-LS sample tray and analyze. 8. Verify that the set screw on the bottom of the transfer line heater block does not interfere with the vertical movement of the sample tray. 9. After the analysis, check for seal on bottom of Teflon substrate. 10. Record below whether the seal on the bottom of Teflon substrate is even and centered on the substrate. If necessary, adjust the mechanical-stop set screw and repeat steps Replace substrate card assembly in tray and run an analysis. During the analysis gently pull on the substrate assembly. It should not be easily removed. RESULTS Is gap correct for inlet/desorber (0.115 )? Is the imprint of seal on the bottom of Teflon substrate (shown in gray below) even and centered on the substrate as shown in the figure below? Was substrate assembly held properly in place during an analysis? Properly Centered Imprint Improperly Centered Imprint

11 Version 5.0 Page 11 of 8 AUTOSAMPLER ALIGNMENT CHECK PURPOSE To verify the accuracy of the autosampler s positional setpoints. BACKGROUND It is critical that an autosampler be able to position itself at various points throughout a run in order for a successful analysis to take place. This test verifies the autosampler s positional setpoints. Once this test is completed, the other qualification tests can be run. TEST EQUIPMENT LIST 1. IONSCAN Autosampler module. 1-mm vial with cap 3. Teflon Substrate 4. Rinse/Waste vials/caps PROCEDURE Note: this test is performed in the negative ion mode only. 1. Place 50 µl of water in a clean, dry autosampler vial, cap the vial and then place the vial in position 1 on the autosampler tray.. Place Rinse and Waste vials with caps in autosampler tray 3. Place Teflon Substrate on sample tray and close 4. Power up autosampler. 5. On autosampler keypad press PROG and select COBRA SETUP. 6. In SETUP Menu, select CONFIGURATION. 7. Select SAMPLE Verify a/s syringe moves to the proper position indicated in the table below. 9. Press ENTER. 10. Repeat steps 6 10 for WASTE, RINSE, INJECT A. Note: If the autosampler is out of position at any of the check points, adjust the setting using the keypad and retest the check point. Be sure that the Right/Left coordinate is the same for all waste and rinse targets. Record any changes to the control parameters in the IM-Station method. RESULTS Target Proper Position Test Result Sample 1 Center of Sample 1 vial Tip of syringe needle must be below the surface of the water, but must not touch the bottom of the vial. Waste Center of Waste 1 vial Vertical Setting = 1000 Rinse Inject A Center of Rinse 1 vial Vertical Setting = 000 Center of Teflon membrane Tip of needle must extend beyond syringe guide, but not contact Teflon substrate

12 Version 5.0 Page 1 of 8 AUTOSAMPLER SYRINGE VOLUME CALIBRATION CHECK PURPOSE To verify the accuracy of the autosampler s syringe volume calibration. BACKGROUND This test verifies the autosampler s syringe volume calibration. It is critical that an autosampler be able to deliver the correct volume of solution in order for a successful analysis to take place. For example, when using a 10-µL syringe, the plunger movement between the zero position and the full-scale position should equal 10 µl, as read from the syringe scale. Once this test is completed, the other qualification tests can be run. TEST EQUIPMENT LIST 1. IONSCAN Autosampler module. 10-µL syringe PROCEDURE Note: This test is performed in the negative ion mode only. With autosampler installed: 1. Power up autosampler.. The gap between bottom of plunger and top of needle(0ul) should be set to smallest possible amount. If an adjustment is needed, loosen the two screws that secure the syringe holder, slide the syringe holder up or down, and re-tighten. Verify Zero position by cycling power on autosampler. 3. On autosampler keypad press PROG and select Cobra Setup. 4. In SETUP Menu, select CONFIGURATION. 5. Select Vol Calib. 6. Press ENTER 7. Verify that the bottom of the plunger is at the 10uL mark on syringe for 100% setting. Press ENTER. 8. Verify that the plunger rises above 10uL mark. Press ENTER then HOLD/STOP when done. 9. Turn autosampler off and on, and verify that the plunger motor can find its home and does not chatter. RESULTS Plunger Position Proper Position Test Result Zero Bottom of the plunger is above 0uL. Smallest gap is desirable. Full Scale (100%) Bottom of the plunger set at 10uL mark. Maximum Bottom of plunger above 10uL line.

13 Version 5.0 Page 13 of 8 AUTOSAMPLER SLIDE TRAY CHECK PURPOSE To verify the autosampler slide drive correctly positions the slide tray above the desorber plate for an analysis. BACKGROUND This test verifies the positioning of the slide tray when the autosampler moves it into position for an analysis. When moved into position, the tray should activate the magnetic switch to initiate an analysis. The tray should also be centered above the desorber plate and below the inlet block. The positioning is determined by the # of slider steps parameter in the A/S general page of the control parameters. This parameter specifies the number of steps made by the stepper motor in moving from the home position to be inserted position. TEST EQUIPMENT LIST 1. IONSCAN Autosampler module PROCEDURE Note: this test is performed in the negative ion mode only. With autosampler installed: 1. Power up autosampler. Place the IONSCAN in Ready mode. 3. Cut a strip of a business card and hold it against the mechanical-stop set screw. 4. Initiate a single injection autosampler run 5. This will bring the slide tray into the analysis position. Verify that: a. The tray does not crash into the mechanical stop. This can be verified by observing no right shift of slide tray upon return to home position after analysis is complete. b. The slide tray gently clamps down on the business card so that there is some resistance when attempting to pull out the card. 6. Record PASS/FAIL in the PV report RESULTS Slide Position Proper Position Test Result Inserted for an analysis About one business card width from the mechanical-stop set screw

14 Version 5.0 Page 14 of 8 NOISE CHECK PURPOSE To verify the IONSCAN-LS detector is operating within the defined acceptance limits for system noise. BACKGROUND Noise is an important characteristic that specifies a detector s performance. Low noise level is especially important when analyzing compounds at low trace levels. IONSCAN detector noise primarily originates from microphonic noise (motion of guard grid relative to collector plate) and preamp noise (resistance noise). The root mean square noise is determined by using a built-im-station software function to measure the root mean square noise in a defined drift time interval. RMS Amp RMS (root mean square) deviation from the mean signal amplitude over all segments of the Seg Range, in the drift time interval specified. P-P Amp Displays the peak-to-peak amplitude of all segments of the range (difference between maximum and minimum of all segments). TEST EQUIPMENT LIST 1. Instrument Manager Software. (IM-Station software). PROCEDURE Negative Ion Mode 1. With slide tray down and no Teflon substrate installed, run three blank samples.. Acquire sample plasmagram with IM-Station software. 3. With built in IM-Station software function, measure RMS and Peak to Peak noise from msec and record in table. Positive Ion Mode 1. With slide tray down and no Teflon substrate installed, run three blank samples.. Acquire sample plasmagram with IM-Station software. 3. With built in IM-Station software function, measure RMS and Peak to Peak noise from msec and record in table. RESULTS Negative Ion Mode Positive Ion Mode Expected Result Actual Result Expected Result Actual Result RMS Amp < 3 du < 3 du P-P Amp < 15 du < 15 du Are noise levels in negative ion mode within specified tolerances? Are noise levels in positive ion mode within specified tolerances?

15 Version 5.0 Page 15 of 8 CALIBRANT ION CHECK PURPOSE To verify that a calibrant peak is present in the correct position in both positive and negative modes. BACKGROUND After the IONSCAN unit has warmed up and temperatures have stabilized, the unit searches for the presence of the calibrant peak before the unit goes into READY mode. The IONSCAN-LS unit uses the calibrant peak position to determine the drift times of all programmed analyte peaks based on the equation below: t anal d K K o = anal t o cal cal d wheret anal d K cal o is the expected drift time of the analyte ion, t cal d is measured drift time of the calibrant peak, K anal are the programmed reduced ion mobility values of the analyte and calibrant peaks. o and Parameters which effect the calibrant ion drift time are drift tube temperature, inlet temperature, drift flow rate, ambient atmospheric pressure and humidity level of the drift gas. All these parameters are either controlled or compensated for. The instrument controls drift tube and inlet temperature and drift flow. An air purification cartridge provides clean dry air for the instrument to use. An absolute pressure transducer determines the absolute pressure that is used to determine the expected position of calibrant. The IONSCAN-LS is designed to operate only when its internal algorithm has identified the calibrant peak. This test will verify that the calibrant algorithm is properly programmed in and the IONSCAN-LS is detecting it within manufacturer s specifications. PROCEDURE Negative Ion Mode 1. Verify IONSCAN entered READY mode within 1 hour.. Record the calibrant installed in instrument. 3. From control parameters, record the calibrant Ko. 4. Run a blank sample and record the FWHM, maximum amplitude, and delta of the calibrant ion peak. The maximum amplitude and delta are taken from the Channel Data summary table. The FWHM is taken from a Gaussian fit of the first segment of the D plasmagram. Positive Ion Mode 1. Verify IONSCAN entered READY mode within 1 hour.. Record the calibrant installed in instrument. 3. From control parameters, record the calibrant Ko. 4. Run a blank sample and record the FWHM, maximum amplitude, and delta of the calibrant ion peak. The maximum amplitude and delta are taken from the Channel Data summary table. The FWHM is taken from a Gaussian fit of the average of the D plasmagram.

16 Version 5.0 Page 16 of 8 RESULTS READY after 1 hour? Calibrant Calibrant Ko Calibrant FWHM (μs) Calibrant Max Amp (du) Calibrant delta (μs) Negative Ion Mode Positive Ion Mode Ready after 1 hour? Calibrant Ko within expected range (See table)? Calibrant FWHM within expected range (See table)? Calibrant Max Amp greater than threshold listed (See table)? Calibrant delta within + 60 μs? Negative Ion Mode Positive Ion Mode Calibrant Ko Range FWHM Range (μs) Max Amp Threshold (du) IBA (Isobutyramide) Nic (Nicotinamide) NBN (4-nitrobenzonitrile)

17 Version 5.0 Page 17 of 8 REACTANT ION CHECK PURPOSE To verify that reactant peaks are present in the correct position in the negative mode. BACKGROUND In the negative mode, a reactant is added via a diffusion source in the sample path to aid in the ionization process. Since the IONSCAN-LS does not actively monitor the reactant level, as it does the calibrant, it is necessary to verify the level to establish that the instrument is operating within specifications. This is done by evaluating the reactant level at the beginning and end of a series of consecutive runs. The IONSCAN-LS must maintain a minimum level over the course of the analyses. PROCEDURE Negative Ion Mode Only 1. Run a blank sample with no substrate present.. Scroll through segments and using the Gaussian fit function, find the maximum amplitude of the reactant peak nearest 7.0 ms. 3. Run 5 consecutive analyses (starting each analysis as soon as the IONSCAN-LS comes READY) with no substrate present. 4. On the last sample, scroll through segments and using the Gaussian fit function, find the maximum amplitude of the reactant peak nearest 7.0 ms. Initial Reactant Amplitude Reactant Amplitude after Sample series Maximum Reactant Amplitude Amplitude Threshold 600 du 00 du Max Amp above threshold?

18 Version 5.0 Page 18 of 8 CARRYOVER CHECK PURPOSE To test for carryover following an injection of a high-concentration standard. BACKGROUND When a high-concentration sample is analyzed, it has the potential to persist in the instrument and contribute to the instrument response observed for the next sample. This is termed carryover. To test for carryover, an analysis of a high-concentration standard is performed, followed by an analysis of a solvent blank. The standard should not be detected when the blank is analyzed. TEST EQUIPMENT LIST pg/µL TNT solution pg/µL diazepam solution 3. Teflon membrane (p/n ) PROCEDURE Negative Ion Mode 1. Prepare TNT solution and 3 hexane blanks in 1-mm amber vials. Cap and place in autosampler tray.. Verify that suitable parameters for an Autosampler Only run are entered in. Refer to Appendix. 3. Run autosampler method of TNT standard followed by 3 blank injections onto Teflon membrane 3 times. 4. Record cumulative amplitude of TNT after each standard and blank run. Positive Ion Mode 1. Prepare diazepam solution and 3 acetone blanks in 1-mm amber vials. Cap and place in autosampler tray.. Verify that suitable parameters for the Autosampler Only run are entered in. Refer to Appendix. 3. Run autosampler method of diazepam standard followed by 3 blank injections onto Teflon membrane 3 times. 4. Record cumulative amplitude of diazepam after each standard and blank run. Note: If the 1 st blank after the TNT or diazepam standard gives no detection, then the remaining two can be skipped. RESULTS Negative Ion Mode, Teflon 500 pg of Sample TNT (CumAmp) A 1 3 Average Positive Ion Mode, HPI 1000 pg of Sample diazepam (CumAmp) A 1 3 Average Blanks (TNT CumAmp) Blank 1 Blank Blank 3 Blanks (diazepam CumAmp) Blank 1 Blank Blank 3 Sum of Blanks (CumAmp) B Sum of Blanks (CumAmp) B % Carry Over: (B/A) x 100 % Carry Over: (B/A) x 100 Is average % carryover in negative mode < %? Is average % carryover in positive mode < %?

19 Version 5.0 Page 19 of 8 LIMIT OF DETECTION CHECK PURPOSE To verify the IONSCAN-LS system is able to detect a minute quantity of TNT and diazepam. BACKGROUND This test verifies the ability of the IONSCAN-LS to detect low levels of a standard. This is accomplished by demonstrating the detection of 5 pg of TNT on Teflon in negative ion mode and 50 pg of diazepam on the HPI in positive ion mode. This is done to test both means of sample introduction. TEST EQUIPMENT LIST 1. Teflon membrane (p/n ). 5-pg/µL TNT solution pg/µL diazepam solution PROCEDURE Negative Ion Mode 1. Place a Teflon membrane in the swipe tray and close tray.. Prepare a 5-pg/µL TNT solution in a 1-mm amber autosampler vial. Cap and place in autosampler tray. 3. Verify that suitable parameters for an Autosampler Only run are entered in. Refer to Appendix. 4. Run a solvent blank. The TNT response must be zero before continuing to the next step. 5. Run autosampler method with 3 replicate injections onto the Teflon membrane. 6. Record if TNT was detected after each standard run. Positive Ion Mode 1. Place a Teflon membrane in the swipe tray and close tray.. Prepare a 50-pg/µL diazepam solution in a 1-mm amber autosampler vial. Cap and place in autosampler tray. 3. Verify that suitable parameters for the Autosampler and HPI run are entered in. Refer to Appendix. 4. Run a solvent blank. The diazepam response must be zero before continuing to the next step. 5. Run autosampler method with 3 replicate injections into the HPI port. 6. Record if diazepam was detected after each standard run. RESULTS Run 1 Run Run 3 TNT signal (Cum Amp) Diazepam signal (Cum Amp) Did the last blank before Run 1 give a response of zero before both tests? Was 5 pg of TNT on Teflon detected in all 3 runs? Was 50 pg of diazepam on the HPI detected in all 3 runs?

20 Version 5.0 Page 0 of 8 DETECTOR LINEARITY CHECK PURPOSE To verify the detector shows a linear response over a working range. BACKGROUND Detectors become non-linear when the amount of the test compound increases above a certain limit. The linearity test is based on a sequence of runs where a TNT solution or diazepam solution is injected several times from vials containing different concentrations using the same injection volume. For the appropriate concentration range, when the instrument response is plotted against the concentration, the points should lie on a straight line. The square of the correlation coefficient, r, of this calibration curve is used to assess detector linearity. Three injections of five standards will be analyzed. TEST EQUIPMENT LIST 1. Teflon membrane (p/n ). 50, 100, 150, 00, and 50 pg/µl TNT solutions 3. 50, 100, 150, 00, and 50 pg/µl diazepam solutions PROCEDURE Negative Ion Mode 1. Place a Teflon membrane in the swipe tray and close tray.. Prepare all TNT solutions in 1-mm amber vials. Cap and place in autosampler tray. 3. Verify that suitable parameters for an Autosampler Only run are entered in. Refer to Appendix. 4. Run autosampler method with 3 replicate injections of each standard onto the Teflon membrane. 5. Record the cumulative amplitude of TNT after each standard run. Positive Ion Mode 1. Verify a Teflon membrane is in the swipe tray and close tray.. Prepare all diazepam solutions in 1-mm amber vials. Cap and place in autosampler tray. 3. Verify that suitable parameters for the Autosampler Only run are entered in. Refer to Appendix. 4. Run autosampler method with 3 replicate injections of each standard onto the Teflon membrane. 5. Record the cumulative amplitude of diazepam after each standard run. Note: Use a suitable program to plot average amplitude versus concentration and to calculate the r values based on the equation y = ax + b. RESULTS Sample Conc. pg/µl TNT on Teflon, Cum Amp Run 1 Run Run 3 Avg. Conc. pg/µl Sol Sol Sol Sol Sol Slope = Intercept = r = Is r > 0.98? Diazepam on HPI, Cum Amp Run 1 Run Run 3 Avg.

21 Version 5.0 Page 1 of 8 PEAK PROFILE CHECK PURPOSE To verify that the peak profile for a compound has the proper appearance time and width. BACKGROUND The peak profile of a standard is an important indicator of optimal performance of the IONSCAN-LS/HPI system. A peak at the characteristic ion drift time for the standard should be detected a certain length of time after the start of the IONSCAN analysis, and the time profile of the peak should have a certain width. This is evaluated by analyzing a 00 pg/ul standard of TNT in the negative ion mode and a 00 pg/ul standard of diazepam in the positive mode. The desorption time at maximum amplitude and number of segments in which the peak is detected are recorded and compared to operational specifications. TEST EQUIPMENT LIST 1. Teflon membrane. 00 pg/µl TNT solution pg/µl diazepam solution PROCEDURE Negative Ion Mode 1. Place a Teflon membrane in the swipe tray and close tray.. Prepare a 00 pg/µl TNT solution in a 1-mm amber vial. Cap and place in autosampler tray. 3. Verify that suitable parameters for an Autosampler Only run are entered in. Refer to Appendix. 4. Run autosampler method that performs three replicate injections using the Teflon membrane. 5. For the third analysis of 00 pg/μl of TNT, record the desorption time at maximum amplitude and the number of segments in which TNT was detected in table below. Positive Ion Mode 1. Verify a Teflon membrane is in the swipe tray and close tray.. Prepare a 00 pg/µl diazepam solution in a 1-mm amber vial. Cap and place in autosampler tray. 3. Verify that suitable parameters for the Autosampler Only run are entered in. Refer to Appendix. 4. Run autosampler method that performs three replicate injections using the Teflon membrane. 5. For the third analysis of 00 pg/μl of diazepam, record the desorption time at maximum amplitude and the number of segments in which diazepam was detected in table below. RESULTS Negative Mode, TNT via Teflon Desorption Max Amp Specified Tolerance s Number of detected segments 5-6 Positive Mode, diazepam via HPI Desorption Max Amp Specified Tolerance s Number of detected segments pg of TNT Pass Specification? 00 pg of diazepam Pass Specification?

22 Version 5.0 Page of 8 INJECTION REPEATABILITY CHECK PURPOSE To verify that IONSCAN-LS repeatability for the analysis of sample aliquots is within acceptable limits. BACKGROUND The injection volume precision is based on a sequence of runs where a TNT standard is used in negative ion mode and a diazepam standard is used in positive ion mode. Each standard is injected 5 times, always with the same volume. The average cumulative amplitude and relative standard deviation (RSD) are determined for each standard, and the RSDs are compared to acceptance criteria. TEST EQUIPMENT LIST 1. Teflon membrane (p/n ). 50 pg/µl diazepam solution pg/µl TNT solution PROCEDURE Negative Ion Mode 1. Place a Teflon membrane in the swipe tray and close tray.. Prepare a 50 pg/µl TNT solution in a 1-mm amber vial. Cap and place in autosampler tray. 3. Verify that suitable parameters for an Autosampler Only run are entered in. Refer to Appendix. 4. Run autosampler method with 5 replicate injections onto Teflon membrane. 5. Record cumulative amplitude of each standard in table below. Positive Ion Mode 1. Verify a Teflon membrane is in the swipe tray and close tray.. Prepare a 50 pg/µl diazepam solution in a 1-mm amber vial. Cap and place in autosampler tray. 3. Verify that suitable parameters for the Autosampler Only run are entered in. Refer to Appendix. 4. Run autosampler method with 5 replicate injections onto Teflon membrane. 5. Record cumullative amplitude of each standard run in table below. RESULTS Sample 1 Sample Sample 3 Sample 4 Sample 5 Average Std Dev Relative Standard Deviation (RSD) Is RSD < 8 % 50 pg TNT Teflon membrane (Cum Amp) 50pg Diazepam HPI port (Cum Amp)

23 Version 5.0 Page 3 of 8 SUMMARY OF PERFORMANCE VERIFICATION Check DESORBER SEAL CHECK AUTOSAMPLER ALIGNMENT CHECK AUTOSAMPLER SYRINGE VOLUME CALIBRATION CHECK AUTOSAMPLER SLIDE TRAY CHECK Negative Ion Mode Positive Ion Mode NOISE CHECK CALIBRANT ION CHECK REACTANT ION CHECK CARRYOVER CHECK LIMIT OF DETECTION CHECK DETECTOR LINEARITY CHECK PEAK PROFILE CHECK INJECTION REPEATABILITY CHECK FINAL CONCLUSION Did Instrument pass all of the tests in the above table? Yes (PASSED QUALIFICATION) No (FAILED QUALIFICATION) Protocol Deviations and/or Comments:

24 Version 5.0 Page 4 of 8 APPENDIX 1 In this appendix the documentation of mathematical or statistical formulas used in the tests described in the previous chapters are discussed. NOISE ANALYSIS During an analysis, multiple scans are co-added to define a segment of analysis and the total number of segments defined by the analysis time. For example a typical scan period is 0 msec, 0 scans are co-added to define segment of analysis (0.4 sec) and the analysis time is 8 seconds giving 0 segments of analysis. The IM-Station software noise analysis feature calculates signal and peak-to-peak amplitude data in the specified drift time interval. A drift time interval at the beginning of the analysis is selected which is free of peaks. The following data is then displayed in the top left corner of the plasmagram: Seg Range: RMS Amp: P-P Amp: Max P-P Seg: Max P-P Amp: Range of segments used in the calculations. RMS (root mean square) deviation from the mean signal amplitude over all segments of the Seg Range, in the drift time interval specified. Displays the peak-to-peak amplitude of all segments of the range (difference between maximum and minimum of all segments). Specifies the segment with the highest peak-to-peak amplitude. Shows the peak-to-peak amplitude of the Max P-P Seg. 3D Plasm agram 40 Peak Height (du) Drift Time (ms) IN THE ABOVE FIGURE NOISE WOULD BE ANALYZED OVER THE DRIFT TIME INTERVAL FROM 5.0 TO 5.3 MSEC. EACH OF THE LINES IN THE FIGURE IS A SEGMENT OF ANALYSIS. DATA SET OVER WHICH NOISE ANALYSIS IS PERFORMED: aij signal (du) for segment j at point i in drift time s j Number of scans per segment for segment j n, n 1 Range of indices ( i ) over which RMS and Peak-to-Peak noise is to be calculated k, k 1 Range of segments ( j ) over which RMS and Peak-to-Peak noise is to be calculated Define:

25 Version 5.0 Page 5 of 8 u b b j = ( n n + 1) u i= u1 a j, min ij j 1 ij = Min( a u ) For n1 i n = Max( aij u ) For n1 i n j, max j σ j = u [ aij u j ] i= u1 ( n n + 1) 1 Therefore, the RMS Amp is σ = k j= k σ j s j 1 k j= k 1 s j Max P-P Amp: Maximum Peak-to-Peak Amplitude: b = Max b [ b ] P P j, max j,max For j= k 1, k Max P-P Seg: Segment associated with Max P-P amplitude kmax = Value of j on which b p-p is based Further: min Min( b j, min ) max Max( b j, max b = b = Therefore, P-P Amp is b abs = ( b max bmin ) )

26 Version 5.0 Page 6 of 8 REGRESSION ANALYSIS The linearity test uses regression analysis during the evaluation. Linearity is derived from the linear function: Let: N = number of discrete observations X i = independent variable, i th observation Y i = dependent variable, i th observation Determination of coefficients: X Y b N = = 1 X i N N = i = 1 N Y i i N { ( X i X )( Yi Y )} i= 1 = N ( X i X ) i= 1 a = Y bx Regression Coefficient: r = Y X = a + bx N { ( X i X )( Yi Y )} N N ( X ) ( ) i X Yi Y i= 1 i= 1 i= 1 DETERMINATION OF INJECTION REPEATABILITY N = number of replicate samples A = Measured value associated with i th sample i Average A Standard Deviation SD = N i= = 1 N A i N ( Ai A) i= 1 N 1 (Results are a small sampling) Relative Standard Deviation RSD SD 100 = A

27 Version 5.0 Page 7 of 8 APPENDIX QUALIFICATION CONTROL PARAMETERS AUTOSAMPLER MODULE Autosampler Only Mode, Negative and Positive Ion Modes (Values listed are for Cobra II Autosampler, with values for Cobra I Autosampler in parentheses) Start Sample Vial: As placed #Sample Rinses 0 Pre-Dispense Delay (s) 0 End Sample Vial: As placed #Sample Pumps 4 Post-Disp. Delay (s) 7 (5) #Repetitions/Sample As needed Sample Fill Rate % 40 (85) Retract Delay (s) 0 #Rinses/Solv #1 5 Sample Dispense Rate % 100 Start Delay (s) 0 #Rinses/Solv# 0 Syringe Offset (μl) 0 Dispense to Target A Rinse Volume (μl) 5 Pre-Fill Air (μl) 0 Min. Sub. Cool Time (s) 10 Rinse Fill Rate % 50 (85) Mid-Fill Air (μl) 0 Oper. Mode No HPI Spike Volume (μl) 0 Post-Fill Air (μl) 0.5 (Continuous) Sample Volume (μl) 1.0 Post-Fill Delay (s) 0 HIGH PERFORMANCE INJECTOR, Autosampler Only UseHPI be set to OFF, which places the HPI in StandBy CRITICAL IONSCAN PARAMETERS, Negative and Positive Ion Modes Analysis delay following start of desorption 0.05 s Scan Period 0 ms Maximum analysis duration 1.00 s No. of co-added scans/analysis 10 Detection Algorithm: Channel Ko Vblty Blok Th Amp Th FWHM Seq Hits TNT μs 1.5 du 30 du 330 μs 1 diazepam μs 1.5 du 30 du 410 μs 1

28 Version 5.0 Page 8 of 8 REVISION HISTORY 1. Version 1.0, Effective Date February 19, Based on a rework of Version.1, Installation and Operation Qualification for IONSCAN-LS With Autosampler Module, Effective Date December 13, 00.. Version.0, Effective Date July 7, Removed Calibrant and Reactant Ion Check. - Removed Data Acquisition tables from Test Procedure - Added option to use Teflon membrane filters 3. Version 3.0, Effective Date, February 0, Based on a rework of Version 5.0, Installation and Operation Qualification for IONSCAN-LS With Autosampler Module, Effective Date March 4, Version 3.1, Effective Date, July 1, Adjust Ranges for Calibrant Ion Check. 5. Version 3., Effective Date, August 19, Based on rework of Version 5.1, Installation and Operation Qualification for IONSCAN-LS With Autosampler Module, Effective Date August, Version 4.0, Effective Date: September 10, Based on a rework of Version 1.50, Manufacturing Operational Qualification: IONSCAN-LS with High Performance Injector (HPI) and Autosampler Module, Effective Date August 5, Version 4.1, Effective November, Changed parameters and specifications for Calibrant Ion Check, Limit of Detection Check, and Injection Repeatability Check. 8. Version 4., Effective October 1, Corrected errors in Injection Repeatability Check 9. Version 5.0, Effective October 16, Based on rework of Version.0 Performance Verification: IONSCAN-LS with High Performance Injector(HPI) and Autosampler Module, Effective Date October 3, 007.