Assignment 4.

Page 1.




(i)  Peaks with d spacings of 3.86, 3.035, 2.845, 2.495, 2.284, 2.095, 1.927, 1.913, 1.875, 1.626, 1.604, 1.587, 1.525, 1.518 and 1.510Å belong to the calcite phase (phase 1.).

    d(Å)I(%)
    3.8612
    3.035100
    2.8453
    2.49510
    2.28418
    2.09518
    1.9275
    1.91317
    1.87517
    1.6264
    1.6048
    1.5872
    1.5255
    1.5184
    1.5103

In the diffraction pattern collected, the intensity of the peaks at 2.28 and 1.510Å are larger than expected (29 and 4% respectively) and the large FWHM values (0.43 and 0.42° respectively) suggests there are peaks belonging to other phases with these d spacings and intensities relative to CaCO3 of 11 and 1 respectively.


(ii)  Normalising the remaining intensities relative to the most intense peak (with d spacing of 3.343Å) gives

    d(Å)I(%)FWHM(°)
    4.27340.27
    3.3431000.30
    2.742140.35
    2.50320.36
    2.458120.22
    2.284130.43
    2.23750.23
    2.128100.23
    2.10270.35
    1.98050.23
    1.93920.37
    1.817180.22
    1.70060.35
    1.67270.23
    1.65920.24
    1.541140.23



(iii)  Choosing the next 3 highest intensities with d spacings at 3.343, 4.27, 1.817Å and searching the Hanawalt manual gives SiO2 (card number 5-490) (phase 2.). The card shows peaks with d spacings of 1.541, 2.458, 2.284, 2.128, 1.672, 2.237, 1.980, 1.659Å belong to this phase.

    d(Å)I(%)
    4.2735
    3.343100
    2.45812
    2.28412
    2.2376
    2.1289
    1.9806
    1.81717
    1.6727
    1.6593
    1.54115



(iv)  Normalising the remaining intensities gives

    d(Å)I(%)FWHM(°)
    2.7421000.35
    2.503170.36
    2.102500.35
    1.939170.37
    1.700420.35
    1.510100.42



(v)  Choosing the 3 highest intensities with d spacings of 2.742, 2.102, 1.700Å and searching the Hanawalt manual gives MgCO3 (card number 8-479) (phase 3.). The card shows that all these peaks belong to this phase.

    d(Å)I(%)
    2.742100
    2.50318
    2.3184
    2.10345
    1.93912
    1.7694
    1.70035
    1.5104



(vi)  In the diffraction pattern, the patterns of the 3 phases overlap at only two d spacings (2.284Å for phases CaCO3 and SiO2 and 1.510Å for phases CaCO3 and MgCO3). The background level in the diffraction pattern masks the weaker peaks for the MgCO3 pattern. The fact that there are no other unaccounted peaks implies that all the phases present have been identified.