Analysis and modelling of dielectric relaxation data using DCALC

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1 Analysis and modelling of dielectric relaxation data using DCALC Short course, Lodz, 8 October 2008 Part II structure of DCALC, data import/export, graphics, quick analysis

2 Schedule 1 st session (8 October 2008): 1) A brief introduction into DRS including dielectric relaxation theory, presentation of dielectric relaxation data in f- and T-domain, empirical relaxation functions and their temperature dependence (~ 45 min). 2) Presentation of the internal structure of DCALC, import/export of data, 2D and 3D graphical presentation capabilities and quick data analysis, example: PVAc. 2 nd session (9 October 2008): 3) General fit-functions in the frequency domain, Fit-functions and options in DCALC, demonstration case PVAc or P2VP 4) "Hands-on" session (Please bring your own laptop with you and have DCALC installed and tested in advance) 3 rd session (date t.b.a.): 5) Advanced numerical algorithm of DCALC: 1D and 2D derivatives, KK-transform, conductivity analysis 6) Fits using ε der and fitting in temperature domain; 2D-fits and temperature depending HNparameters

3 Start of the program Run DCALC.EXE Opening screen 3 resolutions available: SVGA (800x600) VGA (640x480) Welcome to DCALC 4.1 Last version 4.1 (2008): XVGA (1024x768)

4 Setting up the DCALC environment Program directory: c:\dcalc41\ Templates, examples: c:\dcalc41\examples\ Here, focus on Dielectric Measurements (Diel) Directory content: Various file types in DCALC: *.DAS Single sweep data file *.DAT Data file, multiple spectra (e.g. diff. temperatures) *.PRE Dcalc settings file, DEFAULT.PRE Welcome to DCALC 4.1 *.GRS Graphics settings (2D, 3D presentations) *.PAR Fit parameter file (in \PAR\) *.TAU Relaxation times (columnar format) *.TXT Text file, e.g. Windeta ASCII data

5 User management Recommended: Main user directory on HD data partition User record contains: User name Directory Measurement configuration Date and time of last call Last settings file used (*.PRE)

6 User management User data in USER.DEF 6 Last user number Discotic (1 st ) User name d:\users\yildirim\ DEFAULT.PRE :53:49 PEN new D:\USERS\PEN\ DEFAULT.PRE :15:43 Theo D:\USERS\BOSMA\ DEFAULT.PRE :44: 8 PS-films D:\USERS\PS-FILMS\ DEFAULT.PRE Directory Last settings file used (*.PRE) Measurement configuration Date and time of last call

7 Selection of measurement configuration Default for DRS meas.: 4 also for Alpha analyser Here, the specific hardware configuration will be chosen: Dielectric i spectroscopy (1 5, 7 9) TSD (6, 13) LIMM (10) General photothermal experiments (11, 12)

8 Main menu Menusystem toplevel: File Configuration Fit Data Print Window Utilities Important function keys: <F1> Help <F9> View logfile <F10> Top menu <Alt+X> Exit program <Alt+G> 2D plot

9 Main Configuration Measurement mode (default: 4 = DRS) Sample parameters: Sample dimensions, electrode type, description

10 Main Configuration Table: temperature list Table: frequency list

11 Main Configuration File read options: Numeric operations during reading of data file (Fxxx) or during graphics rendering (Gxxx) - optional: parameter, e.g. filename

12 Main Configuration Graphics output devices: - Screen (default) - Screen + screen dump as Bitmap (BMP) file (2 nd option) - All other options: vector graphics (HPGL format), suitable printing by a plotter or PCL5 compatible printer BMP: Automatic numbering BMPxxx.BMP

13 Main Fit Contains all program functions related to data fitting: - Selection of spectra (or ε (T)-curves) - Select fit function in frequency or temperature domain - Fit options, set fit (start) parameters and constraints Computation of relaxation time data τ(t) and their fit to Arrhenius or VFT-law: - Tau-data by NNLS-fit (e.g. Havliliak-Negami function) or by model-free peak analysis ( Master curves ) - Arrhenius plot: fit of tau-data to Arrh. or VFT - Graphical or numerical representation ti of fit data - Write/Read fit parameters to text file

14 Main data Read data: Read data file (*.DAT-format) Import data from various text formats Read and compare data from multiple files Other functions: View raw data in tabular format Graphical representation: 2D plot ( View curves ) <Alt+G> Plot settings (define axis) 3D plot Processing of selected curve (e.g. peak search, filtering) Preset plot: Temperature profile

15 Internal data structures Txt-file, *.DAT-format time (f-list) Frequency (f 1 f Nf ) Operation: Load curve function for fit or display others Time (T-list t) NT Temperatu ure T 1 T N Eps (f,t) Eps (f,t) Nf NT matrix or eps (T,f i ), eps (T,f i ) eps (f,t i ), eps (f,t i ) Graphics processing: Gy 1 (Gx 1 ), Gy 2 (Gx 2 )

16 Reading and displaying a DAT-file

17 Reading and displaying a DAT-file Selection of spectra or isochronal scans Next: demonstration

18 Test case 1: PVAc What we are doing next? View sample information and T-profile Display data in frequency domain selected presentations Create 3D-views Quick analysis peak relaxation times in ε or dε /dlnf f Arrhenius plot of relaxation time data, fit with Arrhenius or VFT-law Export results

19 PVAc: sample info and T-profile Data file: PVAC8-1.DAT Status window File info Measured in heating Freq.-range: 0.1Hz 10 MHz High data quality 2 processes: α-relaxation, l β- process (weak)

20 PVAc: 3D representations eps eps eps : 3D surface + 3D contour lines Same data, different color schema: gray scale

21 PVAc more 3D representations Image plot Contour plot α-peak Very special feature of DCALC: Presentation of local minima (+) and maxima (o) in frequency spectra β Here, both the α and β-peak are detected

22 PVAc Quick analysis Menu: Fit Master plot

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