WARNING: Contact Kaiser prior to installing ic Raman 4.1 to verify system compatibility.
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1 In-situ Spectroscopy Dear Customer, ic Raman TM 4.1 Release Notes Thank you for purchasing ic Raman TM 4.1, the simply powerful software package for select Kaiser Optical Systems RamanRxn Systems analyzers. Everything you need to install and run ic Raman TM 4.1 is stored on the installation media. Contents of the Installation Media - ic Raman 4.1 software (AutoRun.exe) - ic Raman 4.1 Release Notes (this file) - ic Raman 4.1 Installation Guide - ic Raman 4.1 Documentation Portfolio (PDF file) WARNING: Contact Kaiser prior to installing ic Raman 4.1 to verify system compatibility. Installation Guide and System Requirements Please install ic Raman 4.1 according to the installation guide which can be found on the installation media. This also describes the minimum PC requirements to install and run ic Raman 4.1. User Guide and Help File The ic Raman 4.1 Help file is available from the software and can be printed by the user from the User Guide PDF included in the documentation portfolio. To access the context-sensitive Help from a specific place in the software, click in the software window and then click F1 on your keyboard. Customer Support If you encounter any issues with ic Raman TM 4.1, please don t hesitate to contact your sales representative or service engineer, or contact us at: support@kosi.com for RamanRxn Systems analyzers or software support
2 Feature Comparsion Table Key features of ic Raman 4.1 compared with earlier versions and Kaiser s HoloReact software: Easy Data Collection Feature Wizard-guided experiment setup reduces errors and de-mystifies spectroscopy Templates allow reuse of all settings from previous similar experiments Live experiment toolbar consolidates key status and control functions Referee data from HPLC or other methods can be easily captured and used to fit Raman trends to quantitative concentrations Long experiments can contain multiple phases with different sampling intervals allowing for efficient analysis of long experiments. Kaiser Holo React ic Raman v2 ic Raman v3 ic Raman v4.1 X X X X X X X X X Multiple vessel monitoring X X X Large value display let's you monitor key parameters from across the room or under the fume hood X X X Auto collection mode allows non-experts to gather optimized data without manually setting exposures Intuitive Information Analysis Linked views simplify analysis and highlight data relationships ConcIRT Live! Automatic reaction information generation X X + X On-the-fly data treatments Event linked annotations X Auto component profiling functional group based monitoring X User defined trends tailored information Annotation improvements easy to add, move edit and display in different ways X + Import spectra data files from other sources (spc) X Univariate modeling ic Quant multivariate modeling tool option X Appending, merging, and trimming experiments X Import Mettler Toledo WinRC MTE files X X X 2
3 Kaiser ic ic ic Feature Holo Raman Raman Raman React v2 v3 v4.1 Improved single sample analysis functionality X X + Drag-and-Drop Trends Between ic and icontrol 4.x X X X Import Trends from any ic/icontrol 4.x Experiment File Support for ConcIRT Pro module for analyzing data from multiple experiment or multiple techniques Data Treatments applied to reference spectra in experiments Fast Results Reporting X X X X X X X X Data export & import fast and easy X Auto export of spectra or trend data to csv or spc files during experiment Integration with icontrol for automated lab reactors X X Single-click report generation to MS Word X X X New data tab shows trend values for all selected spectra Reporting to XPS read-only format with no need for MS Word to be installed Compatiblilty X X X X X X GAMP and 21 CFR Part 11 compatible X X Windows Vista 32-bit compatible X X X Windows 7 32-bit compatible X X X ic Raman Office compatible with 64-bit Windows 7 X X X = Supported feature + = Supported feature with enhancements X = Not supported 3
4 These release notes summarize incremental changes in ic Raman TM. Issues Addressed in Service Pack Version 4.1 SP2 ic Raman Office Support for 64-bit version of Windows 7 Operating System ic Raman 4.1 supports the 64- bit version of Windows 7 for ic Raman Office installations. Any computer that will be connected to an instrument must use a 32-bit operating system due to current constraints with the device drivers. Issues Addressed in Service Pack Version 4.1 SP1 Full Support for 32-bit versions of Windows 7 and Vista Operating Systems ic Raman 4.1 fully supports the 32-bit versions of Windows 7 and Vista as well as Windows XP for both instrument control and office versions. Install Analyzer Control Update Kaiser has released an update that corrects averaging of multi-channel wavelength calibrations for RamanRXN2, RamanRXN3 and RamanRXN4 multi-channel instruments. This update is included in this service pack. NOTE: This update is installed automatically during a full install of ic Raman 4.1, If ic Raman 4.1 is already present and you re only installing the service pack, then the installation of the Analyzer control update should be coordinated with Kaiser customer service. Enable Compatibility with New ic FBRM 4.2 ic FBRM 4.2 was built using a newer version of the Microsoft.NET framework than ic Raman 4.1. This service pack has been updated to ensure full interoperability between ic Raman 4.1 and ic FBRM 4.2. Resolved Occasional ic Raman Starting Issues Sometimes a failure to open TCP channel for Application Interoperability functions caused ic Raman to not start. This was rare and the root cause of such a failure is yet unclear, but we believe it s something specific to the individual computer configuration. This has been remedied by catching and ignoring the error, allowing ic Raman to complete its startup without Application Interop capabilities. If the error occurs, the user will be notified that Application Interop features may not work and they may not be able to fully share data with other ic software packages like ic FBRM or icontrol. 4
5 Enhancements for Version 4.1 Support for MultiProbe and MultiVessel Instruments ic Raman can now support multiple probes from one computer (historically referred to as multichannel capability in Kaiser literature). Each probe or reactor has its own experiment document so each can be started and stopped independently and have different data acquisition settings and sample intervals. ic Raman uses a scheduling algorithm to efficiently share the instrument between the different experiments. Auto-mode for Data Collection Auto collection mode allows non-experts to gather optimized data without manually setting exposures. The user simply specifies the desired target exposure time and ic Raman will automatically invoke an Auto-expose whenever needed. This target time can be changed any time during an experiment. A manual collection mode is also available that gives the user full control of the exposure settings. Support for Auto-Cal TM and Cal-Check TM For instruments equipped with internal calibration both Cal-Check TM and Auto-Cal TM are now supported. This functionality, when enabled, allows the instrument to periodically check it s laser frequency and wavelength calibration status and if necessary re-calibrate the instrument. The Cal- Check TM and Auto-Cal TM execution frequency is defined by the user. When the last calibration is greater than the user-defined calibration date or time frequency, the instrument will automatically execute a Cal-Check TM and Auto-Cal TM sequence before the next spectrum is taken. Manually Sampled Experiment For at-line applications and analytical labs, the user can elect to create an experiment that is not based on a predefined acquisition schedule and instead manually collect a sample on demand. All Data Treatments and other experiment features behave the same as with a scheduled experiment. Append To Experiment It is now possible to append additional samples to an existing experiment file. This is particularly useful with the Manually Sampled Experiment feature. For example, in an at-line application that involves taking a sample once a day, it is possible to track all the daily samples in a single file. Data Table There is a new data table view that shows the numerical values in each trend for all pinned spectra. 5
6 Import Trends from any ic/icontrol 4.x Experiment File All ic and icontrol 4.x applications now use a common data file format to allow for even better data exchange. All ic and icontrol applications now have the ability to import trends from any ic/icontrol data file. Drag-and-Drop Trends Between ic and icontrol 4.x For users working with multiple ic and/or icontrol 4.x applications, it is now possible to drag and drop trends between any such applications running on the same computer. In the case of trends from a live experiment, the trend will continue to update in the application it is dropped into. Enhancements to Smoothing and Normalization Data Treatments The maximum number of smoothing points is no longer fixed at 25. The maximum now depends on the spectrum s resampling interval to provide a maximum smoothing window of no less than 30 cm -1 Raman Shift. Normalization now supports the optional selection of a single baseline point. Automatic Scaling of ConcIRT LIVE! Input Data Based on Exposure Time If the Normalization data treatment is not enabled, the system will automatically scale the ConcIRT LIVE! input data based on each spectrum s exposure time. This is necessary because ConcIRT LIVE! did not work optimally when the exposure time changed during the course of an experiment. Data Treatments Now Applied to Reference Spectra in Experiments Any reference spectra added to an experiment, as well as those created by ConcIRT LIVE!, will have the same data treatments applied as the spectra that were collected from the instrument. This maintains data integrity by keeping all treatments the same for all spectra used in an analysis and also allows for easier comparison when math functions, like 2 nd derivative, are applied. Note that spectra copied from an experiment into a spectra library will always maintain any data treatments. Annotate Points or Peaks in the Spectra Viewer Users can label peaks or points in a pinned or reference spectrum in the Spectra Viewer pane. The annotation defaults to the wave number, but the user can select an applicable functional group (if available) instead or enter their own text for the label. User-Defined Trends in Result Sets Previously, user-defined trends were only available for Experiments. This feature has been extended to also permit trend math in Result Sets. 6
7 Pin Multiple Spectra at One Time The user can now select multiple samples in the Event log and pin/unpin the selected samples all at once. Quantitative Methods in Sample Library Previously, quantitative methods could be used to create trends in an experiment, but it was not possible to execute a quant prediction against single samples. The Sample Library document has been extended to support Univariate and Multivariate quantitative methods for this purpose. ic Quant New Features The optional ic Quant package has been enhanced to implement the audit trail logging and tamper detection for 21 CFR Part 11 electronic records. The workflow for calibrating and validating a model is simplified and combined with model calibration. Users can now flag a sample as an outlier in the Model Data table and the sample is excluded from model development. It is now possible to display all PLS loading factors in the spectra viewer. For easy reference, Outlier Limits now displays the 95% confidence limit for Mahalanobis distance and F-Test Statistic. The goodness-of-fit R 2 values for the training data, test data, and cross-validation are now displayed on the Actual vs Predicted charts to provide additional diagnostics information. ConcIRT Pro Module Support With a ConcIRT Pro license installed, users can analyze reaction data using the ConcIRT algorithm post process. The ConcIRT Pro module is designed to analyze reaction data from one experiment or multiple experiments from one spectroscopy, or two experiments with two spectroscopies combined (such as Raman and IR, or Raman and UV-VIS). Users can also manually select the number of components to calculate as well as provide reference spectra or trends as additional inputs for ConcIRT Pro analysis. One-Click Reporting to Microsoft Word One-click reporting is available now for all ic Raman document types Experiments, Result Sets, Sample Libraries, Univariate and Multivariate models, and ConcIRT TM Pro documents. The report is a Microsoft Word document that can be edited, saved, and printed by the user. One-Click Reporting to XPS In addition to sending reports to Microsoft Word, version 4.1 also allows reports to be sent directly to an XPS document. XPS (XML Paper Specification) was developed by Microsoft to provide a read-only definition for document layout and formatting (similar to what an Adobe PDF provides). 7
8 Users can now generate non-editable reports using XPS, and they can also create and view reports even if they do not have Microsoft Word installed on the PC. The XPS reader software is included with Microsoft DotNet 3.0 (this is a free add-on that is installed with many software packages, such as ic IR, and is part of the standard Vista operating system). Enhanced Surface Viewer Printability The surface viewer is now saved as an image and copied with a higher DPI to enhance printability. The axis labels are also rendered with better clarity. This enhanced image is available when reporting to XPS or MS Word as well as from the copy option in the Surface Viewer pane. Support for Windows Vista 32-bit Operating System ic Raman 4.1 is compatible with the Windows Vista 32-bit Operating System as well as Windows XP. Integration with Kaiser s Analyzer Control 5.0. ic Raman integrates the latest release of the Kaiser s Analyzer Control 5.0 device driver to communicate with Raman instrumentation. Improved Performance with New Experiment File Format The new experiment file format allows for more efficient access to the raw data, which results in faster user interface responsiveness and faster processing of data treatments. 8
9 Known Issues No. Issue Description and Workaround 1. Multi-variate Opening Issues Multi-variate models saved with this service pack release may fail to open on the original, unfixed release ( ) The solution to this issue is to upgrade all installations of ic Raman 4.1 to the service pack release. 2. FB35287 New Experiment Wizard Probe Type Probe Type shown in New Experiment Wizard may incorrectly show Unknown. It is not known how common this issue is and whether the issue is specific to certain instrument types. It has been reported that the correct Probe Type is shown in the Configure Instrument dialog. Reconfiguring the instrument may fix this. 3. Intermittent Reconnection with Instrument If Communication or Power Is Disrupted The software does not gracefully handle communication or power disruptions. If the disruption occurs during a live experiment, the experiment will go to a failed state. 4. ConcIRT Component Names Can Change During Experiment During a live experiment, the number of components identified by ConcIRT and their component names might change due to a change in significance. In all cases, the recommended action after a communications or power disruption is to shut down both the hardware and software, and then restart the hardware and then the software. If the disruption caused a live experiment to fail, the experiment can be resumed by selecting the Append option in the New Experiment Wizard. This 'component swapping' behavior will not be present if users wait to turn on the 'ConcIRT' option after the experiment is complete. This issue was also present in previous versions of ic Raman but has been considered a more significant issue now that live trends can be used to control reactors with the icontrol software. For advanced users, an auto-naming option can be enabled for ConcIRT. The system attempts to name ConcIRT components after reference spectra and/or referee trend data provided by users. The system-provided names are for information only. Audit messages are displayed 9
10 No. Issue Description and Workaround to indicate what ConcIRT components are named after certain reference source and the associated confidence level. Users are advised to check the audit messages and determine whether to accept or reject the system names according to their process knowledge. 5. Univariate Component Peak Definitions If you delete the peak associated with a component in the model builder, the model viewer will not update the regression results until a new peak is selected. 6. Model Diagnostics are not Cleared when "Auto-select" is Unchecked and the Model is Calibrated Certain ic Quant 1.0 models will not display Model diagnostics information in the Quantitative Analysis task pane when they are initially opened. 7. Data Acquisition Stops on the Transition to Daylight Savings Time The Trend Viewer expects time to advance monotonically. If a live experiment is running at 2am Sunday morning on the one day a year when time moves backward, data acquisition will stop at that point. 8. High Slippage in Multiple Experiments May Result in Uneven Numbers of Samples Ideally, in a high slippage situation, the slippage is not always distributed To force an update of the model viewer, create a new peak and assign the new peak to the component. This is because the latest ic Quant module has combined calibration and validation steps. The workaround is for users to save the model in the latest.icmodel format and click the 'Calibrate' button to calibrate the model. Model diagnostics information will be displayed correctly in the Quantitative Analysis task pane. The workaround if you need to run an experiment over this weekend is to adjust the Windows property to disable the feature that would Automatically adjust clock for daylight saving changes. You can then reset this option after your experiment completes. The user will be notified before starting an experiment if significant slippage is predicted. It is best if the user reduces the slippage by adjusting the sample intervals before starting the experiments. 10
11 No. Issue Description and Workaround evenly across all running experiments. This can result in a few more missed samples than predicted for some experiments. 9 Problems with low-to-high experiments imported from SPC files in Version 3.0 In Version 4.1, the import of SPC data has been fixed to force the data to be high-to-low, but for experiments imported from SPC file in version 3.0, if the SPC files were defined with X values going from low-to-high, the resulting ic Raman experiment would also have X values going from low-to-high. Peaks would then also be defined low-to-high in these experiments. There are a number of issues when using these Version 3.0 low-to-high experiments in Version 4.1: a) ConcIRT will not execute properly on the low-to-high experiment. b) Peaks profiles defined as low-to-high that are copied into a high-to-low experiment may be calculated incorrectly or may throw exceptions. For the issue of ConcIRT not executing on the low-to-high experiment, the workaround is to simply re-import the data using the original SPC files in Version 4.1. This will result in a high-tolow experiment that ConcIRT will handle correctly. For the issue where low-to-high peak profiles are copied into a high-to-low experiment, it is simplest to manually edit the peaks to be highto-low. 11
12 Enhancements for Version 3.0 Experiment Phases ic Raman supports varying sample interval times throughout the course of the experiment. With this feature, samples can be collected more frequently during the fast parts of the reactions, and more slowly during the slow parts of the reaction. The Start Experiment wizard includes a new Experiment Duration page to create the phases. Experiment Templates The user can now apply experiment templates when creating a new experiment. An experiment template is any previously created experiment file. When applying an experiment template to a new experiment, the template s Peak Definitions, Data Treatments, Reference Spectra, and Phase definitions are copied to the new experiment before it starts. Automatically Adjust Exposure Times The user now has the option to allow ic Raman to automatically invoke an Auto-expose whenever the sample interval time changes or when the camera gets close to saturation. The user can specify a Minimum and Maximum Total Exposure time, and the system will use this information and the desired Sample Interval to calculate the appropriate total exposure time and number of scans. Enhanced Live Experiment Tool Bar ic Raman includes an all new Live Experiment Toolbar when running experiments. This toolbar maintains the Pause/Resume and Quick annotation features of the previous edition, while adding advanced functionality. The Toolbar has timers to track the experiment Elapsed Time, time until the Next Measurement, and the Time Remaining in the experiment. A button on the Live Experiment toolbar allows the user to change the Exposure Settings of paused experiment including switching between Automatic and Manual adjustments of the exposure times. Also, the sample interval and phases can be edited from the Toolbar without pausing the experiment. Record Referee/Offline Data Users can record peak data from HPLC s or other offline referee data into ic Raman so it can be correlated with spectra data. During the experiment, the user can record a Chromatography Sample from the Live Experiment Toolbar. The actual offline data can be entered at any time and is saved with the ic Raman experiment. 12
13 User Defined Trends The User Defined Trends Task Pane gives the user the ability to perform certain math operations on existing trends in their experiments. In addition to the basic math operations, the User Defined Trends Task Pane has functions to calculate % Yield and % Conversion. Fit Referee Data With User Defined Trends, users can scale a relative trend (ex. ConcIRT, peak profile, etc.) to quantitative data from HPLC or other offline analytical data sources. The function calculates the linear equation correlating the relative trend to the chromatography data (based on a least squares fit). This linear equation is then applied to each point in the relative trend to scale to the quantitative data. ic Quant Every ic Raman 3.0 is shipped with METTLER TOLEDO s quantitative analysis module, ic Quant. ic Quant incorporates the univariate modeling capabilities from ic Raman 2.0 and optionally allows users to create powerful and versatile multivariate models. Integration with icontrol RC1e, ic IR and ic FBRM ic Raman experiments can be coordinated with experiments in icontrol RC1e 3.3 rev 1. icontrol can choose templates, start experiments, and copy trend data from ic Raman. Similarly, trend data can easily be shared between ic Raman and other ic products like METTLER TOLEDO s ic IR and ic FBRM. Integration with Kaiser s Analyzer Control ic Raman integrates the latest release of the Kaiser s Analyzer Control device driver to communicate with Raman instrumentation. 13
14 Enhancements for Version 2.0 Easy Start Experiment Wizard The Start Experiment Wizard guides the user through all the necessary steps to start an experiment in ic Raman. The wizard helps the user name the experiment, collect reference spectra, focus the instrument, and set the exposure parameters. The wizard will not allow the user to start an experiment if the CCD camera is not at its setpoint temperature. It will also not allow the user to start an experiment if the wavelength or laser calibrations have not been completed. Univariate Modeling and Analysis ic Raman include the creation and use of univariate models as part of its standard features. With the univariate model, the user can correlate concentration data with peak values to create a linear model. This model can then be applied to existing experiments and new experiment for concentration prediction. Pearson s Baseline Correction Gerald A. Pearson at the University of Iowa published a general baseline recognition and flattening algorithm in This algorithm is built into ic Raman and can be applied to both experiment spectra and univariate model spectra. Peak Calculations (Height, Center, Area, Width) The software supports the definition of 4 peak types, Peak Height, Peak Center, Peak Area, and Peak Width. For each of these peak types the user can choose from 3 baseline options, No Baseline, Single Point Baseline, or Two Point Baseline. ConcIRT LIVE Relative concentration profiles are calculated by ConcIRT LIVE for products, intermediates and starting materials. ConcIRT LIVE is especially valuable for trending chemical species that have overlapping peaks. ConcIRT LIVE uses a type of mathematical algorithm known as curveresolution. Curve-resolution algorithms have the capability to group wavenumber values that change absorbance intensity in the same manner. For each group, ConcIRT LIVE calculates the associated component spectrum and relative concentration profile. As each new reaction spectrum is acquired, ConcIRT LIVE re-analyzes all the reaction spectra and updates the individual component spectra and profiles. Thus, the calculation results evolve as the reaction proceeds and additional components such as intermediates are detected. Note, for ic Raman data, ConcIRT LIVE is most effective when the data is normalized against a known peak. 14
15 Spectra Library Documents with Drag & Drop Spectra Libraries are documents that can be used to store spectra. They are opened as tabbed windows just like experiments and result sets. This allows a user to open multiple spectra library documents simultaneously, drag and drop spectra between documents and to open or create a new spectra library without requiring a device to be connected. Solvent Subtraction in Spectra Libraries Solvent subtraction is available in Spectra Libraries as well as experiments. Easy to Add Annotations During live experiments, a Quick Annotation toolbar is available. The annotation will be associated with the time at which you press the Enter key. You can add annotations at other times from rightclick (context) menus in the Event Viewer and Trend Viewer controls or by pressing the F5 function key. Annotation Markers The position of Annotation markers in the Trend Viewer control can be moved by dragging the marker. Just right-click on the marker and select Move Annotation from the context menu to enable dragging. Toolbar View Option After opening a document, the toolbar gives a series of options that can be easily used to arrange the layout of the form s controls. The options under the view menu are customized to the document type. Clickable Legends Clicking on an item in the legend of the Trend Viewer or Spectra Viewer selects the corresponding trend/spectrum. Grid Panel Including Y-Axis Assignments The grid panel of the Trend Viewer and Spectra Viewer provides additional information about the selected trend/spectrum. You can also rename, change color or assign a different Y-Axis to a data series from this panel. Automatically Export Spectra/Trend Data during Experiment While running an experiment, the User can elect to have the system export a Grams SPC formatted file, or a CSV file for every new acquisition. In addition, the User can elect to have each new trend 15
16 data point exported to a file. The target directory and base file name are User configurable. This option is available under the Tools menu. Drag & Drop Reference Trends You can drag & drop reference trends into experiments from other experiments or result sets. High Contrast Charts The Trend Viewer and Spectra Viewer controls support a context menu option for High Contrast Mode which switches to a black background instead of white and draws thinner lines on the chart. Smart Copy As Text in Trend Viewer The user can use the Copy As Text feature of Trend Viewer to allow for easier data analysis using programs such as Microsoft Excel. Pin/Unpin Samples The Trend Viewer provides the ability to select a point in time for an experiment and also provides a Pin function that acts on the sample associated with the selected time. Thus, the user can select a point on the trend and Pin the associate sample in the Spectra Viewer, Surface Viewer, and Event Viewer. 16
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