CHY203 -X-Ray Fluorescence lab report

Department of Chemical Engineering X-Ray Fluorescence Student name: Student number: CHY203, Section 02 Group number: 2 April 17th, 2013 Instructor: David Naranjit TA: Justin X-Ray Fluorescence Data & Result Sheet 1. Collection of a Copper Spectrum Elements Type of Photon Energy Experimental line emission (KeV) Literature line emission (KeV) Sum Peaks + Exp. Litre. % Relative Error Cu k 7.99 8.04778 16.88 16.95307 0.72 k 8.89 8.90529 0.17 Sample Calculation of % Error for Cu k : Relative % Error = [Literature Value-Experimental Photon Value/Literature Value] x 100% = [8.04778-7.99/8.04778]*100% = 0.72% 2. Interpretation of a Quality Control Fused Glass Spectrum Elements Type of Photon Energy Experimental line emission (KeV) Literature line emission (KeV) Sum Peaks + Exp. Liter. % Relative Error Si k 1.75 1.73998 3.60 3.57592 0.58 k 1.85 1.83594 0.77 Ca k 3.66 3.69168 7.68 7.70438 0.86 k 4.02 4.0127 0.18 Mn k 5.86 5.89875 12.37 12.3892 0.66 k 6.51 6.49045 0.30 As k 10.55 10.54372 22.25 22.26992 0.060 k 11.70 11.7262 0.22 Mo k 17.49 17.47934 37.14 37.08764 0.061 k 19.65 19.6083 0.21 Sb k 26.45 26.3591 56.20 56.0847 0.34 k 29.75 29.7256 0.082 3. Interpretation of Steel Slag Spectrum Elements Type of Photon Energy Experimental line emission (KeV) Literature line emission (KeV) % Relative Error Si k 1.75 1.73998 0.58 k 1.91 1.83594 4.03 Ca k 3.67 3.69168 0.59 k 4.02 4.0127 0.18 Mn k 5.91 5.89875 0.19 k 39179511493500 6.49045 4197351168400 Al k 1.49 1.48670 0.22 k 3917951003300 1.55745 419735102235 Mg k 1.26 1.25360 0.51 k 391795850900 1.3022 41973587630 Ti k 4.53 4.51084 0.42 k 4.95 4.93181 0.37 Cr k 5.45 5.41472 0.65 k 391795939800 5.94671 41973595885 Fe k 6.41 6.40384 0.096 k 7.05 7.05798 0.11 Ar k 2.89 2.95770 2.29 k 3.099 3.1905 2.87 K k 3.33 3.3138 0.49 k 33845590170 3.5896 41973590170 P k 2.01 2.0137 0.18 k 33845510985500 2.1391 3721101098550 Cl k 2.87 2.8156 1.93 3. Interpretation of Cheese Powder Spectrum Elements Type of Photon Energy Experimental line emission (KeV) Literature line emission (KeV) % Relative Error S k 2.305 2.30784 0.12 k 410845984250 2.46404 46736098425 Cl k 2.63 2.62239 0.29 k 2.79 2.8156 0.91 K k 3.30 3.3138 0.42 k 4108457874000 3.5896 46736078740 Ca k 3.65 3.69168 1.13 k 4.00 4.0127 0.32 Ti k 4.50 4.51084 0.24 k 4.94 4.93181 0.17 Ne k 0.86 0.8486 1.34 k 41084591440 436245914400 467360914400 p k 2.05 2.0137 1.80 k 410845958850 2.1391 46736095885 3. Collection of the Unknown Sample # 9071 Spectrum Elements Type of Photon Energy Experimental line emission (KeV) Literature line emission (KeV) Sum Peaks + Exp. Liter. % Relative Error Ar k 2.99 2.95770 6.15 6.1482 1.09 k 3.16 3.1905 0.96 Co k 6.90 6.93032 14.55 14.57975 0.44 k 7.65 7.64943 0.0075 Sr k 14.18 14.165 30.03 30.0007 0.11 k 15.85 15.8357 0.090 Cr k 5.51 5.41472 11.48 11.36143 1.76 k 5.97 5.94671 0.39 Mg k 1.18 1.25360 2.49 2.5558 5.87 k 1.31 1.3022 0.60 K k 3.35 3.3138 6.98 6.9034 1.09 k 3.63 3.5896 1.13 Si k 1.75 1.73998 1.75 3.57592 0.58 k 334645844550 1.83594 28575084455 Discussion: 1. If a cement sample contains 60% of CaO. Calculate the values of the three sum peaks that are produced at this high concentration. Ca: k= 3691.68 eV k= 4012.7 eV The three sum peaks values are: Ca k + Ca k= (3691.68 eV) + (3691.68 eV) =7383.36 eV Ca k + Ca k= (3691.68 eV) + (4012.7 eV) = 7704.38 eV Ca k + Ca k= (4012.7 eV) + (4012.7 eV) = 8025.4 eV 2. How does the Energy Dispersive X-Ray Fluorescence instrument differ from the Wavelength Dispersive X-Ray instrument in terms of sensitivity, interferences and theory of operation. The Energy Dispersive X-Ray Fluorescence is an analytical instrument that used to analysis the type of elements present in the sample compounds of interest by measuring the wavelength and intensity of the x-ray radiation energy of the analytic species. EDXRF also has a high energy x-ray tube that used to stimulates the sample molecules as the x-ray beam concentrated on the sample and thus converting the x-ray radiation beam into a pulse as it detected by the silica drift lithium detector. However, the Wavelength Dispersive X-Ray is an instrument that used to measure the wavelength of an element present in the analytical sample by diffracting the photon as it pass through a crystal structure and hence detect by the detector. Although, EDXRF and WDXRF are effective techniques for analysing an elements in a compound, the wavelength dispersive x-ray fluorescence has a better resolution and hence highly sensitivity than the energy dispersive x-ray fluorescence. Also, the wavelength dispersive x-ray fluorescence has a slightly better interfering than the energy dispersive x-ray fluorescence since the x-ray beams loss it energy as it diffracted by the monochromatic crystal in WDXRF as it pass through the analysing sample which in return cause the EDXRF to have a highly efficiency than the WDXRF. On the other hands, in the theory of operation the EDXRF provides a better respond and ability for analysing an element in the sample than WDXRF since it has Al or Ag filter between the x-ray tube and the analysing sample that reduce the diffraction peaks, the unwanted parts of spectrum, the count rate of high concentration species and hence minimize the background noise that caused by the scattering x-ray beams. Graphs of Spectrum Analysis: 1. Collection of a Copper Spectrum 2. Interpretation of a Quality Control Fused Glass Spectrum 3. Collection of a Pressed Pellet Unknown Sample 9071 Spectrum 4. Interpretation of a Cheese Powder Spectrum 5. Interpretation of a Steel Slag Spectrum References: Instrumental Methods of Analysis Laboratory Manual, X-Ray Fluorescence, X-Ray Fluorescence Spectroscopy, Ryerson University 2013, page 56-72 N. Joseph (editor), Energy Dispersive X-Ray Fluorescence Spectroscopy, Shimadzu, Analytical and Measuring Instruments, 2013. http://www.shimadzu.com/an/elemental/edxrf/index.html J. Henry, Comparison of Wavelength Dispersive X-Ray Fluorescence and Energy Dispersive X-Ray Fluorescence Techniques, Rigaku Analytical Chemistry Products,2013 http://www.rigaku.com/products/xrf/primini/app004