Waters 2695D Separations Module

S U P P L E M E N T A L R E L E A S E N O T E S Waters 2695D Separations Module Firmware Update Version 2.04d Firmware Update Version 2.04d Information This firmware update incorporates improved connectivity to various types of dissolution baths from Hanson Research Co and Distek Inc. This eliminates the display of comm error messages when the 2695D is configured for control by Empower. These Supplemental Release Notes assume that the 2695D about to be upgraded with this firmware is already at V2.03. If this is not the case, contact Waters for a copy of earlier Supplemental Release Notes for information pertinent to that version. The information below is to be considered as an update to these manuals; Waters Alliance Dissolution System Operator s Guide, Waters 2695 Separations Module Operator s Guide and Waters 2695 Separations Module Quick Start Guide. The information below is in addition to these guides. Contents of this Release Waters 2695D Separations Module Firmware Update Version 2.04d Kit consists of: Installation Notes 2695D Firmware Update Disk, 1.44 MB, 3.5 inch Supplemental Release Notes (this document) Quality Documents Information Letter System Qualification Letter The 2695D Separations Module firmware is updated by copying the software from the Waters 2695D Firmware Update Disk to the system FLASH ROM chips using the floppy disk drive on the front panel of the unit. Attention: If the floppy disk drive unit has not been used within the last month, it is advisable to exercise it before proceeding with the update by exporting a Separation Method or Sample Set. Since there is a possibility of a corrupt Method or Sample Set do not then import it. Attention: To prevent a mandatory service call to replace ROM chips, make sure that you do not power off the Separations Module during the software update procedure, unless specifically instructed to do so. 716002385, Rev. B Waters, Alliance, MassLynx and Millennium and are registered trademarks, The Science of What s Possible, PerformancePLUS and Empower are trademarks of Waters Corporation. All other trademarks are the sole property of their respective owners. Copyright 2007 Waters Corporation Page 1 of 8

To install the Update Version 2.04d: 1. Insert the Waters 2695D Firmware Update Disk into the floppy disk drive on the front panel of the 2695D. 2. Power on the 2695D. The display will show A reprogramming utility was found. Press Enter to replace the current program. Press Clear to cancel and resume. Press Enter. 3. The display then shows Reading load utility from disk Please wait. 4. After the memory has been erased, the display shows, Loading V 2.04d x percent complete and DO NOT TURN POWER OFF! TURNING POWER OFF NOW WILL MAKE YOUR SYSTEM UNUSABLE! The x percent complete represents the percentage of the new program that has been loaded and proceeds from zero (0) to one hundred (100) percent. At this point, the update disk begins a check of the file system and of the configuration and/or methods. 5. The display shows Checking the file system.., then shows Checking the configuration and methods.., and then shows No errors were found. and Press Enter to continue. Press Enter. This update assumes the 2695D being updated already has Version 2.03 firmware, which prevents creation of corrupted methods. After steps 1 through 5 the 2695D is now ready to complete the software update and the display asks; 6. Do you want to install the available methods? Press Enter for YES. Press Clear for NO. These methods are the Separation Methods and Sample Set AutoStartPLUS described above. Note: If you do not load these at this time you can Import them later (see the Waters 2695 Separations Module Operator s Guide). If you have previously loaded the AutoStartPLUS methods, they will be overwritten if you choose YES. If you press Enter the display shows Installing Methods and when complete shows Installing Version 2.04d, Clear the display shows Installing Version 2.04d, 7. When the display shows, Installing Version 2.04d, Memory will be erased and reprogrammed! and the commands Press Enter to continue. and Press Clear to Abort., you should press Enter. 8. Last Warning! If you proceed, DO NOT turn off power! is displayed, followed by Press Enter to continue. Press Clear to Abort. Press Enter. 9. The display then shows Checking Program Integrity.Please wait. After a few minutes the display then shows, Erasing Memory..Please wait and DO NOT TURN POWER OFF! TURNING POWER OFF NOW WILL MAKE YOUR SYSTEM UNUSABLE! 10. After the memory has been erased, the display shows, Loading V 2.04d x percent complete and DO NOT TURN POWER OFF! TURNING POWER OFF NOW WILL MAKE YOUR SYSTEM UNUSABLE! The x percent complete represents the percentage of the new program that has been loaded and proceeds from zero (0) to one hundred (100) percent. 11. Once the entire program has been loaded, the display shows Program Load Complete and instructs Remove Floppy Disk and cycle power. Remove the disk, turn the Separations Module power switch to the OFF position, wait approximately 5 seconds, and then turn the power switch to the ON position. The Separations Module will go through its initialization sequence. Progress of initialization is viewable in the banner area of the display and when complete, the banner area displays Idle. 12. Verify 2695D Separations Module firmware revision (2.04d), creation date (Mar 30 2007 13:57:20) and checksum (A6B55089H). From the 2695D Main Screen choose Diag, then Other Tests and scroll down to Firmware Checksum. The checksum is listed, and if internally correct, is followed by the letters OK. Note: If your instrument Page 2 of 8

is in a regulated environment and the firmware checksum and version number are confirmed, then the Installation Qualification is complete. Refer to Instrument Qualification section of this Release Note. Items Documented Prior to Product Shipment (version 2.04d) Improved Connectivity to Various Types of Dissolution Baths Version 2.04d firmware supports the control of up to two baths from the following manufacturers: Hanson Research Co. Model SR8-Plus (firmware version 3.10) Distek Inc Model 2100C (firmware version 2.41) and Model 6100 (firmware version 2.15) Note: The 2695D can be connected to only one type of dissolution bath at a time. Provision has been made for the future control of baths from Varian Inc and Erweka AG. The requisite interface modules for these vendors were not available at the time of this release. Configuring the System for Empower Control Problems with the status display when the 2695D is under Empower control have been corrected. The 2695D displays the correct status information when Controlled by Empower is selected in the configuration window. Items Documented Prior to Product Shipment (version 2.04) Improved checking of vial position prior to injection Version 2.04d firmware incorporates improved checking of vial position prior to injection of sample from that vial; this helps to confirm that the correct vial is being injected per programmed sample set sequence. This is accomplished via an improved carousel movement algorithm in conjunction with a smaller carousel encoder slot width parameter (now at 0.5 instead of 0.8 previously). After the carousel has been engaged and homed, all subsequent carousel movements are monitored using the carousel encoder slot sensor. If the slot sensor signature is incorrect, the carousel is rehomed and the move is retried. If the move fails a second time the "Carousel malfunction" alarm is raised. Between multiple injections from the same vial the carousel encoder slot sensor is monitored. If the carousel moves off the vial slot between injections it's re-homed and repositioned back to the correct vial. If the re-homing or repositioning fails they are retried. If the second attempt to re-home and reposition the carousel fails the "Carousel malfunction" alarm is raised. Instrument Qualification The 2695D V2.04d firmware provides improved checking of vial position prior to injection of sample from that vial, as noted above. These corrections and added functionality do not impact the actual functional performance of the instrument with respect to qualification, as long the stroke volume is manually set according to the required flow rate. Therefore, installation of 2695D V2.04d firmware in an instrument having the minimum hardware requirements is not considered to be a major product change and will not require total instrument or system re-qualification. It is imperative to set the appropriate stroke volume for any and all existing methods before using them. Refer to the table shown on page 3 of these Supplemental Release Notes. If your Separations Module-based system is in a regulated (GXP) environment, Waters recommends that you perform the following procedures to verify consistent instrument/system performance before and after loading this firmware update. Page 3 of 8

1. Run system suitability analysis (on a well characterized standard) before and after installing this firmware update. Compare the results. If the before and after results agree to within the analytical method specifications, then the continued performance of the instrument/system is verified. 2. Record the check sum result to verify the firmware has loaded correctly. 3. Record the new firmware revision number in your GXP documents. Items Documented Prior to Product Shipment (Version 2.03 and earlier) Correct Use of Diagnostics Screens Whenever an operator (FSE and/or customer) is within Alliance diagnostics, it is very important that ALL diagnostic screens be exited before any external control (Millennium 32, Empower, MassLynx, etc.) is allowed. Failure to do so may cause unexpected behavior. Adding New Sample Vials during a Run To minimize the risk of a vial being missed when adding new vials to a carousel while the instrument is processing a sample set, the following guidelines should be followed; When adding samples, wait at least 30 seconds after an injection is made (i.e. wait until the run time displayed on the front panel, or within the controlling software, is greater than 30 seconds). Minimize the length of time that the sample compartment door remains open. It is also good practice to make sure the sample compartment door is closed when time injection commands (selecting vial, washing the needle, drawing sample, etc.) are in the process of being carried out. Re-initialization of the System It is good practice to re-initialize the instrument at least once a week: when all instruments (the 2695D and Detectors) are power-cycled (i.e., turn "off", wait for a minimum of 1 minute and then turn "on") on a regular basis), each instrument will perform a complete system initialization, including internal diagnostics and verifications. This helps ensure that the mechanical and electrical components as well as internal firmware, synchronize for proper operation. Minimizing Dust Ingress It is important that the optical sensors on a number of internal components not get covered in dust. If the instrument is in an area that is prone to accumulation of dust, Waters recommends the use of a Dust Filter Kit to minimize dust accumulation inside the instrument. This Filter Kit (includes floppy drive cover and rear panel plug) is standard on all 2695D s manufactured since December 2004, and are available as kits for earlier 2695D instruments. Improved Check Valve Performance As of June 2005, all 2695D Separations Modules and 2695D Performance Maintenance Kits have been delivered with PerformancePLUS check valves as standard; this check valve features a 1/8" ruby ball/sapphire seat. The original check valve (1/16" ruby ball/sapphire seat) is available as an option, along with 2 versions of ceramic check valve (ceramic ball and ceramic seat, either 1/8 or 1/16 ball diameter). Page 283 of the Appendix B (spare parts) of the 2695 Separations Module Operator s Guide should be amended as follows; The spare part number for the PerformancePLUS check valve is 700000254. The optional 1/16" ruby ball/sapphire seat check valve spare part number is WAT270941. Page 4 of 8

The optional 1/16" ceramic check valve spare part number is 700002761. The optional 1/8" ceramic check valve spare part number is 700002399. Import of the Default Separation Method The 2695D Default Separation Method is resident in the 2695D. It is not appropriate to attempt to import a method named Default, even if it was exported from the same unit. The creation of an invalid method may occur. System Control by Millennium 32 Chromatography Data System As stated in the Operator s Guide, Any parameter values not explicitly set in the Millennium instrument method automatically take on the values in the Default method in the Separations Module. These include: 2695D-software-recognized column selection valves (3 column, 6 column and 2 column regeneration valves) Needle wash time selection of normal, double and extended Selection of Post-sample Wash parameter within a dissolution method Selection of Syringe Speed parameter within a dissolution method If you wish to modify these values, verify that Idle is displayed in the banner area before you edit the Default Separation Method or DefaultDM for a dissolution method. When the 2695D is under Millennium control, and actively running a sample, do not edit the 2695D Default Method or DefaultDM. It is an improper operation to edit a running method via the 2695D front panel when under Millennium Quick Set Control. Modification to Automatic Stroke Volume Functionality The information in Figure 6-3 ( Mobile Phase Screen ) in the Operator s Guide is incorrect. The figures below show the settable Stroke Volumes: The lowest recommended flow rate for a 2695D is 0.05 ml per minute, with an upper limit of 5.0 ml per minute. Composition Change Restriction The composition can no longer be changed from the Status page while the 2695D is under remote control. Optional PerformancePLUS Injector Needle In section 7.3.4 and Appendix B, Table B-2, of the Operator s Guide, the part number for the optional PerformancePLUS nickel/cobalt needle is incorrectly listed. The correct part number for the optional PerformancePLUS nickel/cobalt needle is 700001247. Page 5 of 8

Carryover Specification in Appendix A In Appendix A, Table A-5, of the Operator s Guide, the specification for sample carryover is listed incorrectly as <0.1% UV detection (254 nm) or 20 ml, whichever is greater. The correct specification for sample carryover is <0.1% UV detection (254 nm) or 20 nl, whichever is greater. Diagnostics Screen and the C/D Ratio The 2695D Diagnostics Screen is shown below. Figure 8-3 in the Operator s Guide is incorrect. Whenever an operator (FSE and/or customer) is within 2695 diagnostics, it is very important that ALL diagnostic screens be exited before any external control (Millennium 32, Empower, MassLynx, etc.) is allowed. Failure to do so may cause unexpected behavior. Autosampler Parameter Values The 2695D Autosampler Screen is shown below. Figure 6-6 in the Operator s Guide is incorrect. The operator has the ability to choose one of three options for needle wash duration as shown below. Normal, the default value, was the standard, non-programmable value in previous versions of software. The needle wash portion of the injection cycle operates for approximately 13 seconds when Normal is selected. In cases when excess carryover is seen, you may choose either Double (2X) or Extended (4X) to increase the length of time the needle is washed. The needle wash portion of the injection cycle is increased either by an additional ~ 13 seconds or by an additional ~39 seconds, respectively if Double (2X) or Extended (4X) is chosen as compared to Normal. Page 6 of 8

Column Screen The 2695D Column Screen is shown below. Figure 6-7, in Section 6.2.4 of the Operator s Guide is incorrect. If a 2695D-software-recognized column selection valve (3 column, 6 column and 2 column regeneration valve) is not installed, the Equilibration field is grayed-out and not available. If one of these valves is installed, and the Column Selection field is set to a choice other than No Change, the Equilibration field becomes active. The operator has the ability to specify an equilibration time that will be applied whenever the application of the Separation Method involves a change in the column switch position. The screen below describes this behavior and is available when the user presses the help key (?) with the cursor positioned in the Equilibration field. 2 nd Generation Column Heater & New Column Heater/Cooler Subsequent to publication of the 2695 Operator s Guide Rev. B (P/N 71500269502, Rev B), Waters has replaced the original Column Heater with a 2 nd generation Column Heater and introduced a new Column Heater/Cooler Module. Both of these modules are shipped with a copy of the Alliance Series Column Heater and Column Heater/Cooler Operator s Guide (P/N 71500049202, Rev A). The following notes update the column heater references within Rev. B of the 2695 Operator s Guide; Page 48 - under Power Supply should read The 2695 Separations Module is factory equipped with a 600 watt (W) power supply. This provides immediate compatibility for the addition of a column heater. Note that the Column Heater/Cooler module has its own built in power supply. Page 49 - under Column Heater should read The column heater allows you to maintain the column at temperatures from 5 C above ambient (minimum of 20 C) to 65 C. The upper temperature limit is 65 C and not 60 C. Page 52 the drawing shows the original column heater compartment. Refer to Alliance Series Column Heater and Column Heater/Cooler Operator s Guide (P/N 71500049202, Rev A). Page 78 under Adding Hardware Options, the Column Heater/Cooler should be added. Page 140 description against Column Temp parameter should also include Column Heater/Cooler. Page 143 description against Equilibrate parameter should also include Column Heater/Cooler. Page 157 text within the Initial Conds paragraph should also refer to Column Heater/Cooler. Page 7 of 8

Page 180 within Table 6-7, the following should be noted; The value range of 20 C (ambient + 5 C) to 60 C in 1 C increments for the Column Temperature Target Parameter pertains only to the original Column Heater. Refer to Alliance Series Column Heater and Column Heater/Cooler Operator s Guide (P/N 71500049202, Rev A), page 60 for values associated with the 2 nd Generation Column Heater and the Column Heater/Cooler. Page 184 text within the Action Parameters Table 6-10 should also refer to Column Heater/Cooler. Page 189 text within the 2410 and 410 Parameters Table 6-14 should also refer to Column Heater/Cooler. Page 233 text within the Other Diagnostics Screen under Section 8-3 should also refer to Column Heater/Cooler. Page 243 text within the Other Diagnostics Tests Table 8-3 should also refer to Column Heater/Cooler. Refer to Alliance Series Column Heater and Column Heater/Cooler Operator s Guide (P/N 71500049202, Rev A), page 72. Page 256 text within Section 8.4.11 under before you perform the test should also refer to Column Heater/Cooler. Page 257 text within Section 8.4.121 under before you perform the test should also refer to Column Heater/Cooler. Page 258 for information concerning the defrosting procedure of the Column Heater/Cooler, refer to Alliance Series Column Heater and Column Heater/Cooler Operator s Guide (P/N 71500049202, Rev A), page 72. Page 265 - text within the Chromatography Troubleshooting Table 8-9 should also refer to Column Heater/Cooler. Page 276 and 277 for information concerning the physical and performance specifications of the Column Heater/Cooler, refer to Alliance Series Column Heater and Column Heater/Cooler Operator s Guide (P/N 71500049202, Rev A), pages 81 to 83. Note that the original Column Heater, the 2 nd Generation Column Heater and the Column Heater/Cooler all share common dimensions. Page 280 - within Table A-6 the column heater specification should read 20 C (5 C above ambient) to 60 C, in 1 C increments for the original Column Heater only. The 2 nd Generation column heater specification should read 20 C (5 C above ambient) to 65 C, in 1 C increments. The upper temperature limit is 65 C and not 60 C. The Column Heater/Cooler specification should read 4 C (15 C below ambient) to 65 C, in 1 C increments. If a column heater (without cooler) is heating and a set point lower than the current temperature is entered, the column heater is commanded to stop heating. It will only resume heating when the temperature falls below the new set point. Subsequent to publication of the Alliance Series Column Heater and Column Heater/Cooler Operator s Guide (P/N 71500049202, Rev A), some improvements have been made to the Column Heater & Column Heater/Cooler modules that improve consistency of temperature control. The location of the temperature sensor has been changed within both the Column Heater & Column Heater/Cooler modules; the sensor is now located centrally within the compartment, between the 2 column mounting rails. This change has been in place since December 2005 for the Column Heater/Cooler and since June 2006 for the Column Heater. Earlier modules can be updated to current standard please contact your local Waters office. Some changes have been incorporated into the door of the Column Heater & Column Heater/Cooler modules; the door contains an improved hinge mechanism and new foam inserts to better facilitate column outlet tubing connections to the detector module. This new door has been shipping as standard on both Column Heater & Column Heater/Cooler modules since May 2006. Earlier modules can be updated to current standard please contact your local Waters office. The original 120mA fuse used inside the Column Heater & Column Heater/Cooler modules has been changed to a 160mA fast acting fuse; this fuse has Waters part number 330000127. Page 8 of 8