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Calibration-TR-Characterization of Cd primary and secondary reference materials

Calibration-TR-Characterization of Cd primary and secondary reference materials

Calibration-TR-Characterization of Cd primary and secondary reference materials

Product catalog summary
Introduction
This report details the characterization of new Cadmium (Cd) primary and secondary reference materials. Three new Cd primary reference standards in the form of foils were produced and used to create secondary reference standards.

Experimental Details
The primary reference materials were produced using gravimetric measurements and the XRF fundamental parameter method. XRF measurements were conducted using a Fischerscope XDLM device. The primary standards were measured over a 50mm x 50mm area using a 25x25 matrix of 625 spots, while secondary standards were measured over a 2mm x 2mm area using a 4x4 matrix of 16 spots. Key parameters included a voltage of 50keV, a Ni 10 µm primary filter, and an anode current of 300 mA.

Data Analysis and Results
Heatmaps indicated thickness gradients or inhomogeneous distribution in the primary standards. A linear regression analysis using R was performed to correlate gravimetric and XRF measurements. The results showed discrepancies between the two methods, summarized in Table III. The regression was used to calibrate the XRF values for secondary standards, with results summarized in Table IV.

Conclusion
The study successfully characterized the Cd reference materials, providing calibrated XRF values for secondary standards based on primary standards' measurements. This calibration is crucial for ensuring accurate and reliable measurements in future applications.
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Catalog excerpts

Calibration-TR-Characterization of Cd primary and secondary reference materials-1

HELMUT FISCHER GMBH INSTITUT FUR ELEKTRONIK UND MESSTECHNIK Fischer Traceability Report JL-2013-10-Cd Abstract: Three new Cd primary reference standards (Cd foils) have been produced and used for the production of new Cd secondary reference standards. Experimental details Primary reference material (self-supporting Cd foils) has been produced on the basis of gravimetric measurements and data from the universal standard free XRF fundamental parameter method. XRF measurements have been carried out using a Fischerscope XDLM. The experimental XRF parameters are summarized in Tables I and II, for the measurement of the primary reference materials and the secondary reference standards, respectively. For the measurement of the primary standards a 25x25 matrix of 625 equidistant measurement spots covering an area of approx. 50mm x 50mm were chosen to cover the whole surface of the Cd foils. In addition the WinFTM scan mode was used to further increase the measured area. The data of each of the secondary standards to be characterized were obtained as mean value of 16 individual measurements distributed over a 4x4 matrix in a central area of 2mm x 2 mm. Table I : experimental parameters for the XRF measurement of the Cu primary standards. In addition weight and area of the three Cd foils for the production of primary reference standards have been measured following the standards of the DAkkS accreditation D-K-15076-01-00. The obtained mass per unit area is used as reference for the calibration of the standards free XRF values.

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Calibration-TR-Characterization of Cd primary and secondary reference materials-2

HELMUT FISCHER GMBH INSTITUT FUR ELEKTRONIK UND MESSTECHNIK Table II : experimental parameters for the XRF measurement of the Cd secondary reference standards to be calibrated. The following four figures represent heatmaps of Cd thickness values for the three primary reference standards BBJ, BBK and BBL. It is noteworthy that all samples exhibit either thickness gradients or inhomogeneous thickness distribution.

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Calibration-TR-Characterization of Cd primary and secondary reference materials-3

HELMUT FISCHER GMBH INSTITUT FUR ELEKTRONIK UND MESSTECHNIK surface scan of primary reference standard BBK, Cd thickness/pm surface scan of primary reference standard BBL, Cd thickness/pm

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Calibration-TR-Characterization of Cd primary and secondary reference materials-4

HELMUT FISCHER GMBH INSTITUT FUR ELEKTRONIK UND MESSTECHNIK The statistical programming language R has been used to express the correlation of the difference between gravimetric and XRF measurements and the XRF measurements in terms of a linear regression. Linear regression between the difference (gravimetry - standard free XRF) vs. standard free XRF using a linear correlation. The area between the dotted lines represents the confidence band. Fit and graphics have been produced using the statistical programming language R. The results are summarized in table III. Table III : Summary of experimental...

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Calibration-TR-Characterization of Cd primary and secondary reference materials-5

HELMUT FISCHER GMBH INSTITUT FUR ELEKTRONIK UND MESSTECHNIK Table IV : Summary of experimental data from XRF measurements for the secondary Cd reference standards. Calibrated values ("cal") have been calculated using the correlation between XRF and gravimetric measurements for the primary reference standards (see Table III). Sindelfingen, 10/09/2013 Dr. Jorg Leske

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