182_0027_01
Contents
1. ccceceee eee ern eees Deviations Y N Comments 14 of 17 PQ procedure LC 100 pump edition 1 Verified by customer ooococcoccccocconconccnonnnos Deviations Y N Comments Chapter 4 PQ certification 15 of 17 CHAPTER 4 PQ certification The Operational Qualification has been carried out in accordance to the PQ procedure and has been carried out to the satisfaction of both parties All tests as described in this document have been successfully completed and all results are within specifications Pressure pulsations at 20 FS L_ passed _ failed Flow deviation at 20 FS _ passed failed Flow deviation at 40 FS L_ passed failed Executing technician Technician name amp signature Company Date Customer authorised to sign Name amp signature Verified by customer ooococcoccccocconcnnccnnnnno Deviations Y N Comments 16 of 17 PQ procedure LC 100 pump edition 1 Comments Verified by customer ooococcoccccocconconccnonnnos Deviations Y N Comments Chapter 5 Non conformance record 17 of 17 CHAPTER 5 Non conformance record Any case of non conformance found during the PQ procedure should be documented and signed for acceptance or corrective action taken Table Ref Non conformance and action taken Signature Sign executing customer technician 4 Verified by customer ccceceee eee e2. Edition 1 2006 ALEXYS LC 100 Pump PQ ALEXYS 182 0027 Table of contents 1 of 17 Identification The undersigned engineer certifies that he she is trained and qualified to perform an PQ on the LC 100 pump Performer eee Company Title Anted Leyden representative trained and qualified to perform PQ procedures The undersigned reviewer customer accepts that the above mentioned engineer is trained and certified to do PQ OQ on all Antec Equipment Reviewer Customer eee EEE EN Name Signature Initials Company s s s aeee i MA ee ee g Owner designated authorized person Verified by customer ooococcoccccocconcnnccnnnnno Deviations Y N Comments 2 of 17 PQ procedure LC 100 pump edition 1 Instrument LC100 p n S n EEE ees L Pump head Analytical Micro Manufacturer Antec Leyden Supplier Date of delivery Warranty until Test equipment AC 100 Part number Serial number Calibration date or Line recorder Model eee Serial number ss Calibration date Flow meter Model Serial number Calibration date ALEXYS data system Revision Verified by customer ooococcoccccocconconccnonnnos Deviations Y N Comments Table of contents 3 of 17 Table of contents Identification 1 Instrument 2 Test equipment 2 Table of contents 3 Introduction 5 PQ for LC 100 pump 7 Test configuration 7 Pressure pulsations test 8
3. 100 MM 009 16 0024 Specified 3 00 0055 15 9907 Test result passed dir bi Pressure pubsation 1 mi per min lal u O Girod 7 Fig 4 Example of results Residual P pulsations Pressure pulsations P must be smaller than lt 3 9 If the instrument fails test first check for leakage or air in sys tem if pump head is assembled correctly and all critical parts check valves pistons etc are in tact If the problem remains consult the test amp readjustment section in the service manual When using a line recorder to record the pressure profile please follow the procedure below to determine the residual pressure pulsations 1 Connect a line recorder to the analogue pressure monitor 1mV MPa to monitor the pump pressure Set the compressibility Kappa to 45 Set TIME CONST to HIGH 2s Set the flow rate to 1 mL min Press lt R S gt to start the pump Record the pressure signal for 10 minutes via the pressure moni tor output at 1 mL min Do pr nN Verified by customer o ococccococcccccncoccncnconnnos Deviations Y N Comments Chapter 2 PQ for LC 100 pump 11 of 17 7 After 10 minutes stop the flow and record the pressure signal for 5 more minutes to determine the pressure at 0 mL min Pressure pulsations Average Pmax Pressure MPa Pmin JAI time min Fig 5 Pressure signal with lines indicating Pmax and Pmin 8 When using a line recorder determi
4. RIESEN Deviations Y N 8 of 17 PQ procedure LC 100 pump edition 1 All tests described in the PQ procedure are based on a LC 100 with ana lytical pump head In case of a LC 100 with micro pump head all flow rates mentioned in the tests should be changed accordingly The flow rate of the micro head should correspond to the same flow rate in FS Full Scale as the analytical pump head The PQ tests are performed at 20 and 40 FS which corresponds to the following flow rates Analytical o Mao 20 S 1 gt 200 aa 40 FS 2 mL min 400 uL min Pressure pulsations test Before starting the Pressure pulsation test download the latest version of the zip file LC100_P test_revxx zip from the Antec web site at http www antecleyden com The zip file contains ALEXYS system and method files to perform the test and an Excel worksheet LC100_P test_revxx xls were the residual pressure pulsation is calculated auto matically Store the ALEXYS system and method files in the corresponding directories in the ALEXYS program files directory 1 Open the ALEXYS system file LC100_P test_xxxyy smt 2 Connect AC 100 controlled by ALEXYS software to the ana logue pressure monitor 1mV MPa to monitor the pump pres sure 3 Set the compressibility Kappa to 45 4 Set TIME CONST to HIGH 2s 5 Set pump to REMOTE 6 Start run in Alexys Subsequently a run will start of 15 min utes The first 10 minutes the pressure
5. signal is monitored at a flow rate 1 mL min After 10 minutes the flow is stopped auto matically The program will continue measuring for 5 minutes in order to determine the pressure at 0 mL min A typical pres sure profile obtained with such test is shown in figure 2 Verified by customer ccccee cece scene eens Deviations Y N Comments Chapter 2 PQ for LC 100 pump Verified by customer ooococcoccccocconcnnccnnnnno Comments Pressure MPa 10 a b 0 5 10 Time min Fig 2 Calculation of pressure pulsations P 9 of 17 Export the Pressure data to ASCII in ALEXYS using the option export raw data to txt in the file menu Do not include the re tention time for export only the pressure data Open the generated txt file and select all Pressure data Sub sequently copy the data into the second column pressure MPa in the Excel worksheet LC100_P test_revxx xis El Microsoft Excel LC100_P test_rev01 xls al ES gt e Beveiliging Fy 3a N BD Bestand Bewerken Beeld Invoegen Opmaak Extra Data Venster Help Adobe PDF lelx a 100 B OSE SRY tua KD Cu r time min pressure MPa 0 002 0 003 0 005 0 007 0 008 0 010 0 012 0 013 0 015 0 017 0 018 0 020 0 022 a oes A 44 pl Pressure pulsation 1 mL permin 4 Gereed Pre
6. Flow rate deviation test 12 PQ certification 15 Comments 16 Non conformance record 17 Verified by customer ooococcoccccocconcnnccnnnnno Deviations Y N Comments 4 of 17 PQ procedure LC 100 pump edition 1 Verified by customer ooococcoccccocconconccnonnnos Deviations Y N Comments Chapter 1 Introduction 5 of 17 CHAPTER 1 Introduction This document describes the Operational Qualification procedure as ad vised by the manufacturer It is a result from our interpretation of many regulations and laboratory practises In addition feedback from users and representatives helped us to finalize this procedure A complete PQ for the LC 100 pump consists of two qualification checks The following test procedures should be executed to check if the pump operates within specifications Flow rate deviation measurement Residual pressure pulsation measurement It may be necessary to re adjust the pump in case the performance speci fications are not met For detailed information about pump readjustment consult the LC 100 service manual p n 182 0020 All qualification checks have to be approved or should be marked n a if not applicable Any deviation observed must be documented in the non conformance record All relevant documents regarding this operational qualification must be filed together in one location As regulations and customer requirements may change manufacturer reserves t
7. ctly at the moment that the liquid meniscus in the pipette passes the 0 mL line 6 Calculate the actual flow rate Flow rate 4 mL stopwatch time min In case of using a calibrated flow meter complete 5 flow meter readings and calculate the average Subsequently calculate the flow deviation Flow deviation actual flowrate set flow rate 100 set flow rate 7 Repeat the flow deviation measurement three times the Relative Standard Deviation RSD of a triplicate Verified by customer oocooccccccccccccccocnocncss Deviations Y N Comments PQ for LC 100 pump 10 13 of 17 measurement should be lt 1 If this is not the case please repeat all three measurements The average flow deviation n 3 should be smaller than 3 Repeat this experiment at 2 mL min Measure the flow deviation three times the Relative Standard Deviation RSD of a triplicate measurement should be lt 1 If this is not the case please repeat all three measurements The average flow deviation n 3 should be smaller than 3 Also at a flow rate of 2 mL min perform a triplicate the flow deviation should be smaller than 3 If the instrument fails test first check for leakage or air in system if pump head is assembled correctly and all critical parts check valves pistons etc are in tact If the problem remains consult the test amp readjustment section in the service manual Verified by customer
8. he right to introduces changes without prior notice For details on functionality operation and theory reference is made to the instrument users manual Verified by customer ooococcoccccocconcnnccnnnnno Deviations Y N Comments 6 of 17 PQ procedure LC 100 pump edition 1 Verified by customer ooococcoccccocconconccnonnnos Deviations Y N Comments Chapter 2 PQ for LC 100 pump CHAPTER 2 PQ for LC 100 pump Test configuration 7 of 17 Mobile phase Degassed 4 filtered HPLC grade water Piston wash HPLC grade water Capillary 1 16 PEEK restriction capillary 127 um 1 D Flow meter calibrated flowmeter or graduated analytical pipette amp stopwatch P system pressure between 100 200 bar P signal Analog pressure output of the pump monitored using an AC 100 and ALEXYS data system soft ware sampling frequency 10 Hz or line recorder Pmonitor LC 100 time constant high 2 sec kappa 45 compressibility ds Restriction Pressure signal Capillary de Time const 2s Flowmeter AC 100 Fsampling 10 Hz On Pump Degasser 0 2 um filter IN u HPLC grade water Fig 1 Test set up for measuring flow rate deviation amp pressure pulsation Before running a PQ test the pump should be running for at least 5 minutes under the specified test conditions Verified by customer Comments is EEE
9. ne the average maximum and minimum pressure values at 1 mL min as depicted in figure 5 Draw straight parallel lines through minimum and maximum Sub sequently determine c c Pmax Pmin 9 Calculate the residual pressure pulsations in the following way see figure 2 P c 100 a b Where c Pmax Pmin MPa or4o a b Actual system pressure average pressure at 1 mL min average pressure at 0 mL min Pressure pulsations P must be smaller than lt 3 Verified by customer cccee cece ee eeee ees Deviations Y N Comments 12 of 17 PQ procedure LC 100 pump edition 1 Flow rate deviation test 1 Set the flow rate to 1 mL min and check if purge valve is closed 2 Connect the inlet of the graduated analytical pipette to the outlet of the restriction capillary using a short piece of silicon tubing see figure 6 Or connect the restriction capillary to a calibrated flow meter 3 Press lt Run Stop gt to start the pump Correct volume reading from the pipette is at the lowest point of the meniscus Silicone tubing restriction capillary Fig 6 Flow measurement with graduated 5 mL pipette 4 Measure the flow rate with the pipette using the following procedure start the stopwatch exactly at the moment that the liquid meniscus in the pipette passes the 4 mL line for a good reading it is important that the pipette is kept perfectly vertical 5 Stop the flow rate exa
10. rn eees Deviations Y N Comments
11. ssure MPa Deviations Y N Fig 3 Spread sheet to calculate the Residual P pulsations P 10 of 17 PQ procedure LC 100 pump edition 1 The Residual P pulsations P will be automatically calculated in the Excel worksheet ER Microsoft Excel LC100_P test_revOlsds 5 x E gestand Deyeran Deekj Jrroegen Opmask Mira Dita yeratar pl Adobe POF 218 xj DSB GAY IDAS nr BIAHTU BBimom OB Arial un DIU EE _ A ER G33 v 631 632 100 A B c D E F H Fi 1 zu 2 time min pressure MPa 3 0 002 15 02 Pressure pulsations pump 182 000 1 mLimin 4 003 16 1228 5 ow 16 0533 0 6 om 16 0465 7 0 008 1 Fi 7 14 8 010 16 0008 3 001 15 9391 12 10 013 16 0235 p 1 0 0 16 0196 10 12 0017 15 906 g 13 0018 1 g 14 000 15 9794 15 15939 16 023 15 9192 4 17 0 15 9156 18 0027 15 911 19 0008 15 881 2 050 15 8Y a 21 032 15 4 10 1 2 10 15 97 23 0035 16 0715 ume min 24 0 097 16 116 25 038 16 1356 040 16 1585 F 002 16 1743 P at O mL min b 0 28 Mpa 2 003 16 1681 Average pressure at 2 mUmin t 1 9 min a 15 78 Mpa 29 oss 16 1701 Pmax arg max pulsation 1 1 9 min 15 59 Mpa SD 0047 16 1567 Pmin avg min pulsation 1 1 9 min 1558 Mpa 31 0 048 16 1046 Pulsations peak 10 peak c Pimax Pmin 4 STOEV 0 40 Mpa 32 0060 16 0402 Pressure Mpa ab 16 05 Mpa 0 052 16 0241 Residual pulsations chab
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182_0027_01