Creating a Typical Application and Measuring Unknown Samples

Creating a Typical Application and Measuring Unknown Samples Creating New Applications Filling in the Application Window Launch the Epsilon software. 1. From the Main menu: • Select Application • Select New application. 1. Select the type of sample to be analyzed, Solid for this application. 2 Adding Elements of Interest Adding Flux used Applying Condition Sets 1. Elements can be selected from the periodic table. In this case we will use the pure element forms. Elements of interest in this application are: Al, Si, Ca, Ti, and Zn and C which represents the balance CH2. To display the periodic table, click on . C can only be entered manually. 1. It is important to indicate whether a flux has been used, as well as the formula and weights or volumes of the substance used. These are taken into account in the calibration calculations. In this example, Lithium Tetraborate (Li2B4O7) was used as the flux in a ratio of 1 g sample to 4 g flux having a final weight of 5 g. You may also need to account for LOI (Loss on Ignition). The condition sets are proposed automatically, but can be changed afterwards. 2. Once the elements are selected they will be added to the application window. Following selection, several options are activated. 2. Type the name of the new application, in this case Additives in PE. 2. In polymeric applications, a Balance is often required. 3. Select Create New. 3. Also enter the time that the sample is to be analyzed for each condition set under Meas Time (for example 100 s). Measuring Standards Adding Standards 1. Enter the names for the standards used. Add all standards to the list by typing in the name and clicking on . 1. To optimize the conditions, click on Optimize Conditions and follow the instructions. 2 2. Save the application. 3. Click on Standards to move to the standards screen. 2. Fill in the known concentration values for each standard. Deconvolute Spectra 1. Prior to measuring the standards, press the Calculate Default Line Groups icon. 2 3. Save the standards data. 2. Highlight the first standard by a single mouse click. Calculated Linear Regression 2. Once the table is highlighted follow the sequence below: a. Press . 2. Matrix correction model c. Press 2 4. Indicate in which position the sample is located by clicking on the sample position. Repeat this process for each standard. This window is used to view, modify and measure the calibration standards for an application. The names of the standards, and the concentrations of the various compounds (along with dilution and loss on ignition information if required) are all contained on this window. It is also possible to view (but not modify) the raw or corrected intensities for the standards. Calibration Data 1. Arrows to move from element graph to element graph. 1. Arrows to move to the next or previous element. 2. Calibration graph statistics. Note: To exclude a flyer, left-click on the point, then right-click for the pull-down menu to select Toggle Quality. 3. D = Intercept 2. Icons to move you back to the Application window, Linear Regression Calculation window and the Standards window. 4. E = Slope To obtain an element calibration report, click on 2 b. Press . When you are asked to set the alphas to zero: Click Yes. 2. Click the Calibration calculation button. Calibration Graph 1. RMS = Standard error Correlation = Goodness of fit 1. Click the cell Channel to highlight the entire table in blue. 1. Save the standards. Note what position each standard is located in on the sample tray. The cover can also be left open during this operation so that you can see the sample location. 3. Click the Measurement icon. Calculating the Linear Regression 2. Al and Si will be measured on the condition. Ca and Ti will be measured on the condition. Zn will be measured on the condition. Note: CH2 must be entered as compound name. Optimizing Conditions 1. The Condition Name column specifies the condition conform which each element must run. . 3. Calculated concentration base on the calibration graph. 4. Chem = chemical concentration. 5. Diff = calculated concentration - chemical concentration. 6. Matrix correction factor being applied. . 5. Once all the calculations are complete click on the individual calibration graphs. to view RMS = Average Standard Deviation of all Points. Element of interest Measuring an Unknown Sample Test the calibration by measuring one of the standards as an unknown against the calibration. 1. Select Measure > Measure application from the menu. 2. Select the application of interest, in this case Additives in PE. 3. Click OK. Measuring an Unknown Sample (continued) 1. A measurement window will open, type in the sample identification. 2. Once all the information is correct select Measure. 3. Select the position that the sample is located in on the sample tray. This will start the measurement. Measuring an unknown sample (continued) Results are shown for the measurements of Unknown 1 sample. Note: The application repeat factor is set here to 10. Epsilon 4 Quick Start Guide Typical application 4023 000 67901 Edition 1 ©2017 PANalytical B.V. All rights reserved