1593587 en NIRWare 1.
Imprint Product Identification: Operation Manual, NIRWare 1.5 11593587 en Publication date: 04.2013, Version A BÜCHI Labortechnik AG Meierseggstrasse 40 Postfach CH-9230 Flawil 1 E-Mail: quality@buchi.com BUCHI reserves the right to make changes to the manual as deemed necessary in the interest of experience; especially in respect to structure, illustrations and technical depth. This manual is copyright.
Contents 1. Welcome 1 2. Introduction 3 2.1. 2.2. 2.3. NIRWare Management Console ................................................................ 4 2.1.1. Application Designer ..................................................................... 4 2.1.2. Sample Management .................................................................... 4 2.1.3. Administrative Tools ...................................................................... 4 2.1.4. Security Designer .................................
5.5.1. Development of an application for Content Uniformity Testing (CUT) of Solid Dosage Forms..................................................................90 5.6. Using applications and calibrations in Life Cycle state "Created" .........102 5.6.1. Application for development (Life Cycle state "Created") .........102 5.6.2. Application in routine use (Life Cycle state 'Approved') ............104 5.7. Importing license protected applications (e.g. BUCHI or Ingot PreCalibrated Applications) ............
6.7. 6.8. 6.9. 6.10. 7. NIRWare Operator 7.1. 7.2. 7.3. 7.4. 7.5. 7.6. 7.7. 7.8. 8. 8.2. 305 Introduction Operator .............................................................................305 Tab Overview .........................................................................................307 Operator Wizard .....................................................................................309 Select Application ............................................................................
1. Welcome Dear customer, Thank you for choosing the BUCHI NIRFlex N-500 FT-NIR spectrometer with the NIRWare Software Suite. We are sure that it will be a valuable tool for solving your analytical requirements. NIRWare has been developed to design your complete NIR applications, to manage your samples (spectra and reference values) and to customize the user interface for routine work.
2 Welcome NIRWare 1.
2. Introduction NIR spectroscopy covers a wide variety of applications, which in turn place diverse demands on operation and calibration. Especially the software of the NIR system must take this point into account and should therefore be of modular and flexible design. For years, the BUCHI NIRCal Chemometric Software has proven its worth as a powerful and flexible software package for creating calibrations. It has been substantially expanded and improved for the new generation now available.
2.1. NIRWare Management Console NIRWare Management Console is related to Microsoft Management Console (MMC). It hosts all Snap-In Modules of the NIRWare Suite except NIRWare Operator. The Management Console can be configured for different Users or User Groups. Closely linked to the NIRWare Software Suite is the NIRCal Chemometric Software. 2.1.1. Application Designer The design of an application predominantly defines how the operator has to perform a specific analysis.
Life Cycle Templates Different Life Cycle Templates can be selected for configuration. In order to simplify the use of the lifecycle model there are three pre-defined lifecycle model templates: Unregulated, ER (Electronic Records), and ERES (Electronic Records/Electronic Signatures), which cover different requirements. The lifecycle involves all software modules, applications and calibrations.
and period of validity of the passwords. A password history check and an automatic logout function are implemented as well. 2.1.5. Library Designer For identity checking at goods receipt, it is not always necessary to apply chemometric procedures such as cluster analysis or SIMCA. Often, a direct comparison of spectra will also produce unambiguous results directly and require fewer reference samples than in chemometric models.
2.3. NIRCal 5 NIRCal 5 is the proven chemometric software. It is database oriented and includes an integrated user management feature. Calibrations of NIRCal 5 are incorporated directly in the application with the NIRWare Application Designer. NIRCal is a chemometric software to analyze measured spectra and to develop calibrations.
3. General work flow In the development of a routine application, different software modules are used. The application development cycle is summarized below: 1. Develop an application with NIRWare Application Designer 2. Measure the calibration samples with NIRWare Operator 3. Assign reference values to each sample with NIRWare Sample Manager 4. Analyze spectral data and develop a calibration with NIRCal 5 5. Assign the calibration to the application with NIRWare Application Designer 6.
The shown roadmap illustrates the workflow under the Life Cycle Template "Unregulated". The Life Cycle Template "ER" (Electronic Records) and "ERES" (Electronic Records/Electronic Signatures)", usually used in pharmaceutical industry, contains an additional step. An application or calibration is set in the life cycle state "checked" for test runs before it can be set to the "approved" state, which is used for released applications and calibrations. 10 General work flow NIRWare 1.
4. Software Installation This chapter explains how to install or update the NIRWare Software Suite and introduces the license philosophy. 4.1. Important Notes A new version of NIRWare cannot be installed at the same time as a previous version. In case of an existing installation of NIRware it will be removed by the setup of the new version. An existing NIRWare database from a prior installation will be upgraded. Therefore it is recommended to backup all needed data prior to installation. NIRWare 1.
The InstallShield Wizard with the list of software parts to be installed opens. Click ‘Install’ to start the installation. Wait during installation of .NET 4.0 and MS SQL Server 2008 R2… After automatic installation of .NET 4.0 and MS SQL Server 2008 R2, click OK to confirm the warning that any older NIRWare version will be automatically uninstalled when installing NIRWare 1.5. Follow the installation wizard and use the default options.
Click on green check mark to confirm or let the timer run its course. Ensure the setup finishes successfully and no error message is shown. Click Yes to confirm to restart your system 4.4. What has been installed The following three shortcuts have been added to the desktop for all users (Windows 7 and Windows Windows 7: These entries have been added to the start menu for all users Windows 8: These tiles have been added to the Start screen of the user who has done the installation NIRWare 1.
The above tiles are only added to the Start screen of the user who installed NIRWare 1.5. Other users do not see automatically any NIRWare 1.5 tiles on their start screens. Users who want to add NIRWare 1.5 tiles to their start screen have to select the desired apps (right click on the start screen and click on ‘All apps’, or press the keys Windows-Q to open the search app view) and pin them to the start screen: Right click on the app and then click on ‘Pin to Start’ Example: Pin NIRCal to Start.
These three aplications are stored by default here: C:\Program Files\Buchi\NIRSolutions BUCHI Database Manager Windows 7: This application can be started using the Start menu: Start > All Programs > Buchi > Database Manager > Buchi Database Manager Windows 8: This application can also be started using the Start screen, if it has been pinned to the Start screen. Alternatively, just start typing the name of the application on the Start screen until you see the desired application selected.
4.5.2. BUCHI Database Manager Please uninstall the existing software version manually. For this purpose: Windows 7: Start > Control Panel > Uninstall a program Windows 8: On the Start screen start typing control panel until you see the app Control Panel selected, then hit the enter key, then click on Uninstall a program Select BUCHI Database Manager from the list and click Uninstall 4.5.3.
Windows 8: If .NET 3.5 is not enabled then Windows asks to enable it. To download and install this feature, an internet connection is needed. Click OK to confirm the Setup Support Rules Select the instance BUCHISQLSERVER and click Next to remove it NIRWare 1.
Click Select All to select all features and click Next to remove them Click Next to confirm Removal Rules Click Remove to confirm beeing Ready to Remove Click Close to finish the uninstallation of SQL Server 2008 R2 4.5.4.
4.7. Software Registration The registration form can be saved as an *.xml file and needs to be sent to your BUCHI contact person, for example as an email attachment. The form can be opened using the "NIRWare Management Console" Menu: Help > Software Registration... or clicking the button "Register..." on the startup of a trial version. The registration form: Please fill out the bold mandatory fields.
4.8. - Activating the licenses To activate the demo mode start the Management Console and select Demo mode. When the software is in demo mode it is valid for 60 days. To activate the software and make it a fully valid version, licenses are required. Licenses are provided by BUCHI. The form can be opened using the “NIRWare Management Console” --> Menu: Help > Software Registration... or clicking the button “Register...” on the startup of a trial version. 20 Software Installation NIRWare 1.
5. Tutorial 5.1. Logon The NIRWare Management Console, the NIRWare Operator and NIRCal 5 are protected by Logon. After NIRWare is installed, four default users are provided, which do not require password entry at the beginning. Just type in the corresponding user name and click the green checkmark to log on.
Click on the icon behind the Password line. The logon window is extended: Enter your new password in the corresponding line and confirm it below. Then click the check mark button to save your changes. 5.3. Creating a qualitative application 5.3.1. Introduction This tutorial describes how to create an application for identity check. As an example, the NIRFlex N-500 is used with the measuring cell Solids and the Vial Add-on. 22 Tutorial NIRWare 1.
The application should be able to check the identity of four different types / forms of sugar: Fructose (= fruit sugar), lactose (= milk sugar), sucrose (= crystal sugar) and fine sucrose (= sugar powder). Note that sucrose and fine sucrose are of the same chemical composition and only differ in particle size. The process of creating a ready-to-use NIR application requires reference samples. These are samples of doubtless identity and quality.
The upper part of the scheme includes all steps regarding the reference samples. The middle part shows the processes for designing an application for routine use. The last part indicates the routine use, which is the goal of the development process. In the following, we will use the term ‘Operator user’ for a user account from the user group ‘Operators’, and ‘Administrator’ for one belonging to the user group ‘Administrators’.
Left-click on ‘Application Designer’ in the tree menu on the left, then on the subtitle ‘New’. A dialog appears for creating a new application Fill in the application name and all other requested information into the white fields on the right side. The ‘SOP Text’ will later on tell the Operator how to perform the actual measurement, so it is important to give a complete description which is easily understandable. Click the Save icon to save the new application to the database.
Open it by double-clicking on its field in the tree menu, or by clicking once on the plus-symbol in front of it. Then select its subtitle ‘Operator Configuration’. You will now see only one field for the SOP text. To see all of the information fields on the right, click on the ‘Show Advanced Settings’ icon in the menu bar . The fields on the right are greyed out, indicating that they cannot be changed right now. To change the settings, first click on the ‘Edit Data Set’ icon .
You can now make changes to all white fields. For our example, we just change the ‘Number of measurement sequences’ from 1 to 3. This will cause a triplicate measurement of every reference sample, which creates more variation in the spectra set later used for calibration. Thus, we will get more robust calibrations. Save all changes you made to the database by clicking the respective icon . The fields are greyed out again afterwards, indicating successful saving.
Start the operator software by clicking the corresponding icon Click the ‘Select application’ icon: 28 Tutorial and log on as an operator user. . NIRWare 1.
Select the application you created for spectra measurement of the calibration samples. Notice the access restrictions for the Operator: He can only see and use ‘Approved’ applications. Click on the ‘New’ icon of the ‘Measurement description - Batch’ field to create a new batch. NIRWare 1.
Type in the name of your batch, then click on the green check mark button. Then type in the information for AnalysisID and Sample names. Note: For ‘real’ applications, use ‘speaking’ names that precisely identify each sample just from the name. Also think of using the autoname functions described in the NIRWare documentation. If you have filled in and checked all information, prepare the samples for measurement (i.e. place all vials in the Autosampler) and press the green arrow button.
First, the external reference is measured. Then the samples are measured. All spectra are displayed in one window. Since the intensity of the external reference is so much higher than that of the sample spectrum, the latter are just a flat line on the x-axis. NIRWare 1.
To have a closer look on the sample spectrum, deactivate the check box for ‘External Reference’ below the graphic. The vial autosampler will automatically continue with the next samples after confirmation of the following message: 32 Tutorial NIRWare 1.
Turn the sample vials and click on the green check mark icon to start the next measurement sequence. The spectra shown below are all from identical fructose samples. The strong variations along the y-axis (shift) are typical for reflectance measurements of solids and result from variations in particle size and –orientation, and other sources of variation, e.g. thickness of the glass vials. NIRWare 1.
To zoom into the spectrum, click and hold the left mouse icon while dragging the cursor. 34 Tutorial NIRWare 1.
The selected frame will be magnified: To change back to full view, click on the symbol with the magnification lens above the globus. NOTE In the Operator it is possible to delete spectra, but only right after they have been measured and if they are not used for prediction with a calibration. This might be desirable if e.g. a vial was not correctly positioned in the Autosampler.
After completion of the measurement of your reference samples, switch to the NIRWare Management Console to continue with the next step in application development: the assignment of properties and property values. In this case, it means to add the substance identity behind each spectrum. 5.3.4. Defining a property and a property value After the spectra of the reference samples have been measured, the properties (here: identities) have to be connected to the reference samples.
Select ‘Properties’ to open a list with all properties that have been defined so far. NOTE If the property you need is not in the list, create it by clicking on ‘Properties’ in the tree menu, and then selecting ‘new property’. Define the type (here: identification) and name of the property. Note: Additionally, it is possible to define several Substance IDs, for example a company specific number code that is used as substance label.
Switch to ‘Sample Management – Samples’ to open a list with all samples that have been measured. Notice that in the list the ‘Time Stamp’ filter is set to a specific date. Right click the time stamp icon to ignore, or left click on it to edit the filter settings To shorten the list of samples, you can also use additional filters, e.g. on the ‘Application’ column. This can be helpful if you used dedicated applications for reference spectra measurement of each sample type. 38 Tutorial NIRWare 1.
Select your reference samples by clicking on the topmost reference sample in the list. Then press and hold the Shift-button on your keyboard while scrolling down the list (using the mouse or the arrow keys on your keyboard). Alternative: By pressing ‘Ctrl-Shift-End’ on your keyboard you can highlight everything from the first selection down to the end of the list. Then click on the `Open existing data set`-icon in the upper left corner to create a new Sample Set .
Select a property that you want to assign to your samples. Then click on the right-arrow key to shift it to the ‘assigned’ list. Repeat this process for all your properties. Notice that this assignment created a matrix with check icons in the ‘Samples’ window. By activating the check icons you can now easily create a matrix that connects sample (=row) and property (=column). Save these data by clicking on the corresponding icon .
detailed optimization procedures and description of NIRCal features are described in the NIRCal documentation. Start NIRCal and log on as an administrator. NIRWare 1.
From the menu, select View/Toolbars and select the Toolbars as shown in the picture To load spectra from the database into your empty project, click on the binocular icon . Select the spectra from the list, and click on the green check mark icon. 42 Tutorial NIRWare 1.
To simplify the selection, use appropriate filter settings, especially for ‘Time’ and ‘Application’. (Time: right click to ignore time filter, left click to set time filter settings.) Since we performed triplicate spectra measurement of each sample, we now find three spectra for each individual sample. Select the NIR-Explorer window, select ‘spectra’ from the tree menu and check if all spectra have been correctly loaded.
Click on YES to let the C/V-selection wizard create a selection. Note: It is highly recommended to perform the selection sample wise, so that ALL spectra of one individual sample are EITHER in the C- OR V-Set. This is described in detail in the NIRCal documentation. For our example, we will leave the result from the selection wizard untouched. A full calculation is performed, and the result is visualized in nine windows.
Select ‘identification’ as calibration type, and click on ‘OK’. The wizard now starts with the optimization process, which will take a few minutes. The progress is visualized in the ‘Calibration Q-Value overview’. In the course of the optimization process, you see the Q-Value rise from zero (no working calibration) up close to 1 (=perfect calibration). After the wizard is finished, the results are shown in a list where the best calibrations (with the highest Qvalues) are found on top of the list.
The ten best results are stored in the NIRCal Explorer, and the one with the highest Q-value is set to ‘active’. From the plot ‘Scores vs. Scores’ of PC1 vs. PC2 you can see an excellent separation for two of the four properties. Only one overlap is displayed. But since we look at a 2-dimensional projection of a multidimensional space, we have to keep in mind that an overlap might only result from the projection, and not from a spatial interpenetration of the clusters in 46 Tutorial NIRWare 1.
the multidimensional space. In other words: we have to check if the overlap is only a question of perspective. For this purpose, we select a projection to PC1 vs. PC3. Notice that we see an overlap again, but of different clusters. The overlap from the first projection is now resolved. This proves that the four clusters are in fact separated from each other.
Click on the ‘R’ icon on your keyboard to start (and stop) the autorotation function. The plot confirms that the calibration from the wizard is well capable to differentiate between all four sugar types. (Comment: For more complex examples, the same rule for overlap checking applies to 3D- as for 2Dprojections: Look at every overlap from different perspectives.) Now switch again to the NIRCal Explorer window and have a look at the ‘Calibrations’ Note that the ten best calibrations are stored here.
To save the calibration to the database, click on the ‘save’ icon in the menu bar . Type in a name for your NIRCal project and click on the ‘Save As’ icon. So far the calibration is still in the ‘created’ state. If you would try to use it in an application, this would prevent you from changing your application (!) into the next state, because an approved application requires an approved calibration. It is suggested to recalculate the first calibration.
Now your calibration is finished and in the approved state, so it can be used for integration into an application. This is done in the NIRWare Management Console. (Please remember that only applications with an approved calibration can be approved.) 5.3.6. Integrating a qualitative calibration into an application The final step in creating an application for identity control with NIR is to integrate the calibration into the application.
The application is now available as a new point in the tree menu. Click on the ‘Copy’ icon to create a copy of this application. This copy starts in the ‘created’ state, while the original application remains ‘approved’. To change the name, you first have to click on the ‘Edit’ icon . This causes a change from ‘idle’ to ‘edit’ mode. Now you can change application name and description Save this change to the database by clicking on the ‘Save’ icon NIRWare 1.5 Software Manual .
Next we change the ‘number of measurement sequences’ from 3 to 1. From the tree menu, select the ‘Operator configuration’ menu of your application Remember that the complete view as shown above is only visible if the icon ‘show advanced settings’ was activated. Again, first change to ‘edit’ mode. Then change the number of measurement sequences to ‘1’. Also type in an appropriate Standard Operation Procedure (SOP) description: Save this dataset by clicking on the save icon again.
On the Properties level click the button to make the property editable. Select ‘Properties - New’ menu from the tree menu of your application and select the drop down-menu for ‘Assigned Calibration’. In the ‘Assigned’ column, set a check-mark in front of the calibration you want to use. Click on the green check-mark button to assign the chosen calibration to the application. A message appears, which you just confirm: NIRWare 1.
The properties defined in the selected calibration are now automatically assigned to the application. A 'Name' can be entered as a label to e.g. translate a foreign property name. The ‘Unit’ field should be left blank, since we do not create a quantitative application. Save all changes made to this data set . Then select your application from the tree and save it also to the database . Now this newly created application is ready for use in the operator software, but only for administrators.
NOTE: To make this application also available for operators, select the application and put it in the approved state . You can now start with routine ID checking of sugar samples with the Operator software. 5.3.7. Routine use for ID check The previously developed application was designed for routinely testing of the identity of sugar samples. Similar applications are performed in the pharmaceutical industry, especially for ID testing of incoming raw materials.
Create a new batch and define name and expected identity of the substance(s) you want to test: 56 Tutorial NIRWare 1.
We want to use the application to check if our sugar samples really consist of lactose (‘milk sugar’). For demonstration purposes, we choose a sample of fructose (‘fruit sugar’) and one of lactose As expected substance we choose lactose. If our calibration is working properly, the first sample will be rejected, and the second one accepted. Press the green arrow button to start the measurement sequence.
The spectrum residual is judged to be OK, which indicates that the spectrum is very similar to those that the calibration was built on. ‘Distance OK’ tells us that the spectral representation falls within the boundaries of a cluster, but because ‘found’ and ‘expected’ substance differ, the sample is falling into the wrong cluster and is thus rejected. So from the report you can be sure that the sample is not lactose, but -with high probability- fructose.
To ensure that all samples are measured under identical spectrometric conditions, we suggest to start the development of the routine application with a copy of the application for acquisition of calibration data, which is then adjusted. Please keep in mind that only applications in the ‘approved’ Lifecycle state are visible to (and usable by) a user of the ‘Operators’ user group.
The application development starts in the NIRWare Management Console (MC). Start the program and log on as an ‘Administrator’. Left-click on ‘Application Designer’ in the tree menu on the left, then on the subtitle ‘New’. A dialog appears for creating a new application 60 Tutorial NIRWare 1.
Fill in the application name and all other requested information into the white fields on the right side. The ‘SOP Text’ will later on tell the Operator how to perform the actual measurement, so it is important to give a complete description which is easily understandable. Click the Save icon to save the new application to the database . Your newly created application is now shown in the tree menu.
To change the settings, first click on the ‘Edit Data Set’ icon . Notice the change in the icon bar for Lifecycle state from ‘Created Idle’ to ‘Created Editing’ (see above). You can now make changes to all white fields. For our example, we just change the ‘Number of measurement sequences’ from 1 to 3. This will cause a triplicate measurement of every reference sample, which creates more variation in the spectra set later used for calibration. Thus, we will get more robust calibrations.
Measurement of reference spectra is the second step in the development process. Start the operator software and log on as an ‘Operator’. Then press the ‘Select application’ button measurement of reference spectra: NIRWare 1.
The application is now loaded to the Operator. At the left side, you see fields to fill in information about batch, analysis sequence and samples. Click on the ‘New’ button of the ‘Batch’ field to create a new batch: Type in the name of your batch, then click on the green check mark button: Then type in the information for AnalysisID and Sample names: 64 Tutorial NIRWare 1.
NOTE For ‘real’ applications, use ‘speaking’ names that precisely identify each sample just from the name! Also think of using the autoname functions described in the NIRWare documentation. If you have filled in and checked all information, prepare the samples for measurement (i.e. place all vials in the autosampler) and press the green check mark button. During the measurement sequence, the SOP text field is greyed out. If an ‘Instrument Suitability Test’ (SST) starts, just wait until that is finished.
Since the intensity of the external reference is so much higher than that of the sample spectrum, the latter are just a flat line on the x-axis. To have a closer look on the sample spectrum, deselect the check box for ‘External Reference’ below the graphic: 66 Tutorial NIRWare 1.
The vial autosampler will automatically continue with the next samples after confirmation of the following dialog: Click on the green check mark button to start the next measurement sequence. The spectra shown below are all from identical sugar samples: NIRWare 1.
Variations in the spectra result from differences in size and orientation of the particles, and from variations between the glass vials. To zoom into the spectrum, click and hold the left mouse button while dragging the cursor. 68 Tutorial NIRWare 1.
The so defined frame will be magnified: To change back to full view, click on the symbol with the magnification lens above the globus: NOTE It is possible to delete spectra, but only right after they were measured. This might be desirable if for example a vial was not correctly positioned in the autosampler. To delete a measurement, click on the red cross button (red cross in the upper left corner, not the one next to the magnification lens icon).
To select (or deselect) a line in the list, press and hold the Ctrl-button on your keyboard while left-clicking on that line. Click on the ‘Delete’ button to delete the selected measurements. After completion of the measurement of your reference samples, switch to the NIRWare Management Console to continue with the next step in application development: the assignment of properties and property values. (here: concentration values) 5.4.4.
Switch to the NIRWare Management console, and select ‘Sample Management’ from the tree menu. Switch to the MC, and select ‘Sample Management’ from the tree menu. Select ‘Properties’ to open a list with all properties that have been defined so far: NIRWare 1.
If the property you need is not in the list, create it by clicking on ‘Properties’ in the tree menu, and then selecting ‘new property’. Define the type (here: qualification) and edit the name and unit of the property. Also type in your name to document who created this property. Click on the Save icon to write this property definition to the database. Create all new properties accordingly. Now we want to tell the computer which sample belongs to which property.
To shorten the list of samples, you can also use additional filters, e.g. on the ‘Application’ column. This can be helpful if you used dedicated applications for reference spectra measurement of each sample type. Select your reference samples by clicking on the topmost reference sample in the list. Then press and hold the Shift-button on your keyboard while scrolling down the list (using the mouse or the arrow keys on your keyboard).
Then click on the ‘Open existing data set’-button in the upper left corner to create a new Sample Set . This opens a window with three lists: ‘available properties’, ‘assigned properties’, and ‘samples’. This allows you to select properties for the samples by shifting them from the ‘available’ to the ‘assigned’ list. Select a property that you want to assign to your samples: followed by a click on the arrow key to the right. The property ‘Lactose’ has now been shifted to the ‘assigned’ list.
Repeat this process for all of your properties: The highlighted matrix cells allow you to define the lactose- and fine sucrose concentrations of each sample: Complete the matrix list, and save these data to the database by clicking on the save button . You can now switch to NIRCal to build a calibration on this reference data set. NIRWare 1.
5.4.5. Creating a basic calibration by using the NIRCal wizard This chapter describes how to create a calibration with NIRCal, using the reference spectra with previously assigned properties. The description here is limited to the use of the NIRCal wizard, since detailed optimization procedures and description of NIRCal features are described in the NIRCal documentation. Start NIRCal and log on as an ‘Administrator’.
To simplify the selection, use appropriate filter settings, especially for ‘Time’ and ‘Application’. (Time: right click to ignore time filter, left click to set time filter settings.) Since we performed triplicate spectra measurement of each sample, we now find three spectra for each individual sample.
It is not possible to develop only one calibration for determination of both properties. So we need to create two calibrations, one for each property. First we start with a calibration for Lactose quantification, so we deselect the unwanted property ‘Fine Sucrose’. This is done by selecting ‘Properties’ in the NIRCal tree menu, followed by a right-click on the respective property name in the right part of the explorer window.
Click on YES to let the C/V-selection wizard create a selection. Note: It is highly recommended to perform the selection sample wise, so that ALL spectra of one individual sample are EITHER in the C- OR V-Set. This is described in detail in the NIRCal documentation. A full calculation is performed, and the result visualized in seven windows. Notice that in the ‘Predicted property vs. original property’ window a diagonal calibration curve is shown for the Property Lactose.
Select ‘quantification’ as calibration type, and click on ‘OK’. The wizard now starts with the optimization process, which will take a few minutes. The progress is visualized in the ‘Calibration Q-Value overview’: In the course of the optimization process, you see the Q-Value rise from zero (no working calibration) up close to 1 (=perfect calibration).
Now switch again to the NIRCal Explorer window, and have a look on the ‘Calibrations’: Note that the ten best calibrations are stored here. The one with the highest Q-value is set to active (indicated by a red dot). Since we only need one calibration, we select everything, except for the one we want to keep. This is done by holding down the Ctrl-Key while left-clicking in the right window pane on the calibration to be selected: NIRWare 1.
Right-click on the selection and choose ‘delete’. A confirmation message appears, which you will answer with ‘YES’: To change the name of the calibration, right-click on the calibration name in the left window pane and select ‘Rename’ from the context menu: 82 Tutorial NIRWare 1.
In this case, we rename it to ‘Lactose Quan’. (Hint: With more complex projects it is also a good idea to start with an identical project name for the calibration name and then just add a suffix for the respective property. Example: ‘Sugar mixture – lactose’ and ‘Sugar mixture – fine sucrose’.) To save the calibration to the database, click on the ‘Save’ button in the menu bar .
and ‘Next’ . Now your calibration is finished and in the approved state, so it can be used for integration into an application. Remember that the just created calibration works only for lactose. So we need to start over again to create a second calibration project for fine sucrose. Create a new project by clicking on the respective button and start over again with spectra loading etc.
Both the creation of the routine use application and the integration of the calibration into this is performed in the NIRWare Management Console (MC) . Load the application for reference measurement by choosing ‘Open’ from the ‘Application Designer’ in the tree list. Then select the reference application from the list on the right: The application is now available as a new point in the tree menu: NIRWare 1.
Click on the ‘Copy’ icon to create a copy of this application: This copy starts in the ‘created’ state, while the original application remains ‘approved’: To change the name, you first have to click on the ‘Edit’ icon . This causes a change from ‘Idle’- to ‘Edit’ mode, allowing you now to make changes to the ‘Value’-fields. Change the application name, then save . The application for routine use has been prepared, and the calibration can now be assigned to it. 86 Tutorial NIRWare 1.
On the Properties level click the button to make the property editable. Select ‘Properties - New’ menu from the tree menu of your application and select the drop down-menu for ‘Assigned calibration’ by clicking on the down arrow symbol at the end of the corresponding value field: In the ‘Assigned’ column, set a check-mark in front of the calibration you want to use. Click on the green check-mark button to assign the chosen calibration to the application.
The property defined in the selected calibration is now automatically assigned to the application (‘Assigned Property’). A 'Name' can be entered as a label to e.g. translate a foreign property name. 88 Tutorial NIRWare 1.
The ‘Unit’ field has to be filled out as well. Save all changes to the database by clicking on the icon . These steps have to be repeated for every other calibration to be used in the application. In this example the Fine Sucrose is calculated = 100-Lactose content. Edit also the lower, upper, warning and action limits beside the property name, unit. Now you can already use this newly created application as an administrator user in the operator software.
5.5. Content Uniformity Test (CUT) 5.5.1. Development of an application for Content Uniformity Testing (CUT) of Solid Dosage Forms The US Pharmacopeia, the European Pharmacopoeia and the Japanese Pharmacopoeia describe detailed procedures to test the content uniformity of single dosage units. The test indicates the uniformity of the active pharmaceutical ingredient (API) in the dosage unit, such as tablets or capsules, based on the assay of a defined number of samples.
From the dropdown list under “Content Uniformity Test according to”, select the procedure you with to use for testing (e.g. General Procedure (Japanese Pharmacopeia, edition 14) General Procedure (Japanese Pharmacopeia edition 15, European and United States Pharmacopeia)). For details, please refer to the parameter list of the Application Designer. Please note.
The parameters L1, L2 and T are given by the respective Pharmacopeia. Choosing "Individual Monograph", the values for L1, L2 and T can be edited. It is recommended to use the Autoname function of the Operator Configuration to create sample names automatically from basic entries as shown in the below example (autoname part 1 = Batch information; autoname part 2 = none; autoname part 3 = Counter).
Create a new batch. Each CUT is handled as an individual batch. When the CUT is finished, the batch will be closed. With the autoname function, the sample names are generated automatically. NIRWare 1.
Press on the Start Button to start the CUT. In case a SST is necessary, the following message appears: Follow the instructions and click OK. After the SST is finished successfully, the following message appears: 94 Tutorial NIRWare 1.
Follow the instructions and click OK. Now the CUT starts. When the results of the 10 tested samples are conform, the following message appears: Comments entered in the entry field will appear on the report. After confirmation, the report will be displayed on the right, containing a detailed statistical evaluation of the data according the chosen Pharmacopoeia procedure. NIRWare 1.
96 Tutorial NIRWare 1.
In case the results of the 10 tested samples were not conform, the following message appears: Click the arrow in front of Continue if you wish to continue with the required 20 additional samples immediately or complete the test at a later time by selecting the batch from the drop down menue in the Operator.
98 Tutorial NIRWare 1.
NIRWare 1.
In case a sample measurement results in a residual outlier or is outside the calibration range, a prediction of this sample is not possible. In this case the CUT stops with the following message: The corresponding report states the reason for the aborted test. 100 Tutorial NIRWare 1.
NIRWare 1.
5.6. Using applications and calibrations in Life Cycle state "Created" The calibrations and applications can be used in the Life Cycle state 'created'. This can be helpful to test a calibration during calibration development or to adjust instrument and application parameters before setting it into the 'checked' state (only Life Cycle 'Electronic Records' or 'Electronic Records'/'Electronic Signatures') or 'approved' state for routine use. 5.6.1.
If you select an application which is in the Life Cycle State 'Created' the following message appears: Under Life Cycle model 'Electronic Records'/'Electronic Signatures' it will not be possible to apply an electronic signature on results. Under Life Cycle model 'Electronic Records'/'Electronic Signatures' the measurement sequence will remain in the life cycle state 'created', therefore it can be differentiated from measurement sequences generated with 'approved' applications.
NOTE: If you modify a calibration in life cycle state 'created' that was used for predictions already, all previous measurement sequences and result reports generated with that calibration will be modified according to the new calibration setting. To update the calibration in the application, you need to de-select the calibration and re-asign the calibration new to the corresponding property or property group.
Results generated with these applications are logged in the database. Depending on the life cycle state, it will be possible to disable or delete the results but they can not be modified afterwards. With the use of life cycle model 'Electronic Records'/'Electronic Signatures', it will be possible to use the electronic signature to sign results and reports. To update the calibration or modify application parameters (e.g.
A licence request file will be generated and saved to your disk (ending '.xml'). Send this file to your BUCHI distributor. BUCHI will then create a licence file which is bound to the name and HostID of your computer ('nodelocked'), so that the application will only run on that specific PC. This licence file (ending '.lic') will then be sent to you. Just import it to your software by choosing Help > Import license in the NIRWare Management Console.
5.8.1. Manual SST measurement 1. Start NIRWare Operator 2. select an Application from the DB 3. In the menu under Advanced select "Perform Suitability Test." Or start NIRWare Operator, use "Open service tool" and choose "Suitability test". After completion of the System Suitability Test a Report is displayed on the right side of the Operator window. A detailed Report can be viewed in the NIRWare Sample Manager. 5.8.2.
The following window opens: Press start to execute the NADIA test and follow the instructions on the screen. Once the test is finished, the window shows the following information: 108 Tutorial NIRWare 1.
An *.xml file is generated and stored in the directory shown in the report window (example: "C:\Users\\Documents\MyNadiaFiles\LL-2013-03-05_15-24-53.xml"). Send this file to a service technician for evaluation. To archive the file, copy it to another location. 5.10. Measuring a reference To measure a reference spectrum, proceed as follows: 1. Start the NIRWare Operator. 2. Select an Application from the DB 3.
where the first internal reference was recorded right before the external reference. Internal referencing minimizes the need for (inconvenient) user interaction in situations where no automatic placement of the reference is possible. NOTE Different modes for reference measurements are available. Batch, Manual, Temperature Drift, Once a day, Measure Sequence, Interval and Disabled.
The Logon window will close if the user name and password are accepted. The user then clicks on the “Binoculars” icon NIRWare 1.5 Software Manual to see the available Applications.
NOTE Applications which are not saved in the Management Console remain in the Life Cycle state '....Editing'. Applications in this state will not be shown in the selection window. The user selects the row for the desired application, then clicks the green check mark at the bottom right corner of the “Select Application” window. The windows appearance changes as shown below (particular fields and their labels may vary, depending on how your Application has been configured).
Click on the "Expected substance" field, the substance name, which should be identified should be selected. NIRWare 1.
If the Substance ID is used (deactivate "Use drop down for expected substance" filed in the application), the user has to enter the substance code (article number). Several codes can be used for the same substance (enter them in "MC: Sample Manager/ Properties"). This code with many other substance information can be entered also by barcode. 114 Tutorial NIRWare 1.
The user types in the Batch (or Lot) number in the “Batch” field. The user goes to the batch dropdown menu and selects the batch that he is running. Since this batch was run previously, the Expected Substance field will fill in automatically. The user now sees the sample’s Batch number and Expected Substance appear on the screen. NIRWare 1.
Any additional required fields (such as “Analysis ID” and “Sample”) now need to be filled in by the operator. To start the measurement, the user clicks the green arrow in the top left corner, or clicks the button on the fiber optic probe. 116 Tutorial NIRWare 1.
If the system determines that a new external reference needs to be collected, the external reference scan will begin automatically. As long as the user has placed the reference cap on the probe he does not need to take any action other than waiting for the scan to finish (as indicated by the progress bar at the bottom of the screen). If the reference cap is not in place, a warning prompt will appear, advising the user to place the reference cap on the probe.
If the system determines that a new internal reference needs to be collected, that measurement will automatically be collected. No special action is required of the user other than waiting for the scan to finish. A message will appear saying “Please Prepare for measurement”. 118 Tutorial NIRWare 1.
Now the reference cap is removed and the probe window is brought in good contact with the sample. The user now clicks the green check mark or the button on the probe to initiate the scan. During the scan, the progress bar will be moving on the bottom of the screen. Once the measurement is complete, the result report will appear on the right side of the screen. Two report formats are available (but only one will be presented to the user).
For both report formats, for a material to be successfully identified, a green “OK” should appear next to the Name, Distance, and Spectral Residual in the area of the report corresponding to the calibration that identifies the material just scanned. If one of the 3 criteria is not fulfilled, the substance is not identified. Only if Distance and Residual are OK, there is a substance name in the "Found substance" field. Reports may be printed by clicking the print icon above the report.
Additional samples are measured accordingly. NIRWare 1.
For identification, the "Atline View" can be activated. In this case the user has only the symbol green check: ID OK or red cross: ID NOT OK will be visible. 122 Tutorial The user can see only the report, no spectra are available. NIRWare 1.
For quantitative measurements for measurement option for only ONE sample, the "Overview" always shows the average of the already measured sample results (here the average of 3 repeated measurements of the same sample). NIRWare 1.
By "Results" the 3 single results and the average is available, if the Report type "Detail" is activated. 124 Tutorial NIRWare 1.
There are 4 report types available, please choose the best suitable for your application (in "MC: Application Designer"). By "Spectra" the measured spectra are visible. 5.12. Extended Wavelength Range -1 Commonly the NIR spectral range is defined from 780 – 2’500 nm (appr. 12'800 – 4'000 cm ). The -1 accessible default range for NIRFlex N-500 is 1'000 – 2'500 nm or 10’000 – 4'000 cm for all measurement cells except Solids Transmittance.
Go to Security Designer => Users and Groups => User Groups and add the group of Superusers i.e. to the group of Designers: Now you need to assign some privileges to the group of Superusers. Go to Security Designer => Security Policy => Edit expert values and add the User Groups "Superusers" to the "Assigned users and groups".
Go to Security Designer => Users and Groups => New user and create the new user. Go to Security Designer => Users and Groups => User Groups and assign her/him to the group of “Superusers”. The next time this user logs in with this account she/he will be able to change the settings in applications. (Instead of the group “Designers” you may also use the group of “Administrators”.) The Application Designer for this user will now look as shown below: NIRWare 1.
In order to change the wavenumber range first changes the number of datapoints. Using an interval of 4 -1 -1 -1 cm and starting at 4,000cm the upper limit will be reached at 10,000cm using 1,501 datapoints -1 (default) and at 12,200cm using 2051 datapoints. -1 -1 For Solids Transmittance an interval of 4 cm and starting wavenumber at 6,000cm is used. The default -1 number of datapoints is 1,381 (11,520-6,000 cm ). The upper limit will be reached with 1,551 datapoints -1 (12,200-6,000 cm ).
-1 The noise increases considerably above 12.000 cm and the baseline is less stable. These limitations are caused by physics and they are not specific for the NIRFlex N-500 but can be observed for every FT-NIR spectrometer regardless of the manufacturer. WARNING Spectra recorded in the extended range will have a different number of datapoints than spectra measured in the default range. Mixing up these types of spectra in the same database can cause problems.
6. NIRWare Suite 6.1. NIRWare Management Console 6.1.1. Management Console The NIRWare Management Console is structured similar to the Microsoft Management Console (MMC). It hosts all SnapIn Modules of the NIRWare Suite except NIRWare Operator and NIRCal 5. To open the NIRWare Management Console, click on the Start button in your task bar and select All Programs / BUCHI / NIRSolutions / Management Console or click the corresponding icon on your desktop, if applicable. .
The Management Console is divided into three sections: On the left side is a tree view for navigation through all available SnapIn Modules. The right side is horizontally divided into two areas. The upper area displays the parameters, which can be modified. The lower area displays an advanced help for each value selected in the upper area. Menus and icons Console New No function in current software version Save As...
Lifecycle related icons (represent the same functions as contained in the Lifecycle menu): Edit Change data of an application which is already implemented in the database Save Save data into the database Copy Copy data from one data set into another Next Put data set into the next stage Delete Delete data set Help Help NIRWare ... Open the NIRWare HTML Help Software Registration ...
To move a Snap In from one side to the other, click it so that it is highlighted and press the corresponding arrow button. Then click save button to confirm your settings. NOTE Generally all entries within the Module windows of the Management Console have to be saved by means of the Save icon. When new settings in an active window have not been saved, yet, this can be seen from an asterisk next to the window header. 6.1.2.
Entries can be searched according different time definitions: Specific Date and Time If checked, only samples measured on the selected day will be available in the selection list. Period Alternative to a specific date/time; if checked only samples measured within the selected time interval will be available in the selection list.
With the second variant of drop down filter, you can select the entry from the list or activate a special Custom Row Filter. Selecting (custom) opens the Custom Row Filter: Here you can specify the cell content by which you want to filter the table. Fill in the fields and click OK to apply the filter.
Create new template. Activate selected template. Save existing template. Delete selected template. Reset all user specific filter settings, excluding the templates. Templates: Enter a new template name or search for existing templates from the drop down menu. Persist column widths and filter strings can be deactivated. To create a new template, first configure the filter settings in the table. Then open the above shown dialog. Under "Templates" enter a template name.
For expert users an advanced mode can be activated by a mouse-click. All advanced parameters have a default value and can be edited, if needed. To open the Application Designer proceed as follows: In the file tree on the left side of the NIRWare Management Console select Application Designer. The following dialog opens: Creating a new application To create a new application open the submenu by clicking on "New" in the file tree or on "New Application " in the center of the Application Designer window.
By default, only the basic settings are visible. To show and hide the advanced settings again, click the corresponding icon Parameter Name Description Application name Entry for application name Application type Select: "Quantification" or "Identification". Application description Entry for an application description (optional). Instrument Select: "NIRFlexN500". Measurement Cell Select used measurement cell: . 1. NIRMaster 2. Fiber Optic SMA (for continuous measurement) 3.
6. No Option Transflection Head 7. No Option (Cuvette) 8. Vial Petri USP Testkit (only for BUCHI internal use) Tablet XL License Key* Application of a license protection to this application * non bold parameters are advanced settings. Some basic parameters are mandatory, i.e. the corresponding fields have to be filled in. If you try to save your settings with some mandatory fields still empty, an error message is displayed and the fields to be filled in are marked with a red frame.
Select an application and open it by clicking on the "Open existing DataSet" button click on the corresponding row indicator or with double . The following dialog opens: Parameter Name Description Application name Entry for application name Application type "Quantification" or "Identification". Application description Entry for an application description (optional). License Key Application of a license protection to this application Max.
Modifying parameters Click the "Edit" icon and change the application name, the application description and for qualitative applications the hitlist size. The application parameters are grouped in 4 different categories. Properties Instrument Report Operator Configuration Each of this categories contain basic and advanced settings which can be modified. 6.2.2.
cannot change it by default. If you really need to, you have to log in as a user with the right to ‘Edit expert values’ (Management Console – Security Designer – Security Policies). 6.2.3. Parameter list Properties: Assigning a property or several properties to an application This menu is used for assigning calibrations to the application. The calibration properties will be used for prediction during the routine use. NOTE: Leave the property field empty for applications used for spectra collection.
First select the calibration desired to use by the “Assigned Calibration”. Confirm this with the green check: The name of the Assigned Property, Name and Unit will be automatically filled in accepting the following message: 144 NIRWare Suite NIRWare 1.
The following list of parameters is available: Parameter Name Description Assigned Calibration Name of the calibration which has been calculated in NIRCal. Only assigned calibration allows prediction of a measurement result. Quantitative: Select the corresponding quantitative calibration model for the property.
Unit of the quantitative property in the database (e.g. % or ppm or g/kg, please edit it by creating the property). Identification: Leave this field empty. Position Quantitative: Position of the parameter to be displayed in NIRWare Operator and all printed documents. Only needed if more than one property is added to the application for predicted. Identification: The position of a calibration has no influence on the prediction. 146 NIRWare Suite NIRWare 1.
6.2.5. Calculated property Only for quantitative property there are following parameters: Calculated property formula This is new in NIRWare 1.5 and enables the user to define properties which are calculated from other properties, e.g. Dry matter =100-Moisture A calculated property is defined as a normal property, but without assigning a calibration and property. Pressing on the drop down in the right side brings up the formula editor.
Formulas are written as C# code (read: C-sharp), and can use most of the constructs for flow control which are available in C# In the following a number of examples illustrate how calculated properties can be used. The examples can be copy/pasted directly to the formula editor for tests. DM is expressed in % and calculated as 100 minus the moisture content. Select: Constructs / General / CalculatedValue Replace the with “100-“ 148 NIRWare Suite NIRWare 1.
Choose Variables. Select the desired property and choose the value: CalculatedValue = 100 - ApProperty["Moisture"].Value; Take care, that the semicolon is at the end. The calculated property can be controlled with editing values in the property window and use “Check”. Save the formula. Edit the name of the property, the unit and if possible the upper and lower action and warning limits. NIRWare 1.
Save the new property and change the position if necessary: Example 1: Dry Matter Add conditionality based on the residual: if(ApProperty["Moisture"].ResidualOK) { CalculatedValue = 100 - ApProperty["Moisture"].Value; } If CalculatedValue is not defined in the formula the value will be set to a very high or low number which one might want to avoid. In this case it is advised to define CalculatedValue to a value which the user will interpret as not valid, e.g. -999.
if(ApProperty["Moisture"].ResidualOK) { CalculatedValue = 100 - ApProperty["Moisture"].Value; } In the report this measurement then appears as -999 and can easily be interpreted as an invalid measurement. In case frequent error due to too high residuals occurs, the limits can be extended. Here the residual limit is compared to the residual and the limit is multiplied with 1.20 to add 20% higher tolerance limit. CalculatedValue = -999; if(ApProperty["Moisture"].Residual < ApProperty["Moisture"].
//Othwerwise if a value larger than 100 is predicted then set the calculatedValue to 100 else if(ApProperty["Moisture"].Value > 100) { CalculatedValue = 100; } //Othwerwise use the predicted value else { CalculatedValue = ApProperty["Moisture"].Value; } } Example 3: Two properties and local variables The results from two or more properties can be combined. Here a result present if the residuals of both Fat and Moisture are OK. CalculatedValue = -999; if(ApProperty["Moisture"].
Tips and tricks The notation used is C# notation. Refer to C# reference documentation for more detailed description of the notation. Not all C# functions and constructs are available. Terminate lines with semicolon “;” Set the action and warning limits manually for calculated properties. Action limits can be set to catch the value used to indicate an error, e.g. -1000 in the examples above. Comments can be written as “//” in front of a line, or after the code in a line.
To edit already created property entries, click on the corresponding entry in the file tree list. The following list of parameters is available: Parameter Name Description Name Quantitative: Name of the quantitative property (e.g. Name = grassi / assigned property = fat) to be displayed in the Operator Interface. Identification: Name of the qualitative property (e.g. sucrose for SIMCA) or property group (e.g. white powders for libraries and CLUSTER calibrations).
Identification: Name of the qualitatve property (SIMCA) or all qualitative properties in the property group (CLUSTER). Select the correct qualitative property/properties from the drop down menu: For Libraries, no entry should be done. Assigned Calibration Name of the calibration which has been calculated in NIRCal. Only an assigned calibration allows prediction of a measurement result. Quantitative: Select the corresponding quantitative calibration model for the property.
Position Quantitative and Identification: Position of the parameter to be displayed in NIRWare Operator and all printing documents. Only needed if more than one property / property group is added to the application. predicted. Decimal Places (Result) Quantitative: Define, how many positions after decimal point will be displayed for the prediction result. Default: 2 Decimal Places (Average) Quantitative: Define, how many positions after decimal point will be displayed for the result average.
See also "Definition of calibration range, warning and action limits". Default: lower limit of calibration range To set back the default value for the action limit, click on this button Bias . Linear correction of a predicted result using bias function. Correction will be displayed in report. Default: 0 Slope Linear correction of a predicted result using slope function.
"Warning Limits" define the range around an acceptable result (e.g. production optimum). indicates, that the predicted result is within the acceptable tolerance limits (warning limits) or limits). indicates an under- or overshooting of these defined limits (but within the defined action "Action Limits" define the limits, which if exceeded or under-run, indicate that results are outside of acceptable tolerance. Action needs to be taken e.g.
Select the points and click the right mouse button to get the Add Trendline: NIRWare 1.
The regression coefficient is visible: 160 NIRWare Suite NIRWare 1.
y=0.9091*x-0.9091 To get the original laboratory values, the correction is: Bias = -0.9091, Slope = 0.9091 NIRWare 1.
6.2.9. Instrument parameters To get access to the instrument parameter list, click on the entry "Instrument" in the file tree list on the left. By default, only the basic settings are visible. To show and hide the advanced settings again, click the corresponding icon 162 NIRWare Suite . NIRWare 1.
The following list of parameters is available: Parameter Name Description Instrument Type of NIR Instrument to be implemented in this specific application: NIRFlex N500 Measurement Cell Selected measurement cell: 1. NIRMaster 2. Fiber Optic SMA (for continuous measurement) 3. CheckMaster Transmittance 4. Solids Transmittance 5. Fiber Optic Liquids 6. Fiber Optic Solids 7. Liquids 8. Solids Measurement Cell Add-On Selected measurement cell add-on.
5. Fiber Optic Liquids 8 scans (Qualitative) 16 scans (Quantitative) 6. Fiber Optic Solids 8 scans (Qualitative) 32 scans (Quantitative) 7. Liquids 8 scans (Qualitative) 16 scans (Quantitative) 8. Solids with Vial Add-On 8 scans (Qualitative) 32 scans (Quantitative) 8. Solids with XL Add-On 8 scans (Qualitative) 32 scans (Quantitative) 8. Solids with Petri Add-On 8 scans (Qualitative) 32 scans (Quantitative) 8.
-1 -1 -1 -1 10000cm - 4000cm : 1501 (default) 12200cm - 4000cm : 2051 -1 -1 12500cm - 4000 cm : 2126 (max. allowed range) Recommendations for Solids Transmittance with lower wavenumber limit -1 6000 cm and Datapoint interval 4: -1 -1 -1 -1 -1 -1 11520cm - 6000cm : 1381 (default) 12200cm - 6000cm : 1551 12500cm - 6000cm : 1626 (max. allowed range) To get access to the entry field, the right to "Edit Expert Values" need to be assigned to you in the Security Designer under Security Policies.
24 (default) Successful suitability test is required for measurement A routine measurement can be started only if the SST was successful. Checked = A routine measurement can be started only with a successful SST. It is suggested to work with this adjustment. Unchecked = A routine measurement can be started regardless of the SST result (default) Save Spectra Interferogram Next to the spectral information, the interferogram of each measurement can be stored in the system.
8. Solids with XL Add-On Interval (20 min) 8. Solids with Petri Add-On Interval (60 min) 8. Solids with Tablet Add-On Measure Sequence External Reference Interval Interval in minutes to measure the external reference, if the mode to measure the external reference was selected as “interval”. Internal Reference Mode Mode to measure the internal reference (not available for Solids Transmittance).
Determination Definition of the gain determination procedure: Manual: The gain specified in 'Gain of ADC Detector for samples' is used for all sample measurements. Optimized: The optimum gain is determined when the application is run for the first time by analysing one or more samples. Auto: The optimum gain is determined automatically for each sample before the measurement. Determine best gain before the next measurement (Optimized) Setting for NIRFlex Solids Transmittance.
Manual: The gain specified manually in 'Gain of ADC Detector for samples' is used for all sample measurements. Increasing gain levels: 0,1,2,3,4 Auto: The optimum gain is determined automatically for each sample before the measurement. One scan is performed prior to every sample measurement and the gain is automatically determined afterwards. Individual spectra of one measurement sequence can have different gain settings.
Parameter Name Description Report type Different report templates are available from which you can choose.
Show the serial number Instrument and measurement cell serial number will be shown in report header. Checked = Instrument and measurement cell serial number shown in report (default) Unchecked = Instrument and measurement cell serial number not shown in report * non bold parameters are advanced parameters.
useful in combination with “Number of repetition…” is greater than zero) "Unchecked": No continuation possible Number of repetition measurements in case of an Out of Specification (OoS) "0": If a sample result is not ok, no repetition is requested. Number of measurement sequences "1…N": A sequence is the max. number of possible measurements without changing the samples: e.g. Fiber Optics => 1 sample, Solids and Liquids => 6 samples.
mandatory Signature on Sequence "Unchecked": No comment is necessary For LC "ERES" and selected report type "Detail : "Electronic signature on report" is set active (signature on batch will be deactivated).
Parameter Name Description SOP Fields List of all sample description fields available. Remark: Some of these fields are related to the sample and some are related to the batch information.
Error Text Links the above defined Error Text 1 to 5 to the sample SOP fields in the Operator module Field Reset "Checked": The field content is reset after each measurement "Unchecked": The field content is not reset after each measurement Remark: If field reset is set to yes, a keybord or barcode input is mandatory for every sample measurement. Validation Range A lot of constraints for input verification can be set, e.g. batch numbers shall be nine digit numbers.
The same number can be read by human eye and entered via keyboard - the system will notice no difference. Bar code fractionation Alternatively, several code numbers can be concatenated to form one mutual bar code. Example: Code0 = ‘0000’ (four leading zeroes) Code1 = Substance-ID: Integer number with 5 digits Code2 = Batch-ID: Integer number with 6 digits Code3 = Container-ID: Integer number with 7 digits This sums up to one bar code with 4+5+6+7= 22 digits, e.g.
Start @ digit 10, read 6 digits --> “222222” will go into “Batch” field; Start @ digit 16, read 7 digits --> “3333333” will go into “Analysis ID” field; The leading four zeroes (“0000”) are used nowhere, and thus be discarded. NOTE The bar code must contain information about both, the Batch as well as the Expected Substance. These two fields depend on each other. Comment Field: If activated, you can enter information in the Operator to describe the samples.
All defined fields for LIMS Import should be activated in the application as well. The "repetition measurements in case of Out of Specification" should be deactivated (value =0) and the "number of measurement sequences" should be set to 1. Multiple measurements of the same sample should be triggered by the LIMS. 6.2.15.
Prerequisites and limitations Cyclic measurements are intended to monitor one or more analytes over the course of time. The repetition mode for applications can be generally used. Nevertheless, extra care should be taken with application design to ensure smooth operation - the system cannot judge if a specific configuration does indeed make sense or not. So please have a look at the ‘Tips and Tricks’ chapter to avoid some common pitfalls.
Activate the checkbox "Cyclic measurement enabled". The cyclic measurement is started when the green start button is pressed, and ends when the red stop button is pressed. In the meantime, the system will 1. Trigger a measurement, 2. Wait for the countdown to finish, 3. Start over again with step 1. The picture shows the order of events during a cyclic measurement run. You can see that the individual measurement times (tm1, tm2. tm3) are spaced at constant times; this is the ‘cyclic measurement interval’.
The optimum measurement interval is as long as possible to avoid unnecessary data creation, but short enough to cover changes in the process to be observed. Application 2: Interval < Runtime for Measurement Cyclic Measurement Interval = 0:10 [min:sec], and 64 scans/ measurement * 0.5 sec/ scan = ca. 32 seconds / measurement Here the measurement is taking longer than the specified countdown time (32 sec. > 10 sec.
After the first measurement is done, the number next to the stopwatch-symbol counts down the remaining time before the second measurement is started- and so on. The measurement cycle is running infinitely until it is manually stopped (via the usual red stop button). Tips and Tricks Application name indicating cycle mode Using a reference to cyclic measurement in the name of the application can be very helpful to differentiate cyclic- from single measurement- applications (e.g.
Additionally, we configure the application so that it will expect the Substance-ID to define the “Expected Substance”- simply by deactivating “Use drop down for expected substance” (found under Application Designer - - Operator Configuration, see the application example above). Tips and Tricks Property-IDs must be UNIQUE Each property must have its own, unique PropertyID! Otherwise you loose the traceability of a substancecode to the corresponding substance.
NOTE Make sure that inside an application the Property Names and the SubstanceIDs are unique. The software will not check this! NOTE The start position for the first character is 1. For not using bar code fractionation set positions to 0. 6.3. Sample Management 6.3.1. Introduction Sample Manager The Sample Manager is designed to check and review previous measurement results and system reports and to enter reference values.
To open the Sample Manager proceed as follows: In the file tree on the left side of the NIRWare Management Console select Sample Management. The following dialog opens: You can now open a submenu by clicking on their names in the file tree or in the center of the Sample Management window. The Sample Manager comprises the following menus: Manage Samples In this menu property information can be linked to sample information and reference values can be entered.
Reports for USP Overview over USP test results. USP reports can be reviewed and printed out (visible only with valid license). 6.3.2. Batches Batches In the file tree on the left side of the NIRWare Management Console select Sample Management Batches. The following dialog opens: If necessary, narrow down the information displayed in the table, using appropriate filter settings.
NOTE You can sort alphabetical and inverse the order of the individual column entries by clicking the corresponding column header. Closing a batch and batch verification with electronic signature Narrow down the information displayed in the table, using appropriate filter settings. Select a batch and open it by clicking on the "Open existing DataSet" button click on the corresponding row indicator . The following window opens: or with double Detailed Information of the selected batch will be displayed.
Closing a batch and batch verification with electronic signature Enter User, Password and a Comment or reason. Confirm your entry. The Lifecycle state of the batch changes from created to checked (if Lifecycle template "High" is selected in the Management Console). Note: The same action (closing a batch) can be done in the Operator directly be clicking on the corresponding button. To verify the batch information with an electronic signature, click on in the menu bar again.
The Lifecycle state of the batch changes from checked to approved (if Lifecycle template "High" is selected in the Management Console). Note: With the electronic signature on batch, all individual measurement sequence reports related to this batch will be signed automatically. 6.3.3. Properties Properties In the file tree on the left side of the NIRWare Management Console select Sample Management Properties. The following dialog opens: NIRWare 1.
If necessary, narrow down the information displayed in the table, using appropriate filter settings. Table columns The table consists of the following columns: Name Property name Type Property type (Identification or Quantification) Unit Unit of quantitative reference data (e.g. %, mg/kg,....
The following dialog opens: Property Type Select from the drop down menu the property type: Identification or Quantification Name Enter the property name or for identification the substance name Substance ID Substance ID code for identification properties entered during property creation. Leave this field empty for quantitative property. Unit For Quantification Properties, the unit of quantitative reference data (e.g. %, mg/kg,....) can be entered.
Multiple Substance IDs Introduction In ID-tests (=qualitative analyses) a substance-specific code can be used to identify the substance to be tested; this is the so-called ‘Substance ID’, which can be very helpful if a bar code reader is used. In many companies the same material is received from different vendors, therefore one material can have n code numbers for the n suppliers of this material. This allows traceability of deliveries back to the source.
Clicking the green check-mark button confirms the entries made as Substance ID s, and copies them into the Substance ID’s value field; clicking the red X-button, however, will just close the pop up window without making any change to the Substance ID’s value field. NOTE: You can specify any string as Substance ID, no matter what length or symbols you use: any number (0…9), character (a…z, A…Z), or symbol (*/-+…) can be used – except for the semicolon, which serves as separator.
Table columns The table consists of the following columns: Name Sample name Application Name of the related application Version Copy number in the course of the lifecycle Batch Batch information Time Stamp Date and time No.
The sample name is now changed. Sample names can be changed as long as the corresponding samples are not part of an approved measurement result or approved calibration. Assign qualitative property information (identification) to samples To assign qualitative property information (identification) to samples, select all samples you wish to edit (multi selection). If neccessary, narrow down the information displayed in the table, using appropriate filter settings.
Here a property needs to be assigned to the samples first, before the classification information can be entered. The following dialog opens, if the samples were recorded with an routine application to which one ore more qualitative calibrations are assigned to: All samples have the properties related to the application assigned automatically. The labeled name contains as information the property group name and the name of the assigned property.
The property is now added to the samples and the classification information can be entered directly by clicking on the check box or use "Enter" and the arrow down button to fill in the information. After all entries are made, click on to save changes to the database. With two exceptions, properties can also be removed from samples. To remove a property, select the corresponding entry in "Other Assigned Properties" and click on . The entered reference values will be lost.
Assign quantitative property information to samples To assign quantitative property information to samples, select all samples you wish to edit (multi selection). If necessary, narrow down the information displayed in the table, using appropriate filter settings. Open the selected samples by clicking on the "Open existing DataSet" button on the last corresponding row indicator . or with double click NOTE Imported samples show no entries under 'Application'.
All samples have the properties related to the application assigned automatically. The labeled name contains as information the assigned property name and the name used in the operator. The reference value can be entered directly. To assign a property to the samples, select from the shown "Other Available Properties" window the correct property: Table content: Name Property name Type Property type (Identification or Quantification) Unit Unit of quantitative reference data (e.g. %, mg/kg,....
The property is now added to the samples and reference values can be entered. The reference values for each sample can be entered manually or with copy/paste (Ctrl + C / Ctrl + V) from Windows Excel or other office programs. After all entries are made, click on to save changes to the database. With two exceptions, properties can also be removed from samples. To remove a property, select the corresponding entry in "Other Assigned Properties" and click on . The entered reference values will be lost.
Property assigned by user. This property can be removed from samples as long as the corresponding samples are not used in a calibration.
Application Name of the related application Version Copy number in the course of the lifecycle Batch Batch information Batch Lifecycle state Lifecycle state of the batch Start Time Date and time End Time Date and time Sample Names Name of the sample Type Type of measurement (Identification or Quantification) Report Type Type of report Sequence Lifecycle State Lifecycle state of the sequence Prediction Type of measurement sequence (0= sequence without prediction result; 1=sequence with p
NOTE You can sort alphabetical and inverse the order of the individual column entries by clicking the corresponding column header. View and Print Reports To open a report, proceed as follows: 1. Use filters to specify the table content or reset your filter settings listed in the area below the table by clicking the corresponding button. 2. To select the measurement from the list of which you want to see the report, click the corresponding row. 3. The row shows the measurement sequence.
Hitlist (for Identification results) For Quantification you can choose between 'Detail' report, 'Overview' report, 'Batch Detail' report and 'Batch Overview' report.
only a direct print-out is possible. All sequence reports will be printed out as individual reports (as defined in the application). Electronic Signature on Reports Using the LC model "ERES", electronic signatures have to be applied to the reports. Only report types defined in the application can be signed electronically.
In case "Batch report" is defined in the application, select a corresponding measurement sequence with prediction results and open it by clicking on the "Open existing DataSet" button on the corresponding row indicator . or with double click The batch report preview window opens. To verify the result of this batch click on the"Next" button appears: in the Life Cycle bar.
Select one or more measurement sequences and click on in the menu bar. In case some report entries are listed in the file tree on the left, the following message appears: Close all entries in the file tree list before continue deleting measurement sequences without prediction results by selecting each entry individually an click on the red cross button.
Close all entries in the file tree list before continue deleting measurement sequences without prediction results by selecting each entry individually an click on the red cross button. Library reports When a library report is opened, the following window appears: Under Report Options you can determine another Report Type by clicking the arrow and highlight another one from the drop-down list.
To refresh the report so that it displays possible modified settings of the report options, click the refresh icon . The report is divided in three parts: Header Contains all information for traceability of the measured samples. A customer address, instrument and measurement data can be indicated. Results The results are shown as a hitlist of the most similar spectra in the library. Calibration details The calibration name and used method are indicated.
Cluster and SIMCA reports When a cluster or SIMCA report is opened, the following window appears: 210 NIRWare Suite NIRWare 1.
Under Report Options you can determine another Report Type by clicking the arrow and highlight another one from the drop-down list. Under Details you can define whether the Address, the Instrument, the SerialNo and the Hitlist are indicated on the report by activating the corresponding check box. To refresh the report so that it displays possible modified settings of the report options, click the refresh icon .
6.3.6. Reports overview SST report In the file tree on the left side of the NIRWare Management Console select Sample Management Reports SST. The following dialog opens: 212 NIRWare Suite NIRWare 1.
The complete SST test contains out of four test categories.
There are some additional functions available via the report icon bar. Use the icons in the icon bar to navigate within the report and to process it. USP report In the file tree on the left side of the NIRWare Management Console select Sample Management Reports USP.
Info additional test information such as reason for "not passed result" User User login account ValidUp date up to which the USP Test is valid Installed at Installation date Installed by full name who has performed installation Standard standard type Std. Serial serial number of standard wheel Std. Version version of standard wheel Instrument Instrument type Instr.
There are some additional functions available via the report icon bar. Use the icons in the icon bar to navigate within the report and to process it. 6.4. Administrative Tools 6.4.1. Introduction Administrative Tools The Administrative Tools enable to make general administrative settings within the software package. They comprise logging functions, lifecycle settings, system configuration, maintenance and import / export options.
You can now open a submenu by clicking on their names in the file tree or in the center of the Administrative Tools window. 6.4.2. System Logger The system logger is the logbook for all events taking place during operation of the software package. To open it, in the file tree on the left side of the NIRWare Management Console select Administrative Tools - System Logger or click System Logger Audit trail in the submenu list in the center. The following dialog opens: NIRWare 1.
The System Logger consists of a table in the upper part, listing all events in chronological order, an area in the center, giving source string information about the filter currently applied in the table above, and an area at the bottom, concisely listing the information of the line currently highlighted in the table above.
You can inverse the order of the individual column entries by clicking the corresponding column header. Use the filter functions to narrow down the content of the table. Buttons By means of the three buttons in the right center, you can change the information displayed in the table above. By clicking the buttons Each event is displayed by default as a single line. This function increases the line and column width to show the whole content of the messages.
The following dialog opens: Four different template types are provided: Electronic Records/Signatures: Covering all requirements of 21 CFR Part 11 (relevant for pharmaceutical applications) This template is only available together with the NIRWare Advanced License or with the additional NIRWare Regulatory Kit License. It is designed for user in a regulated environment who work with electronic signatures and records.
When changing the lifecycle template to a less restrictive one, the following message appears: Confirm the corresponding message by clicking the Okay button. A second message is displayed: Confirm it again with the Ok button. NIRWare 1.
For further information on the lifecycle philosophy and templates, see Templates. 6.4.4. NIRWare Configuration The NIRWare Configuration dialog serves to set certain instrument parameters. To open it, in the file tree on the left side of the NIRWare Management Console select Administrative Tools - NIRWare Config.
Database Connection In the fields Database Server the path of the database server running the database which the software package accesses is indicated. The field Database Name shows the name of the corresponding database. Language and Culture NIRWare Management Console and NIRWare Operator are multi-language capable. In order to switch to a different language a language package needs to be installed additionally. From the drop-down menu select the language in which the software should be displayed.
Via the Database Maintenance dialog one additional functions are accessible: Archive Operations and the access to Buchi Database Management (BDM). In BDM the regular database backup can be performed. The archiving process allows you to transfer only part of the database into a new one, thus enabling you to get rid of outdated data to accelerate your current working routine. The Warning limit for the database size can be configured.
Every week the above reminder dialog recommends to backup the database. Click OK to close the dialog and create a backup as desired. Archive Operations General information The archiving function allows to store outdated data in a separate ‘container’ called archive, and to continue seamlessly with only those (reduced) data which are relevant for your current work. In the archive all data from the original database are stored, i.e.
A Wizard window appears and guides you through the archiving process: You can use the double arrow buttons to switch back and forth between dialog windows or click on the red cross button to abort. To continue click the right double arrow button. 226 NIRWare Suite NIRWare 1.
Under Archive Name enter a name for your new production database. NOTE: We recommend to add a speaking database label, e.g. indicating the local plant and time period. The date and the name of the database creator will always be documented in the audit trail automatically. To continue click the right double arrow button. The master and log data file (.MDF and .LDF) are controlled by the SQL server and are thus shown for information purposes only. NIRWare 1.
To continue click the right double arrow button. To ensure seamless continuation of operation, part of the database content is transferred automatically and listed in the appearing screen: NOTE Batches are not copied to the new database. NIRCal projects and spectra that are not assigned to any calibration are not copied to the new database.
You can now select the applications to be copied into your new database. For this purpose activate the checkbox in the first column of the corresponding line. If nearly all applications should be copied, click Select All and then deselect the ones you do not need. The checkbox "Show latest versions only" will hide all older versions of a calibration. The checkbox "Do not copy calibration spectra" will copy the calibrations without spectra.
You can now select the libraries to be copied into your new database. For this purpose activate the checkbox in the first column of the corresponding line. If nearly all libraries should be copied, click Select All and then deselect the ones you do not need. The checkbox "Show latest versions only" will hide all older versions of a calibration. Filters can be used to reduce the list to relevant entries... To continue click the right double arrow button.
Now select an archive from the list and click "Review selected archive". This will initiate a process that will restart the management console in archive-mode. You have to log in again and will see the following message: Now click the green checkmark button to have read-only access to the selected archive. The archive mode is indicated by a black frame around the window and an additional header: NOTE: NIRWare 1.
The productive (new) database contains an audit trail entry with the following content: - Time stamp, User, PC name, name of archive - Names and files for productive and archive database - List of copied applications, version, GUID - List of copied library designer calibrations - Remarks Tips and tricks No interference during backup- or archiving activities IMPORTANT RECOMMENDATION: Never switch off the computer or interfere in any other way with a running backup- or archiving process! Even though NIRWare
If the NIRWare Operator is still open, close it now. If the Control System Service is still running, you can stop it via the Windows Task Manager: For this purpose, right-click it in the list and select "Stop Service". 6.4.6. Customer Information Configuration The Customer Info Configuration dialog serves to define the customer information displayed in the header of the measuring results report. NIRWare 1.
To open it, in the file tree on the left side of the NIRWare Management Console select Administrative Tools - Customer Info. The following dialog opens: Enter the corresponding information in the provided cells and click the Save icon to save your settings. NOTE All customer information is optional. The cells can also be left blank. 6.4.7. Import / Export Introduction Import / Export The Import / Export functions enable to export data from the local database to an *.
Export Application With the Function "Export Application" applications including all necessary parameters such as instrument settings, operator configuration, calibrations and property settings will be exported. Applications can be exported with or without spectra and corresponding reference values. To export applications proceed as follows: In the file tree on the left side of the NIRWare Management Console select Administrative Tools Import/Export - Export Application.
Table columns The table consists of six columns: Name Application name Description Optional information entered during application design Version Copy number in the course of the lifecycle State Lifecycle state Type Application type (Identification or Quantification) GUID Global Unique Identifier Different possibilities are available to export an application with different attached information.
Export Calibration With the Function "Export Calibration" calibration models can be exported. Calibrations can be exported with or without spectra and corresponding reference values. To export calibrations proceed as follows: In the file tree on the left side of the NIRWare Management Console select Administrative Tools Import/Export - Export Calibration. The following dialog opens: The dialog lists all calibrations available in the software in a table. NIRWare 1.
Table columns The table consists of six columns: Name calibration name Comment Optional information entered Version Copy number in the course of the lifecycle State Lifecycle state Type Calibration type (Cluster, Spectra Compare, SIMCA, PLS, PCR,...) GUID Global Unique Identifier When you activate the check box Calibration Samples the calibration will be exported with corresponding spectra and reference values.
Export Samples With the Function "Export Samples" spectra with their corresponding reference values can be exported. To export samples, proceed as follows: In the file tree on the left side of the NIRWare Management Console select Administrative Tools Import/Export - Export Samples. The following dialog opens: NOTE When you open the Export Samples dialog, the table is empty, since the loading procedure when opening NIRWare 1.
the dialog would take some time (depending on the amount of data). To display samples in the table, use the filter functions. Table columns The table consists of eight columns: Name sample name Application application name Version Copy number in the course of the lifecycle Batch Batch name entered during analysis TimeStamp Date and time Customer Fields Optional information of the customer entered during analysis (content of Customer Fields 1-6 is summarized here) No.
Export Lifecylce To export a lifecycle template, proceed as follows: In the file tree on the left side of the NIRWare Management Console select Import/Export - Lifeycle. The following dialog opens: Export Click the Export icon ( ). A dialog opens, where you can select the name and path under which the corresponding lifecycle template should be saved. Click Save. Export USP With the Function "Export USP" performed USP reports and the data recorded during test procedure can be exported.
The following dialog opens: Narrow down the information displayed in the table, using appropriate filter settings.
Export To export a USP result, highlight the corresponding row in the table and click Export. NOTE Only one USP report can be exported at a time. A dialog opens, where you can select the path and the file name under which the exported USP result should be saved. Click Save. Export SST With the Function "Export SST" performed SST reports and the data recorded during test procedure can be exported.
Narrow down the information displayed in the table, using appropriate filter settings.
Export To export a SST result, highlight the corresponding row in the table and click Export. NOTE Only one SST report can be exported at a time. A dialog opens, where you can select the path and the file name under which the exported SST result should be saved. Click Save. Export NIRCal Project With the Function "Export NIRCal Project" projects created in NIRCal can be exported.
The dialog lists all NIRCal Projects available in the software in a table. Table columns The table consists of six columns: Project Name Name of NIRCal Project GUID Global Unique Identifier Calibration Info Information describing the contained calibration NOTE You can sort alphabetical and inverse the order of the individual column entries by clicking the corresponding column header. Narrow down the information displayed in the table, using appropriate filter settings.
Exporting data from archives Although archives cannot be modified, it is nevertheless possible to extract information from them. This is done by using the export functions of the Management Console, which are always available in archive mode. For this purpose select Administrative Tools - Import/Export. NOTE: Importing data to an existing archive is not possible.
Click the Browse icon . A dialog opens, where you can select the xml-file with the corresponding information you want to import. Click Open. NOTE Depending on the file size, the import can take several minutes. Importing applications, calibrations and sample spectra During import there are 3 major types of sample property related data fields that are compared with already existing values in the database.
The rename dialog appears in case of conflicts between name, substance ID, unit and GUID. A renaming has to be done first. In the next step the property can be assigned to existing ones in the database or be imported as a new one. The assign dialog allows to link properties that are imported to existing ones in the database. Reference values The reference values contain a time stamp. NIRWare 1.
Reference value (GUID) is already in the database, value is the same Will not be imported Reference value (GUID) is already in the database, value is not the same Cancel = the reference value in the database will be kept OK = the imported reference value will be taken Reference value for sample and property exists in the database, times tamp of the data being imported is older Will not be imported Reference value for sample and property exists in the database, time stamp of the data being imported is n
Cancel = import breaks OK = import continues 6.5. Security Designer 6.5.1. Introduction Security Designer To open the Security Designer proceed as follows: In the file tree on the left side of the NIRWare Management Console select Security Designer. The following dialog opens: NIRWare 1.
You can now open a submenu by clicking on their names in the file tree or in the center of the Security Designer window. The Security Designer serves as user administration tool within the NIRWare and NIRCal software packages. It enables you to realize your own security policy for user access. The general user management concept within the NIRWare Security Designer provides that every user is part of a user group.
+ Administrators and Designers (user group) QManagers Quality Assurance Managers QManager (individual user) + Administrators (user group) Service Service Technicians Service (individual user) + Administrators (user group) NOTE: Working with user groups helps to reduce administration work for the account policy. All members of a user group have the same rights. That means, it is not needed (but possible) to define for each NIRWare user individual settings (not recommended).
The number of signs required for a user name is set in the Account Policy. The default value is 0.The user name may only consist of one word, spaces are not accepted. To provide more information about the user, enter it in the Full Name field, where spaces are allowed. Full Name Full name of the user providing more information. Comment Optional comment for the user.
A new dialog opens: The upper table in the center lists all users defined in the software with their name and full name and with the comments assigned, i.e. it also contains the user you recently added. Creating a new user group The 3 given user groups (Administrators/Designers/Operators) are sufficient for most NIRWare installations.
NOTE The number of signs required for a user group name is set in the Account Policy. The default value is 3. To save your entries, click the Save icon. A new dialog opens: The upper table lists all user groups defined in the software with the comments assigned, i.e. it also contains the user group you recently added.
NOTE After you added a user group you will automatically get to this dialog. To assign a user to a user group proceed as follows: 1. In the dialog for user groups (see above) highlight the user group to which you want to add a user in the upper table. The group members already assigned to this user group are now listed in the table below. 2. Click the arrow next to the upper listbox. A drop-down list opens, listing all available users. 3.
3. Select the user group you want to add by highlighting it and click Add Group. The user group is now added to the table below. To save your entries, click the Save icon. Changing name and comments for existing users NOTE Once a user account has been created and has been used, 'Name' or 'Full User Name' should not be changed at any time. In case the user's family name has changed and the profile needs to be updated, you need to create a new account for this user and disable the existing one.
Password: Password This line appears twice and represents the user password and the password verification. Change Password at next logon When this check box is activated the user is prompted to change his password during the next logon. Password never expires When this check box is activated the user password always remains active. Password expires When this check box is activated the user’s password expired, so that he cannot log on anymore. To undo this, deactivate the check box.
Defining the account policy A general account policy is defined in the submenu Account Policy: Here you can see the default definition of the account policy. By entering a new value in the value column and activating or deactivating the checkboxes you can change the preset definition. Click the Save icon afterwards.
Reasons for electronic signature The electronic signature is required for the lifecycle transition of applications in the Lifecylce model ERES. To apply the electronic signature you have to state a reason. The lists given in the submenu "Reasons for electronic signature" enable you to define the reasons available for the different user groups: The list on the left shows all reasons currently available. To create a new reason, click New.
6.5.3. Security Policies Default user group access rights The following table gives an overview of the access rights of the default user groups to individual software modules and actions. If you create a new users group and add it to one of the existing groups, all rights will automatically be handed down. If you create a new users group without adding it to an existing group, its access rights have to be configured in the Security Policies.
Assigning user rights for applications By default, all users and user groups have full access to all calibrations and applications created in the software. To define access rights only for certain users or user groups, on the left side of the NIRWare Management Console select Security Designer – Security Policies – Application. NOTE There are two slightly different types of dialogs on which to assign user rights.
In the upper area, select the item for which you want to modify the user rights by highlighting the corresponding line and click Add. The selected item is now added to the Object ID list. The access to all items in the Object ID list is restricted to the users and user groups listed in the lower area. To assign user rights to an item in the Object ID list, select the corresponding Object ID by clicking the arrow and highlighting it in the appearing drop-down list.
Only the users and user groups listed in the center of the dialog have defined access rights to the software or function. All other have no access rights. To add a user or user group to this list, click the corresponding arrow, highlight a user or user group from the appearing drop-down list and click Add. The selected user or user group is added to the list in the center. You can now define the access rights for the added user or user group by activating or deactivating the corresponding check boxes.
6.6. LIMS Interface 6.6.1. Introduction LIMS Interface NIRWare LIMS Interface offers the possibility to link the NIRWare Software Suite to a LIMS. With this interface, job data from a LIMS can be transferred directly to the NIRWare Operator and measurement results are passed over to the LIMS. Job data with all necessary information (application name, batch information, sample description, ...) will be written into a file by the LIMS and stored in the Inbox.
NOTE The LIMS settings will be saved per PC, so that all settings will be reset to default when the PC name is changed. 6.6.2. General Options Here, general output options are listed. To open it, in the file tree on the left side of the NIRWare Management Console select LIMS Interface - General or click General Options in the submenu list in the center. NIRWare 1.
Parameter Name Description Inbox Path for the input files. The Operator receives the LIMS jobs from this folder Outbox Path for the output files (result files) Type of Job selection Selection mode of the LIMS jobs: Use LIMS Export Oldest first Newest first Manual file selection Activate the export function (per default this function is deactivated).
Parameter Name Description Enabled Enabled digital signature Crypto Service Type of Crypto Service used Hash Algorithm Type of Hash Algorithm used Public Key The public key if for the recipient. It is needed to check if the digital signature is un-changed.
Parameter Name Description Format Defines the file format used (XML and CSV) File extension Defines the extension of the import file Ignore redundant lines in input file In case the maximum number of samples in import file exceeds the number of samples possible for the application/instrument configuration (redundant lines): checked = redundant information is ignored for import unchecked = redundant information results in a warning message and the import is canceled Use Unicode Defines whether the
CSV file import Parameter Name Description Format Defines the file format used (XML and CSV) File extension Defines the extension of the import file Separator Separator used Ignore redundant lines in input file In case the maximum number of samples in import file exceeds the number of samples possible for the application/instrument configuration (redundant lines): checked = redundant information is ignored for import unchecked = redundant information results in a warning message and the import i
For this purpose, a double-click on the sample name field will fill all the other used fields in ascending order. A double-click on the 1. property field will automatically fill all other used fields including their position number.
Parameter Name Description Format Defines the file format used (XML and CSV) File extension Defines the extension of the export file. Please omit the dot (e.g. xml instead of .xml Use Unicode Defines whether the export file is coded for Unicode. For XML this is standard. Unicode is necessary for all languages that have an expanded character set (e.g. Asian languages) NIRWare Field Available fields for export Used Defines whether the field is used.
Export XML schema The XML schemas of import and export are located on the NIR Software Suite CD in the folder 'fscommand\Operation_Manuals\LIMS Schema'. CSV export file Select the fields that should be shown in the export file. Parameter Name Description Format Defines the file format used (XML and CSV) File extension Defines the extension of the export file Separator Separator used Use Unicode Defines whether the export file is coded for Unicode. For XML this is standard.
are line separated lines (one line for each property) Number of properties Number of properties (results) in export file (visible in case the function "Multiple Properties are line separated" is not active) NIRWare Field Available fields for export Position Position of the field (as it appears in the export file). All used fields must have a well defined position. Used Defines whether the field is used.
NOTE: If the configuration in the LIMS Interface is changed, the Operator and the Control System Service have to be restarted.
Found SubstanceID Text I found substance ID (equals first entry in the hitlist; if no substance ID was found, the entry remains empty) Identification OK Integer I see description above Residual Double I residual of prediction result Distance Double I distance of prediction result MaxAllowedResidual Double I maximum allowed residual MaxDistance Double I maximum distance PropertyName Text Q name of the property PropertyPredictedValue Double Q prediction result PropertyUnit Tex
6.7. Library Designer 6.7.1. Introduction Library Designer For identity control in the warehouse it is not always necessary to work with chemometric calibration methods such as Cluster or SIMCA. When sample identification is needed, often a comparison of spectra leads to good and reliable results, is much easier to handle and requires only little reference analysis. The NIRWare Library Designer serves to create and administrate spectra libraries for spectra comparison.
You can now open a submenu by clicking on their names in the file tree or in the center of the Library Designer window. 6.7.2. Creating a new library To create a new library proceed as follows: In the file tree on the left side of the NIRWare Management Console select Library Designer – New or click New Library in the submenu list in the center. The following dialog opens: NIRWare 1.
If necessary, narrow down the information displayed in the table, using appropriate filter settings. In case you do not see the samples contained in the database in the lower table, click the grey cell in the Timestamp column with the right mouse button.
The library will now be added to the tree view on the left side under the menu Open and three additional submenus are assigned to it: Spectra, Validate Library, Library Test. NOTE The library can only be saved when a library name and a template spectrum was defined.
Method formulas Maximum Distance of 2nd Derivative Maximum Distance NOTE To use this algorithm there must be at least 3 spectra of the same property inside the library.
Library window Additional library parameters As soon as a new library is saved, it can be opened via the tree view on the left of the Management Console and three additional parameters are added to the upper parameter list: Valid: When this check box is activated the library has been validated Number of Substances: Number of substances within the library Number of Spectras: Number of spectra within the library Spectrum template parameters Sample Name Name of the sample Property Name Name of the determ
Optical Resolution Optical resolution of the instrument used for measurement Datapoint interval Resolution of datapoints used for the measurement Lower wavenumber limit Lower wavenumber limit of the range within the spectrum was measured Datapoints Datapoint used for spectrum measurement Time Stamp Date and time the spectrum was measured 6.7.3. Spectra After the library has been initially created, qualitative spectra have to be selected to built up the library.
The tables comprise the following columns: Sample Name: Date and time the sample was measured and name of the sample Property Name: Name of the property Time Stamp: Date and time the sample was measured Scans: Number of scans with which the sample was measured Resolution: Resolution with which the sample was measured Comment: Optional comment to the sample Spectrum ID: ID of the sample spectrum To be able to assign spectra to your library, you first have to set the corresponding library to the Lifecycle s
To be able to change the library parameters, you first have to set the corresponding library to the Lifecycle state "Editing". For this purpose, click the Edit DataSet icon 6.7.4. . Library Spectra Viewer By means of the Library Spectra Viewer the spectra saved in the library can be displayed. 286 NIRWare Suite NIRWare 1.
6.7.5. Validate Library Before the library can be used for routine operation it has to be validated to ensure a clear separation of all samples from each other with the chosen settings (wavenumber selection, Method formula, distance limit). To open the corresponding window in the file tree on the left side of the NIRWare Management Console select Open, click on the name of the library which you want to validate, then select Validate Library. The following dialog opens: NIRWare 1.
The window contains a list of all libraries in the database.
Distance limit of the library Limit value defining the maximum allowed distance between a given/measured spectrum and the most similar spectrum within the library. The value depends on the method formula selected for prediction and is defined in the library parameters. Maximum distance into one substance Describes the maximum difference between different measurements of the same substance. NOTE The values might be different depending on the method formula selected. 6.7.6.
The Library test window contains a table listing all samples contained in the database. In case the tables is empty, click the grey cell in the Timestamp column with the right mouse button.
The column titles have the following meaning: HitList Property name (the name of the property with the closest distance to the predicted spectrum is the first in the column) Found substance Name of found substance If the name of the found substance in the hitlist matches the name of the expected substance, it will be marked with 'OK' , otherwise a red X is displayed. Distance allowed Allowed distance of checked spectrum to the "hitlist" spectrum in the library.
6.8. Lifecycle 6.8.1. Lifecycle introduction NIRWare has been designed to comply with 21 CFR Part 11. The Lifecycle model is the core of this compliance. The Lifecycle approach enables to control the user access to the NIRWare software, transitions from one lifecycle state into the other and to keep a history of actions done (Audit Trail). The following picture shows the principal lifecycle configuration. There are three relevant modes: 1.
Electronic records can be transferred into the next phase actively only. The user needs to save the electronic record and put it into the next stage. 6.8.2. Lifecycle states In the lifecycle model there are four principal states for the data sets. Created In this state new data sets are generated and edited or developed, optimized. Two modes need to be differentiated: principally the data set is in the read-only mode. For editing it is necessary to press the Edit icon.
Disabled The data set is no longer in routine use. It is read-only and in a frozen mode. State Not Created Description No lifecycle data set is defined. Read only mode Created A lifecycle data set is defined. Read only mode Editing This state allows editing by pressing the Edit icon. A lifecycle context is defined Write mode Checked A lifecycle data set is defined. Read only mode in the templates ER and ERES.
Pressing this icon puts the data set into the next lifecycle state. Discard Discard Pressing this icon discards or aborts the Edit session. Delete Data Set Delete Pressing this icon deletes the data set Action Condition New Created The data set is the read-only. Edit Created Changes to Write mode. Save Created Changes to read-only mode. Allows the user to save the data set Save Checked The data set remains unchanged. The read-only mode remains. Used to change the User.
From state Checked To state Action Created Copy Audit Trail Log: Reason Checked Save Audit Trail Log: User changed Approved Next state Audit Trail Log: ready for routine use LC Condition: Checked disabled Delete Delete Audit Trail Log: Deleted From state Approved To state: Action Created Copy Audit Trail Log: Copy reason Approved Save User changed Disabled Delete No longer in routine use From state Disabled to state: Action Checked Copy Reanimate for testing Approved Next Stat
Example: Lifecycle transitions using Template Unregulated. In Lifecycle Unregulated there is no Checked state, the application is set to Approved by clicking Next instantly. NIRWare 1.
6.8.5. Lifecycle templates The requirements for various industries are very different. Only GMP relevant areas of the pharmaceutical industry must comply with all requirements of 21 CFR Part 11. On the other hand there are industries, which are not affected by these requirements at all, e.g. Food&Feed industries. In order to simplify the use of the implemented lifecycle model, there are three pre-defined templates available, which fulfill various requirements.
Delete Edit Approved Edit Save Disabled Copy Next Not created New Deleted Delete Electronic Records Most transitions do need just a comment and no formal electronic signature. Again the checked state is missed out. There are various Audit Trail entries. However electronic signatures are not needed. With this template it is possible to edit the lifecycle data sets in the Approved state as well.
Disabled Copy Next Electronic Records/Signatures This template covers all requirements of 21 CFR Part 11. An electronic signature is required for all phase transitions. Going from the checked state into the approved sate, the electronic signature must be given by a different person (Constraint Signature). When signing electronically it is mandatory to enter a comment giving the reason for the action. Everything is documented in the Audit Trail. Editing is allowed only in the Create state.
Custom Settings If users do have special requests BUCHI can provide a customized template, which will be tailor made to the customers specifications. It can be imported into NIRWare via the import functions. 6.9. Administration 6.9.1. Installshield Update Service Update over Internet is discontinued with NIRWare 1.4. 6.9.2.
Icon indicating that the BUCHI Control System is running Icon indicating that the BUCHI Control System is stopped To quit the Control System Service: double click the Icon in the SysTray Click "Stop the ControlSystem Service" Close the User Interface "BUCHI ControlSystem Service" Click with the right mouse the Icon in the Systray (e.g.
The Control System is designed to act as a background service in a Microsoft Windows operating system and starts automatically when the operating system is started. The purpose of the Control System Service is to establish the communication between the spectrometer and the PC. The Control System tries to locate the configured instrument and establishes a connection. 6.10. System test 6.10.1.
Temperature Several temperature sensors are provided within the spectrometer. Temperature is checked at the following positions against reference values: wedge drive, instrument, laser and main board and, depending on the measuring cell, detector, detector board, application board. For every sensor a lower and upper limit value is predefined. The SST for temperatures is passed, when all temperatures are between the lower and the upper value.
7. NIRWare Operator 7.1. Menu: Introduction Operator Windows Start / Programs / BUCHI / NIRSolutions / Operator Icon: Start the application by clicking the Icon for the Operator or using Start Menu. When prompted type in User and Password into the Logon dialog. Icon description: Starts a measurement sequence (F2) NIRWare 1.
Stops the current running Operator process (F3) Opens the "Delete Samples" menu (only in use with applications for data aquisition (no calibration assigned) Close Batch Opens the Logon Dialog to change user.
7.2. Tab Overview For the measurement cells Solids (with Petri and XL Add-On), Fiber Optic Solids and Fiber Optic SMA the so called tab overview is the default screen in the NIRWare Operator. By clicking either on or NIRWare 1.5 Software Manual you will find a detailed result window popping up.
The Detailed Result window shows the predicted value for the last measurement (in case the “Number of measurement sequences" is > 1). When changing from Overview to Results, you will see the results of the individual measurements and the average values. 308 NIRWare Operator NIRWare 1.
7.3. Operator Wizard In addition to the standard NIRWare Operator a simplified version is available, where an Operator Wizard will guide you through the process of application selection, batch, sample naming etc. The Operator Wizard is available for the measurement cells Solids (with Petri or XL Add-On), Fiber Optic Solids and Fiber Optic SMA. The NIRWare Operator can be launched from the Start menu. NIRWare 1.
In the NIRWare Operator icon bar click the binocular to start the Operator Wizard. Select an application. Create a new batch or choose an existing one. Enter all information that was selected in the Management Console (e.g. Analysis ID). 310 NIRWare Operator NIRWare 1.
Confirm your settings in the final overview. The application will be loaded and the measurement can be started. NIRWare 1.
NOTE The Operator Wizard contains no menu bar. That means e.g. that it is not possible to measure an external reference manually. 7.4. Select Application Clicking the Icon opens a dialog with all accessible applications. NOTE Depending on the logged on user the list can differ. The default access restrictions for the user group "Operators" is set so that only applications which are in the lifecycle state "Approved" can be selected.
Selecting an Application which is in the Lifecycle State Created the following message appears. 7.5. Deviating reference spectrum 7.5.1. Introduction Spectral references are used to compensate for signal drift and other unwanted effects that could compromise the measured spectra. This is best done by using the ‘External Reference’, because it is measured at exactly the same position as the sample. NIRWare now offers an improved automatic test of the measured spectrum.
The graphic enables to compare both spectra, so that experienced users can get an idea about the cause of the observed deviation (see Tips and Tricks section). Furthermore, helpful information is given in the green column on the left-hand side of the dialog. The user can now decide on how to proceed: Pressing the red X button will discard the ‘new reference’ spectrum, and abort the measurement.
NOTE: By default, only administrators are allowed to give the signature for acceptance. Everyone else will get an error message. -This security setting can be configured within the Mangagement Console under Security Designer – Security Policies: Acceptance of External References. 7.5.3. Tips and Tricks Frequent causes for deviations Temperature drift The performance of lamp, detector and electronics is influenced by the temperature.
Interpretation of the spectra in the example above The two spectra shown in the picture further above show pretty similar max. intensities (ca. 85.000 vs. 90.000 AU); furthermore, we can see an extra band at around 6.000 1/cm, and around 4.500 1/cm; in addition, the curves are well separated from each other in the range of 4.000 – 4.500 1/cm. These extra bands hint an extra material in the optical pathway as most probable cause of the observed spectral deviation, rather than just a simple temperature drift.
If the test passes, the Operator loads the job, starts the corresponding application and fills in the selected fields in the input mask. All fields activated for LIMS should be also activated in "Operator Configuration - Sample Description Fields". To start the measurement, click the "Start" button . During the measurement the import file is locked. If the measurement is interrupted no export file will be generated.
This input will automatically be fractionated into the following fields: 318 NIRWare Operator NIRWare 1.
Please note that “11111” was automatically translated into “Sucrose” as “Expected Substance” by means of the respective PropertyID. 7.8. Service module 7.8.1. Introduction to the Service module Menu: NIRWare Operator / Advanced / Service Icon: NIRWare 1.
The Service module is intended mostly for a service engineer to see and change instrument parameters. The default setup only allows the User "Service" with the corresponding password access these advanced functions of the service module.
The screen shot above is an example when the cover of the laser module was opened. To reset the sensor of the laser click the Reset icon. To reset the lifetime counter of the laser click the Start icon. Device Configuration The TCP/IP address of the instrument (NIRFlex N-500) can be changed from default (192.168.1.1) to any other address.
Reports Calibration Parameter Hardware parameters of the instruments can be seen, printed or exported, e.g. to pdf. Click on 7.8.2. Menu: to open the report view. Changing the instruments TCP/IP address NIRWare Operator / Advanced / Service / Device Configuration Icon: Every NIRFlex N-500 has the static IP-address 192.168.1.1 (Subnet 255.255.255.0) per default.
NOTE In order to change the static IP-address of the NIRFlex N-500 (e.g. to the local requirements of the IT) the communication between PC and NIRFlex N-500 must be established. The user needs administrator rights on the OS. 1. Select Device Configuration 2. Select the Host tab Edit the new IP-Address of the spectrometer and click the OK button. 3. Select the Device tab Edit the new IP-address of the spectrometer including the Subnet mask again and click the OK button. 4.
Reconnect the control system afterwards in order to establish the connection. NOTE The configuration of the instrument IP and the connection information in the database have to match. To connect to a different instrument, it will be necessary to edit the connection information in the database under Administrative Tools (NIRWare Management Console), NIRWare Config so that the Control System service connects to the new address.
As soon as the primary lamp has been replaced, the described steps should be followed and the system should be switched back to the primary lamp. For this purpose, open the following dialog and click the button Activate Primary Lamp. To reset the Primary lamp counter, see also Resetting the lamp lifetime counter. 7.8.4.
As instrument covers must be opened to replace the lamp or the laser, the sensors of the cover need to be reset in the Service module as well be means of Assembly Setup. See Running an instrument setup Click the icon Reset primary lamp counter to set it to 0 hours. Confirm the following security message by clicking OK. 7.8.5. Running an instrument setup During the initialization process, the instrument recognizes when a cover was opened and the following message appears.
Reset every position by clicking the Reset icon . The following message appears: Confirming it by clicking the green check mark button. After you have reset every parameter marked with the red frame around the name field, leave the Assemblies menu by clicking the Back icon twice. The Initialization process continues until the Instrument icon changes to green NIRWare 1.5 Software Manual .
8. Server installation of a database 8.1. Typical installation scenarios 8.1.1. Standalone In this scenario the PC is directly connected to the N-500, but to no other network device. PC configuration: Database Free, but limited SQL Server SQL Express 2005 version, installed locally Licenses Installed and used locally Network Cable: crossed! Adapter: IP-address: 192.168.1.2 Subnet mask: 255.255.255.0 Data security Burn database backups on several DVDs in regular intervals, e.g.
The following PCs are involved: PC name Role Used software PCMeas Measurements - NIRWare Operator PCQuality Quality Control - NIRWare Management Console - NIRCal PCDevAdmin Calibration development - NIRCal - NIRWare Management Console Administration Users, Backup PCQuality configuration: Database Located on database server: SrvDB Licenses NIRCal / NIRWare Network Cable: straight 330 Server installation of a database NIRWare 1.
Adapter: IP-address: Obtain automatically Subnet mask: Obtain automatically Data security solved on database server PCMeas configuration: Database Located on database server: SrvDB Licenses NIRWare Network Cable: straight Adapter: IP-address: Obtain automatically Subnet mask: Obtain automatically Connection to N-500: Cable: crossed Data security solved on database server NIRWare & N-500 N-500's IP-address: NIRWare Management Console > Administrative Tools > NIRWare Config > Connection Info: 192
8.2. Worldwide connected N-500 network This scenario describes a company with a headquarter and several production sites around the world. The plants work with local databases. The DB's in the plants are backed up periodically. Then the template database with actual applications at the headquarter is transferred to all plants. NIRAnywhere takes over this function. BUCHI has contract specialists, who do this in cooperation with the customer’s IT.
9. NIRWare Database Manager 9.1. NIRWare Database Manager 9.1.1. Introduction Because the use is restricted to qualified personnel only, just a few functions are explained. Qualified personnel are certified MS SQL Server administrators or developers. 9.1.2. Main window of NIRWare Database Manager When a database is selected the main window looks as follows: NIRWare 1.
9.1.3. Restore database To activate the restore function, click Restore... on the right of the main window with a database selected. The following window opens: You have two possibilities for a restore: 334 NIRWare Database Manager NIRWare 1.
Restore to default database: When this radio button is activated, the currently selected database will be overwritten with the content of the backup when clicking OK. Restore to new database: When this radio button is activated, you have to enter a unique and valid name for the new SQL database. The content of the backup is then copied to this new database when clicking OK. This function is not available via NIRWare. NOTE After the restore of a databases from an earlier NIRWare version (less than 4.
