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




Comment: Well done spotting that the two lines, 2.28 and 1.510 Å have both an anomalous intensity and large FWHM values and therefore should still be included in the list of remaining lines. For some reason, however, you did include 2.28 but didn't include 1.510 in the list, but I assume this was just a typo.
4.5 Marks

(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




Comment: Correct solution and then to follow you compared the patterns in detail and concluded correctly that they matched; there were some lines which didn't appear but this is understandable since they were weak lines (see model answer).
7.5 Marks

(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




Comment: Correct solution and similar comments to the previous solution.
7 Marks

(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.


Comment: Exactly correct re the overlapping lines. Some comment re the actual solution and that the microprobe analysis is in agreement could have been given (see model answer).
3 Marks


Overall Comment: Basically all the solutions were correct and correct logic was used to arrive at these solutions. I hope this assignment was useful in giving you some further grasp of the procedures involved in search/match analysis.


Total Mark 22