Quantitative Spectroscopy Chapter 3 Software

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1 Quantitative Spectroscopy Chapter 3 Software Copyright 2006 Mettler-Toledo AutoChem, Inc. 1

2 Chapter 3 Outline P-matrix P-matrix with automatic frequency select PLS: Choosing a region PLS: Selecting the appropriate number of factors Putting the quant into service, monitoring reaction concentrations MonARC: Uploading the calibration ReactIR ic 10, exporting spectra to the spc format, importing calibrations in the cal format. Quantitative analysis software / hardware summary 2

3 Introduction to QuantIR Example: Measure ethanol dissolved in acetone over a range of 2% to 25%, with a worst case accuracy of 0.35% by weight. 3

4 Introduction to QuantIR Concentration of ethanol (ideal)% Concentration of ethanol (actual)% Function (Cal or Eval) Cal and and Cal Cal Cal and Eval Cal Cal Cal and Cal 4

5 Introduction to QuantIR Collect all of the spectra using ReactIR 3 software. Save the spectra in the spa format. 5

6 Introduction to QuantIR Open the QuantIR application and select File. Give the quant a name and click OK. 6

7 Introduction to QuantIR Select initial standards for the quant. 7

8 Modify Menu: Calibration Type From the Modify menu, select Calibration Type 8

9 Modify Menu: Calibration Type Under Calibration type, select Inverse Least Squares [P-Matrix]. Under Correction, select None. Click OK. 9

10 Modify Menu: Pathlength In the Choose Pathlength Option window, select Constant then click OK. 10

11 Modify Menu: Standards In the Quant Standard Selection window, use the Add and Remove buttons to select standards from the calibration. 11

12 Modify Menu: Components From the Modify menu, select Components. Type a component into the Enter components: field and click Add. 12

13 Modify Menu: Units For each Component, enter a Unit (e.g., % wt/wt) IMPORTANT! To make the change permanent, be sure another cell is selected before clicking OK. 13

14 Modify Menu: Concentrations 14

15 Display: Standards From the Spectra menu, select Display Standards 15

16 Display: Standards Select between one and five spectra and click OK. 16

17 Display: Standards 17

18 Modify: Peaks and Regions From the Modify menu, select Peaks/Regions then select Edit Current Peak Graphically. 18

19 Modify: Peaks and Regions Use the arrow to select three height to zero points to use for the calibration. 19

20 Modify: Peaks and Regions 20

21 Calibrate From the Calibration menu, select Calibrate now. 21

22 Calibrate Predicted-vs-Actual plot 22

23 Calibrate Predict quant standards. Quant Name: Unnamed quant as of 16:53:30 Calibration type: Inverse Least Squares (P-Matrix) Post calibration correction: None Pathlength option: Constant Peaks/Regions: Pk.Start Pk.Stop B.Start B.Stop Type Height to zero Height to zero Height to zero Height to zero Results of predicting quant standards: Standard: 0.99 ETOH Actual Calc. Error PctErr Component Ethanol (%) Standard: 3.61 ETOH Actual Calc. Error PctErr Component Ethanol (%) Standard: ETOH Actual Calc. Error PctErr Component Ethanol (%) 23

24 Leave One Out: The Beginning of Validation From the Validation menu, select Leave one out 24

25 Leave One Out: The Beginning of Validation The Leave One Out plot is accompanied by a table. 25

26 Leave One Out: The Beginning of Validation Peaks/Regions: Pk.Start Pk.Stop B.Start B.Stop Type Height to zero Height to zero Height to zero Height to zero Leave one out Cross-Validation results: Standard: 0.99 ETOH Actual Calc. Error PctErr Component Ethanol (%) Standard: 3.61 ETOH Actual Calc. Error PctErr Component Ethanol (%) Standard: ETOH Actual Calc. Error PctErr Component Ethanol (%) 26

27 Run Current Quant: Used for On-Going Validation From the Run menu, select Run current quant 27

28 Run Current Quant: Used for On-Going Validation Run current quant. Quant Name: Ethanol in Acetone Calibration type: Inverse Least Squares (P-Matrix) Post calibration correction: None Pathlength option: Constant Peaks/Regions: Pk.Start Pk.Stop B.Start B.Stop Type Height to zero Height to zero Height to zero Height to zero File: ETOH Ethanol (%) 28

29 Autofrequency Select: A Tool for P-Matrix Models From the Modify menu, select Automatic frequency selection 29

30 Autofrequency Select: A Tool for P-Matrix Models Set the maximum number of frequencies to n/2+1 or n/2+2, where n is the number of calibration standards. 30

31 Autofrequency Select: A Tool for P-Matrix Models Graphically select the region for the algorithm to search. Run the quant on the 12.01% sample. 31

32 PLS Return to the Modify menu and select PLS Parameters 32

33 PLS: Choosing Regions From the Modify menu, select Peaks/Regions 33

34 PLS: Choosing Regions In the Peak Type pull-down menu, choose Region to zero and then Edit Current Peak Graphically. 34

35 PLS: Choosing Regions The region we have chosen contains a lot of information relating to ethanol, acetone, and the baseline. 35

36 PLS: Choosing the Appropriate Number of Factors From the Diagnostics menu, select PRESS. In the PRESS window, select Plot. 36

37 PLS: Choosing the Appropriate Number of Factors 37

38 PLS: Choosing the Appropriate Number of Factors Return to the Modify menu and select Number of Factors. Enter a value in the NumFactors box based on what the PRESS indicated. 38

39 PLS: Choosing the Appropriate Number of Factors Save the method, close QuantIR, and open ReactIR

40 Using the Model to Monitor the Component s Concentration in a Reaction 40

41 Using the Model to Monitor the Component s Concentration in a Reaction From the Analyze menu, select Post Process 41

42 Using the Model to Monitor the Component s Concentration in a Reaction In the Post Process window, click View Sequence. 42

43 Using the Model to Monitor the Component s Concentration in a Reaction Right-click on the REACTOR 1 icon (located underneath the COLLECT icon). 43

44 Using the Model to Monitor the Component s Concentration in a Reaction Select Add Quant. 44

45 Using the Model to Monitor the Component s Concentration in a Reaction Browse to the directory containing the quant, select the quant, and click Apply. 45

46 Using the Model to Monitor the Component s Concentration in a Reaction Right-click on the DISPLAY icon and select Add Profile Display. 46

47 Using the Model to Monitor the Component s Concentration in a Reaction Select a profile by highlighting it in the Profile Sources box and using the right-pointing arrow to move it to the Profiles Selected box. Enter a name in the Window Name box. Click the Apply button and close the window. Answer Yes when asked if you want to make the changes. 47

48 Using the Model to Monitor the Component s Concentration in a Reaction In the Post Process window, click Run. 48

49 Using the Model to Monitor the Component s Concentration in a Reaction This is the profile of the ethanol concentration in the reaction. 49

50 Uploading the Method to the MonARC system 1. Open the Remote Configuration Tool (RCT) 2. Choose Manage and log in 3. Download archived spectra (calibration and validation spectra) 4. Build calibration / save calibration. 5. Attach QuantIR model to processing and upload to MonARC. 6. Subsequently collected spectra will be analyzed and the results will be reported for instance via TCP / Modbus 50

51 Exporting from icir software (ReactIR ic 10) to SPC file format (Grams) 51

52 Selecting and configuring CAL file to run on reaction in ic IR 52

53 Quantitative analysis software / hardware summary MonARC 1. Download SPA files 2. Build model in QuantIR 3. Upload model to MonARC ReactIR Save spectra as SPA files 2. Build calibration in QuantIR 3. Convert calibration to MTQ file 4. Attach MTQ to processing 53 ReactIR ic Export SPC files 2. Build calibration in Grams (CAL file) 3. Import CAL to ic IR software

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