diff --git a/cif_pow.dic b/cif_pow.dic index 3399f86..71cd7a9 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -2061,6 +2061,43 @@ save_PD_CALC_OVERALL _name.category_id PD_GROUP _name.object_id PD_CALC_OVERALL _category_key.name '_pd_calc_overall.diffractogram_id' + _description_example.case +; + _pd_diffractogram.id DIFFRACTOGRAM_NUMBER_7 + _pd_calc.method Rietveld + + _pd_calc_overall.component_presentation_order + [ PHASE_A_ID PHASE_B_ID PHASE_C_ID ] + + loop_ + _pd_data.point_id + _pd_meas.2theta_scan + _pd_meas.intensity_total + _pd_calc.intensity_total + _pd_calc.component_intensity_net_list + 0 3.99875 1061.8 1076.653 [ 20.20 203.215 512.256 ] + 1 4.03625 1053.9 1074.628 [ 21.34 204.535 513.156 ] + 2 4.07375 1060.2 1072.667 [ 21.45 205.755 516.456 ] + 3 4.11125 1017.3 1070.768 [ 21.55 206.975 513.256 ] + #... +; + _description_example.detail +; + Tabulation of diffraction data consisting of measured and + calculated data, where the calculated data also include intensities + ascribed to the different phases which make up the model. The phases to + which the intensities belong are given by the value of + _pd_calc_overall.component_presentation_order. These values correspond + to the _pd_phase.id values of the phases contributing to the current + diffractogram. As _pd_calc.component_intensity_net_list is used, the + intensities given do not include any background contribution. + + The category key value associated with _pd_data.point_id is given + with every data point. The category key value associated with + _pd_calc_overall.diffractogram_id and _pd_data.diffractogram_id would + be taken as 'DIFFRACTOGRAM_NUMBER_7', the value of + _pd_diffractogram.id given in the data block. +; save_ @@ -2556,6 +2593,48 @@ save_PD_CALIB_DETECTED_INTENSITY '_pd_calib_detected_intensity.detector_id' '_pd_calib_detected_intensity.id' + loop_ + _description_example.case + _description_example.detail +; + loop_ + _pd_calib_detected_intensity.detector_id + _pd_calib_detected_intensity.detector_response + _pd_calib_detected_intensity.detector_response_su + _pd_calib_detected_intensity.diffractogram_id + _pd_calib_detected_intensity.phase_id + A_27a6a2a6 1 . DIFFRACTOGRAM_A 676A + B_27a6a2a6 1.035 0.013 DIFFRACTOGRAM_B 676A +; +; + The two detectors, A and B, have responses of 1 and 1.035, + respectively, meaning that their measured intensities must be divided + by these values to retreive their true values. These response values + were derived from an analysis of the diffraction patterns + DIFFRACTOGRAM_A and DIFFRACTOGRAM_A, both of which contain the phase + 676A. +; +; + loop_ + _pd_calib_detected_intensity.detector_id + _pd_calib_detected_intensity.detector_response + _pd_calib_detected_intensity.diffractogram_id + _pd_calib_detected_intensity.phase_id + _pd_calib_detected_intensity.special_details + 1_4913c6ed 1 . . 'Scanned through direct beam.' + 2_4913c6ed 0.973 . . 'Scanned through direct beam.' + 3_4913c6ed 0.997 . . 'Scanned through direct beam.' + 4_4913c6ed 1.039 . . 'Scanned through direct beam.' + #... +; +; + A position-sensitive detector was scanned through the direct beam to + calibrate the response of each channel to a constant-intensity source. + The measured intensity of each channel must be divided by the given + response to obtain the actual value. No diffraction pattern or phase + was involved in the derivation of the response values. +; + save_ save_pd_calib_detected_intensity.detector_id @@ -2708,7 +2787,7 @@ save_PD_CALIB_INCIDENT_INTENSITY _definition.id PD_CALIB_INCIDENT_INTENSITY _definition.scope Category _definition.class Set - _definition.update 2023-06-10 + _definition.update 2023-06-17 _description.text ; This section defines the parameters used for the incident intensity @@ -2727,6 +2806,34 @@ save_PD_CALIB_INCIDENT_INTENSITY _name.object_id PD_CALIB_INCIDENT_INTENSITY _category_key.name '_pd_calib_incident_intensity.instr_id' + loop_ + _description_example.case + _description_example.detail +; + _pd_calib_incident_intensity.instr_id a3643812 + _pd_calib_incident_intensity.incident_counts 4231 + _pd_calib_incident_intensity.special_details 'From beam monitor.' +; +; + The number of counts incident on the specimen in the instrument + identified as a3643812 is 4231, as measured by a beam monitor. The + uncertainty on the incident counts is given as the square root of the + counts. +; +; + _pd_calib_incident_intensity.instr_id 9deaa4f1 + _pd_calib_incident_intensity.incident_intensity 453.3 + _pd_calib_incident_intensity.incident_intensity_su 1.6 + _pd_calib_incident_intensity.diffractogram_id STANDARD_30ffb964 + _pd_calib_incident_intensity.phase_id SRM1796_15341c3a +; +; + In the instrument identified as 9deaa4f1, the intensity incident on the + specimen is 453.3 +- 1.6. This was determined through an analysis of + the diffractogram, STANDARD_30ffb964, which contains the phase, + SRM1796_15341c3a. +; + save_ save_pd_calib_incident_intensity.diffractogram_id @@ -4027,6 +4134,15 @@ save_PD_CHAR _name.category_id PD_GROUP _name.object_id PD_CHAR _category_key.name '_pd_char.id' + _description_example.case +; + _pd_char.colour white + _pd_char.mass_atten_coef_mu_calc 4878 + _pd_char.particle_morphology + 'Large equiaxed chunks, approx. 3 mm across.' + _pd_char.special_details + 'Bottle labelled "corundum". MAC calculated from XRF.' +; save_ @@ -4431,6 +4547,38 @@ save_PD_DATA _pd_data.diffractogram_id would be taken from the value associated with the data name _pd_diffractogram.id given in that data block. ; +; + _pd_calc_overall.component_presentation_order + [ PHASE_A_ID PHASE_B_ID PHASE_C_ID ] + + loop_ + _pd_data.point_id + _pd_meas.2theta_scan + _pd_meas.intensity_total + _pd_calc.intensity_total + _pd_calc.component_intensity_net_list + 0 3.99875 1061.8 1076.653 [ 20.20 203.215 512.256 ] + 1 4.03625 1053.9 1074.628 [ 21.34 204.535 513.156 ] + 2 4.07375 1060.2 1072.667 [ 21.45 205.755 516.456 ] + 3 4.11125 1017.3 1070.768 [ 21.55 206.975 513.256 ] + #further data points follow +; +; + Tabulation of diffraction data consisting of measured and + calculated data, where the calculated data also include intensities + ascribed to the different phases which make up the model. The phases to + which the intensities belong are given by the value of + _pd_calc_overall.component_presentation_order. These values correspond + to the _pd_phase.id values of the phases contributing to the current + diffractogram. As _pd_calc.component_intensity_net_list is used, the + intensities given do not include any background contribution. + + The category key value associated with _pd_data.point_id is given + with every data point. In the usual case that only one diffractogram + is present in the data block, the category key value associated with + _pd_data.diffractogram_id would be taken from the value associated + with the data name _pd_diffractogram.id given in that data block. +; save_ @@ -6149,6 +6297,14 @@ save_pd_diffractogram.id _type.container Single _type.contents Text + loop_ + _description_example.case + '1991-15-09T16:54:00Z|SEPD7234|B.Toby|SEPD.IPNS.ANL.GOV' + '76d675f5-9f0b-4bd9-8be3-1266edf74908' + 'DIFFRACTOGRAM Z2' + 'Insitu_pattern_0123' + 'Synthesis number 1' + save_ save_pd_diffractogram.spec_id @@ -6216,6 +6372,112 @@ save_PD_INSTR _name.object_id PD_INSTR _category_key.name '_pd_instr.id' + loop_ + _description_example.case + _description_example.detail +; + _diffrn_radiation_wavelength.type 'Cu K\a~1~' + _diffrn_radiation_wavelength.value 1.540596 + + _pd_instr.id b4131be5 + _pd_instr.geometry + ; + Bragg-Brentano, pre-specimen double-bounce monochromator. + Dual strip detectors covering ~20\% each. Scanned to cover all angles. + ; + _pd_instr.2theta_monochr_pre 45.31 + _pd_instr.monochr_pre_spec 'Ge 220' + _pd_instr.divg_eq_mono_spec 0.2 + _pd_instr.cons_illum_flag no + _pd_instr.detector_circle_radius 320 + _pd_instr.dist_mono_spec 402 + _pd_instr.dist_src_mono 39 + _pd_instr.beam_size_ax 10.5 + _pd_instr.slit_ax_mono_spec 10.0 + _pd_instr.slit_eq_mono_spec 0.5 + _pd_instr.soller_ax_mono_spec 2.5 + _pd_instr.source_size_ax 12 + _pd_instr.source_size_eq 0.4 + _pd_instr.location 'Physics, Anytown University.' +; +; + This instrument is identified by the id b4131be5. The instrument is + described as a Bragg-Brentano diffractometer with a pre-specimen, + double-bounce Ge 220 monochromator. It has two detectors; these are not + described here, see PD_INSTR_DETECTOR. The monochromator is set at + 45.31\% 2\q. The equatorial divergence between the monochromator and + specimen is fixed at 0.2\%; this instrument is not run in constant + illumination length mode. + + The distance from the virtual source to the specimen for all + measurement points is 320 mm, whereas the distance from the + monochromator to the specimen is 402 mm. The monochromator is + situated 39 mm from the source. The width of the beam on the specimen, + in the axial direction, is 10.5 mm, and the width of the beam is + defined at the monochromator by a 10 mm mask. There is a 0.5 mm + equatorial slit between the monochromator and specimen, which can be + assumed to be on the detector circle, and acts as the virtual source. + + There are 2.5\% axial Soller slits between the monochromator and the + specimen. The size of the source in the X-ray tube is 12 x 0.4 mm. + + The instrument is located in the Department of Physics in Anytown + University. + + The radiation used in the instrument is defined by data names from the + DIFFRN_RADIATION_WAVELENGTH category. In this case, it is pure Cu K\a~1~ + radiation with a wavelength of 1.540596 \%A. +; +; + loop_ + _diffrn_radiation_wavelength.id + _diffrn_radiation_wavelength.value + _diffrn_radiation_wavelength.wt + _diffrn_radiation_wavelength.type + _diffrn_radiation_wavelength.details + 1 1.7889847 0.378 'Co K\a' 'G. H\"olzer et al. Phys. Rev. A 56, 4554' + 2 1.7892524 0.144 'Co K\a' 'G. H\"olzer et al. Phys. Rev. A 56, 4554' + 3 1.7896946 0.127 'Co K\a' 'G. H\"olzer et al. Phys. Rev. A 56, 4554' + 4 1.7888515 0.088 'Co K\a' 'G. H\"olzer et al. Phys. Rev. A 56, 4554' + 5 1.7927905 0.197 'Co K\a' 'G. H\"olzer et al. Phys. Rev. A 56, 4554' + 6 1.7930637 0.095 'Co K\a' 'G. H\"olzer et al. Phys. Rev. A 56, 4554' + 7 1.7934738 0.050 'Co K\a' 'G. H\"olzer et al. Phys. Rev. A 56, 4554' + + _pd_instr.id 58b6d83b + _pd_instr.geometry Bragg-Brentano + _pd_instr.cons_illum_len 12.0 + _pd_instr.detector_circle_radius 117.5 + _pd_instr.dist_src_spec 117.5 + _pd_instr.beam_size_ax 9.8 + _pd_instr.slit_ax_src_spec 9.5 + _pd_instr.soller_ax_src_spec 5.0 + _pd_instr.source_size_ax 8.5 + _pd_instr.source_size_eq 0.4 + _pd_instr.location + 'ACME Measurements, 123 Main St. Maintown.' +; +; + This instrument is identified by the id 58b6d83b. The instrument is + described as a Bragg-Brentano diffractometer. The instrument is run + with a constant illumination length of 12 mm. + + The distance from the source to the specimen for all measurement points + is 117.5 mm, which is identical the distance from the source to the + specimen, as the X-ray tube is mounted on the detector circle. The width + of the beam on the specimen, in the axial direction, is 9.8 mm, and the + width of the beam is defined at the source by a 9.5 mm mask. + + There are 5.0\% axial Soller slits between the source and the specimen. + The size of the source in the X-ray tube is 8.5 x 0.4 mm. + + The instrument is located at ACME Measurements in Maintown. + + The radiation used in the instrument is defined by data names from the + DIFFRN_RADIATION_WAVELENGTH category. In this case, it is Co K\a + radiation as described by the constituent seven wavelengths, as + described by G. H\"olzer et al. Phys. Rev. A 56, 4554. +; + save_ save_pd_instr.2theta_monochr_pre @@ -7120,6 +7382,76 @@ save_PD_INSTR_DETECTOR _name.object_id PD_INSTR_DETECTOR _category_key.name '_pd_instr_detector.id' + loop_ + _description_example.case + _description_example.detail +; + # _pd_instr.id b4131be5 + + loop_ + _pd_instr_detector.id + _pd_instr.dist_spec_detc + _pd_instr.slit_ax_spec_detc + _pd_instr.slit_eq_spec_detc + fd343493 320 8.5 0.075 + 47540661 320 8.5 0.075 +; +; + Assume these detectors are paired with the instrument identified by the + id b4131be5. + + There are two detectors, fd343493 and 47540661. Both detectors are + positioned 320 mm from the specimen, and are defined by two slits, + 8.5 mm in the axial direction, and 0.075 mm in the equatorial direction. + As the instrument description says that this instrument has 'Dual strip + detectors', it can be assumed that the detector window is 8.5 mm wide, + and each strip, or pixel, in the dector is 75 \mm high. +; +; + # _pd_instr.id 58b6d83b + + _pd_instr.2theta_monochr_post 31.0 + _pd_instr.dist_anal_detc 47 + _pd_instr.dist_spec_anal 135 + _pd_instr.monochr_post_spec 'Graphite mosaic monochromator' + _pd_instr.slit_ax_spec_anal 9.5 + _pd_instr.slit_eq_spec_anal 0.5 + _pd_instr.soller_eq_spec_anal 2.5 +; +; + Assume this detector is paired with the instrument identified by the + id 58b6d83b. + + The post-specimen, graphite, mosaic monochromator is set at 31.0\% 2\q. + The monochromator is situated 47 mm from the detector. The distance from + the specimen to the monochromator is 135 mm. The width of the beam is + defined at the monochromator by a 9.5 mm mask. There is a 0.5 mm + equatorial slit between the specimen and monochromator, which can be + assumed to be on the detector circle, and acts as the virtual detector. + There are 2.5\% axial Soller slits between the specimen and the + monochromator. +; +; + # _pd_instr.id 58b6d83b + + _pd_instr.dist_spec_detc 117.5 + _pd_instr.monochr_post_spec 'Fe filter' + _pd_instr.slit_ax_spec_detc 12 + _pd_instr.slit_eq_spec_detc 0.075 + _pd_instr.soller_ax_spec_detc 2.5 +; +; + Assume this detector is paired with the instrument identified by the + id 58b6d83b. + + The distance from the specimen to the detector is 117.5 mm. The X-ray + beam is "monochromatised" by a metal Fe filter. The detector is defined + by a 12 mm axial and 0.075 mm equatorial slit. The small size of the + equatorial slit might lead the reader to assume a strip detector was + used. This should be documented using _pd_instr.special_details. There + are 2.5\% axial Soller slits between the specimen and the detector. +; + save_ save_pd_instr.2theta_monochr_post @@ -7933,6 +8265,91 @@ save_PD_MEAS_OVERALL _name.object_id PD_MEAS_OVERALL _category_key.name '_pd_meas_overall.diffractogram_id' + loop_ + _description_example.case + _description_example.detail +; + _pd_diffractogram.id PATTERN_37 + + _pd_meas.2theta_range_min 5.00 + _pd_meas.2theta_range_max 95.00 + _pd_meas.2theta_range_inc 0.02 + _pd_meas.number_of_points 4501 + _pd_meas.scan_method cont + + _pd_meas.datetime_initiated 2023-02-27T22:45:00+08:00 + + _pd_meas.rocking_angle 180 + _pd_meas.rocking_axis phi + _pd_instr.geometry Bragg-Brentano + + loop_ + _pd_data.point_id + _pd_meas.counts_total + 1 1234 + 2 1256 + #... +; +; + The measured diffractogram is in equally spaced 2\q points, starting + at 5.00\% 2\q, going up in steps of 0.02\%, with the last data point at + 95.00\% 2\q. In total, there are 4501 data points. The data were + collected in a continuous scan, such that the detector did not stop + moving, and the intensities were binned according to the goniometer + angle during the collection time per step. Data collection was started + on the 27^th^ of February, 2023 at 2245 h in a timezone +8 h from UTC. + The specimen was rotated 180\% during the collection of the data for + each measurement point +; +; + _pd_meas.rocking_angle 2.5 + _pd_meas.rocking_axis omega + _pd_meas.scan_method step + + _pd_instr.geometry Bragg-Brentano + + _pd_meas_overall.diffractogram_id PATTERN_96 + + loop_ + _pd_data.point_id + _pd_data.diffractogram_id + _pd_meas.2theta_scan + _pd_meas.counts_total + 1 PATTERN_96 5.02 1234 + 2 PATTERN_96 5.04 1256 + #... +; +; + The information here applies to the diffractogram with the id + 'PATTERN_96'. For each measurement point, the specimen rotated +-2.5\% + from its standard position about the omega axis. +; +; + _pd_diffractogram.id EDD_123 + + _pd_meas.2theta_fixed 5 + _pd_meas.angle_chi 45 + _pd_meas.units_of_intensity + 'Proportional to current (Ampere) from Si(Li) detector.' + _pd_meas.scan_method disp + + loop_ + _pd_data.point_id + _pd_proc.energy_detection + _pd_meas.intensity_total + _pd_meas.intensity_total_su + 1 50300 1234 23 + 2 50400 1256 24 + #... +; +; + The information here applies to the diffractogram with the id + 'EDD_123'. The detector was fixed at 5\% 2\q and tilted at + 45\% \c. The data were collected in energy-dispersive mode, where + the intensity recorded was proportional to the current measured in + the Si(Li) detector. +; + save_ save_pd_meas.2theta_fixed @@ -8408,6 +8825,58 @@ save_PD_PEAK '_pd_peak.diffractogram_id' '_pd_peak.id' + loop_ + _description_example.case + _description_example.detail +; + loop_ + _pd_peak.id + _pd_peak.2theta_centroid + _pd_peak.width_2theta + _pd_peak.intensity + _pd_peak.intensity_su + A 12.35 0.26 1023 7 + B 24.74 0.56 2318 15 + C 37.79 0.61 506 2 +; +; + The details of three peaks are given. Their peak position is given as + the position of the peak centroid (eg 12.35\% 2\q), and the + width is the full-width at half-maximum (eg 0.26\% 2\q). The peak + intensity is given as the peak area with an associated standard + uncertainty (eg 1023 +- 7). +; +; + loop_ + _diffrn_radiation_wavelength.id + _diffrn_radiation_wavelength.value + _diffrn_radiation_wavelength.wt + 1 1.534753 0.0159 + 2 1.540596 0.5691 + 3 1.541058 0.0762 + 4 1.544410 0.2517 + 5 1.544721 0.0871 + + loop_ + _pd_peak.id + _pd_peak.d_spacing + _pd_peak.pk_height + _pd_peak.pk_height_su + _pd_peak.wavelength_id + a 6.25 10432 132 2 + b 3.17 8973 87 2 + c 1.25 25632 167 2 +; +; + The details of three peaks are given. Their peak position is given as + the position of the peak in angstroms (eg 6.25 \%A). The peak intensity + is given as the peak height with an associated standard uncertainty + (eg 10432 +- 132). The particular wavelength used to calculate the + d-spacing from the data's original 2\q results is given in the final + column, which corresponds to 1.540596 \%A, as given in the top-most + loop. +; + save_ save_pd_peak.2theta_centroid @@ -8762,6 +9231,26 @@ save_PD_PEAK_OVERALL _name.object_id PD_PEAK_OVERALL _category_key.name '_pd_peak_overall.id' + loop_ + _description_example.case +; + _pd_peak_overall.id PEAK_GROUP_1 + _pd_peak.special_details + ; + Peak positions allowed to refine freely. Peak widths + constrained to follow UVW relationship. Peak shape + constrained to be Lorentzian. + ; +; +; + _pd_peak_overall.id peaks + _pd_peak.special_details + ; + Peak positions fixed by second-derivative analysis. + Widths allowed to refine freely. Pearson-VII peakshape. + ; +; + save_ save_pd_peak.special_details @@ -8835,6 +9324,13 @@ save_pd_phase.id _type.container Single _type.contents Text + loop_ + _description_example.case + '1991-15-09T16:54:00Z|Si-std|B.Toby|D500#1234-987' + '9d0e3eef-614a-4127-aef5-8b859168fd13' + 'PHASE A' + 'Calcium sulphate hemihydrate. ACME Chemicals, batch #12090.' + save_ save_pd_phase.name @@ -8954,6 +9450,10 @@ save_PD_PHASE_MASS their associated standard uncertainties. The values are associated with one diffractogram and three phases. + The method of presentation given here would be associated with being + present in a block which does not contain a _pd_diffractogram.id or + _pd_phase.id data item. + Blocks containing information about more than one phase must set a non-default value for _audit.schema. ; @@ -8961,6 +9461,8 @@ save_PD_PHASE_MASS ; _audit.schema Custom + _pd_diffractogram.id A_DIFFRACTOGRAM + loop_ _pd_phase_mass.phase_id _pd_phase_mass.percent @@ -10053,6 +10555,21 @@ save_PD_PREP _name.category_id PD_GROUP _name.object_id PD_PREP _category_key.name '_pd_prep.id' + _description_example.case +; + _pd_prep.id 'rutile 1234' + _pd_prep.conditions + ; + 1 kg of anatase from Acme, Lot#1234 was placed in several + platinum crucible in a furnace at atmospheric pressure. + The furnace was heated at 5 K/min to 1100 K, and held there + overnight. The furnace was then switched off and allowed to + cool naturally. The batch was combined, homogenised, and + riffle-split into 50 g packets. + ; + _pd_prep.pressure 101.3 + _pd_prep.temperature 1100 +; save_ @@ -10071,6 +10588,21 @@ save_pd_prep.char_id _type.source Related _type.container Single _type.contents Text + _description_example.case +; + _pd_prep.id 'rutile 1234' + _pd_prep.conditions + ; + 1 kg of anatase from Acme, Lot#1234 was placed in several + platinum crucible in a furnace at atmospheric pressure. + The furnace was heated at 5 K/min to 1100 K, and held there + overnight. The furnace was then switched off and allowed to + cool naturally. The batch was combined, homoginised, and + riffle-split into 50 g packets. + ; + _pd_prep.pressure 101.3 + _pd_prep.temperature 1100 +; save_ @@ -10444,6 +10976,68 @@ save_PD_PROC_LS _name.category_id PD_GROUP _name.object_id PD_PROC_LS _category_key.name '_pd_proc_ls.diffractogram_id' + loop_ + _description_example.case + _description_example.detail +; + _pd_diffractogram.id PATTERN_42 + + _pd_proc_ls.peak_cutoff 0.0001 + _pd_proc_ls.prof_wr_expected 0.12324 + _pd_proc_ls.prof_wr_factor 0.15432 + _pd_proc_ls.profile_function 'Fundamental parameters' +; +; + The PD_PROC_LS information applies to the diffractogram with the id of + PATTERN_42. The peak intensities are calculated out to a point where + the intensity is 0.0001\\times the intensity at the peak maximum, or + 0.01%. The value of R~exp~ is 12.324% and R~wp~ is 15.432%. The peak + profiles were calculated using fundamental parameters +; +; + _pd_proc_ls.diffractogram_id cae4f697-ae84-4e3f-a0c1-4569d60b6191 + _pd_proc_ls.peak_cutoff 0.005 + _pd_proc_ls.prof_wr_expected 0.0273 + _pd_proc_ls.prof_wr_factor 0.0569 + _pd_proc_ls.profile_function + ; + The profiles were calculated using the modified Thompson-Cox-Hastings + formulation, where: + + tch_L = X * tan(\q)) + (Y / cos(\q) + tch_G = (U * tan(\q)^2^ + V * tan(\q) + W + Z / cos(\q)^2^)^1/2^ + tch_P = ( tch_G^5^ + + 2.69269 * tch_G^4^ * tch_L + + 2.42843 * tch_G^3^ * tch_L^2^ + + 4.47163 * tch_G^2^ * tch_L^3^ + + 0.07842 * tch_G * tch_L^4^ + + tch_L^5^ )^1/5^ + tch_Q = tch_L / tch_P + eta = 1.36603 * tch_Q - 0.47719 * tch_Q^2^ + 0.1116 * tch_Q^3^ + + The full-width half-maximum of the Lorentzian and Gaussian peaks are + given by tch_L and tch_G, respectively. + + The mixing parameter between the amount of Lorentzian and Gaussian is + given by eta. + + U, W, Y, and Z were fixed at zero. + + The refined values of V and X were 0.059(2)\% and 0.037(1)\%, + respectively. + + For further details, see J. Appl. Cryst. (1987). 20, 79-83 + https://doi.org/10.1107/S0021889887087090 + ; +; +; + The PD_PROC_LS information applies to the diffractogram with the id of + the given GUID. The peak intensities are calculated out to a point + where the intensity is 0.005\\times the intensity at the peak maximum, + or 0.5%. The value of R~exp~ is 2.73% and R~wp~ is 5.69%. The peak + profiles were calculated using the modified Thompson-Cox-Hasting + algorithm, as described, with final refined parameter values given. +; save_ @@ -10754,6 +11348,48 @@ save_PD_PROC_OVERALL _name.object_id PD_PROC_OVERALL _category_key.name '_pd_proc_overall.diffractogram_id' + loop_ + _description_example.case + _description_example.detail +; + _pd_diffractogram.id PATTERN_42 + + _pd_proc.2theta_range_min 5.00 + _pd_proc.2theta_range_max 95.00 + _pd_proc.2theta_range_inc 0.02 + _pd_proc.number_of_points 4501 + + loop_ + _pd_data.point_id + _pd_proc.intensity_total + _pd_proc.intensity_total_su + 1 1234 23 + 2 1256 24 + #... +; +; + The processed diffractogram is in equally spaced 2\q points, starting + at 5.00\% 2\q, going up in steps of 0.02\%, with the last data point at + 95.00\% 2\q. In total, there are 4501 data points. +; +; + _pd_proc_overall.diffractogram_id PATTERN_43 + _pd_proc.info_datetime 2042-12-13T02:37:23Z + _pd_proc.info_data_reduction + ; + Background removed by spline fitting. K\a~2~ removed using + the built-in function. Pattern smoothed by Fourier methods. + Used EVA 15. + ; + _pd_proc.info_excluded_regions '30-31\% due to quartz impurity.' +; +; + The information here applies to the diffractogram with the id + 'PATTERN_43'. The data were processed at 2:37 h GMT on the 13th of + December 2042. The data were modified as described. The data between + 30 and 31\% 2\q should be ignored, due to an impurity. +; + save_ save_pd_proc.2theta_range_inc @@ -10969,6 +11605,8 @@ save_PD_QPA_CALIB_FACTOR divided by in order to allow quantitative phase analysis to be undertaken. Further normalisation may be necessary, and can be indicated. + See also PD_QPA_INTENSITY_FACTOR and _pd_qpa_overall.method. + For a description of the quantification methodologies below, and a review on quantitative phase analysis in general, see Chapter 3.9 of International Tables, Vol. H, and references therein. @@ -10977,6 +11615,55 @@ save_PD_QPA_CALIB_FACTOR _name.object_id PD_QPA_CALIB_FACTOR _category_key.name '_pd_qpa_calib_factor.phase_id' + _description_example.case +; + data_phase_1 + _pd_phase.id PHASE_A + _pd_qpa_calib_factor.I_over_Ic 3.26 + + data_phase_2 + _pd_phase.id PHASE_B + _pd_qpa_calib_factor.I_over_Ic 4.79 + + data_phase_3 + _pd_phase.id PHASE_C + _pd_qpa_calib_factor.I_over_Ic 1.00 + + data_diffractogram_block + _pd_diffractogram.id UNKNOWN_DIFFRACTOGRAM + + loop_ + _pd_phase_mass.phase_id + _pd_phase_mass.percent + PHASE_A 52.02(15) + PHASE_B 17.90(15) + PHASE_C 30.08(14) + + _pd_qpa_overall.method I/Ic + + loop_ + _pd_qpa_intensity_factor.phase_id + _pd_qpa_intensity_factor.value + PHASE_A 242.54(81) + PHASE_B 122.6(12) + PHASE_C 43.02(25) +; + _description_example.detail +; + A diffraction pattern containing three phases (PHASE_1, PHASE_2, and + some NIST SRM646a) has been quantified using the I_over_Ic + specialisation of the RIR algorithm. + + The I/Ic value for each of the phases is specified by the values of + _pd_qpa_calib_factor.I_over_Ic. The intensity factors to which each + of the I/Ic values are applied are given by the values of + _pd_qpa_intensity_factor.value. + + The quantification values given by _pd_phase_mass.percent can now be + confirmed by following the I_over_Ic algorithm detailed in + _pd_qpa_overall.method. +; + save_ save_pd_qpa_calib_factor.absorption_diffraction @@ -11380,6 +12067,61 @@ save_PD_QPA_EXTERNAL_STD _name.object_id PD_QPA_EXTERNAL_STD _category_key.name '_pd_qpa_external_std.diffractogram_id' + _description_example.case +; + data_diffractogram_block + _pd_diffractogram.id DIFFRACTOGRAM_2 + + loop_ + _pd_phase_mass.phase_id + _pd_phase_mass.percent + _pd_phase_mass.percent_su + PHASE_1 42.81 0.56 + PHASE_2 14.73 0.24 + + _pd_qpa_external_std.diffractogram_id THE_REFERENCE + _pd_char.mass_atten_coef_mu_calc 6940 + _pd_qpa_overall.method external_standard + + data_ext_std_diffractogram + _pd_diffractogram.id THE_REFERENCE + + loop_ + _pd_phase_mass.phase_id + _pd_phase_mass.percent + _pd_phase_mass.percent_su + NIST_ALUMINA_676A 99.02 1.11 + + _pd_qpa_external_std.k_factor 293.36 + _pd_char.mass_atten_coef_mu_calc 3159 + _pd_qpa_overall.method external_standard +; + _description_example.detail +; + A diffraction pattern containing two phases (PHASE_1 and PHASE_2) has + been quantified using the external standard algorithm after Rietveld + refinement. + + The K factor, or diffractometer constant, is calculated from a + diffraction pattern of a previously characterised standard, collected + under the same conditions as the unknown, as + + K = S~s~ * (Z * M * V)~s~ * \m^*^~s~ / W~s~ + + where the subscript s denotes the standard, and S is the Rietveld scale + factor, Z is the number of formula units per unit cell, M is the + chemical formula weight, and V is the volume of the unit cell. + \m^*^~m~ is the mass absorption coefficient, and W is the crystalline + fraction. + + The absolute weight fraction of phase p, W~p~, can now be given by + + W~p~ = [S~p~ * (Z * M * V)~p~ / K] * \m^*^~m~ + + where \m^*^~m~ is the mass absorption coefficient of the entire + specimen. +; + save_ save_pd_qpa_external_std.diffractogram_id @@ -11500,7 +12242,8 @@ save_PD_QPA_INTENSITY_FACTOR quantitative phase analysis to be undertaken. Further normalisation may be necessary, and can be indicated. - The supported methodologies are enumerated in _pd_qpa_overall.method. + The supported methodologies are enumerated in _pd_qpa_overall.method. See + also PD_QPA_CALIB_FACTOR. For a review on quantitative phase analysis, see Chapter 3.9 of International Tables, Vol. H, and references therein. @@ -11513,6 +12256,55 @@ save_PD_QPA_INTENSITY_FACTOR '_pd_qpa_intensity_factor.diffractogram_id' '_pd_qpa_intensity_factor.phase_id' + _description_example.case +; + data_phase_1 + _pd_phase.id PHASE_A + _pd_qpa_calib_factor.I_over_Ic 3.26 + + data_phase_2 + _pd_phase.id PHASE_B + _pd_qpa_calib_factor.I_over_Ic 4.79 + + data_phase_3 + _pd_phase.id PHASE_C + _pd_qpa_calib_factor.I_over_Ic 1.00 + + data_diffractogram_block + _pd_diffractogram.id UNKNOWN_DIFFRACTOGRAM + + loop_ + _pd_phase_mass.phase_id + _pd_phase_mass.percent + PHASE_A 52.02(15) + PHASE_B 17.90(15) + PHASE_C 30.08(14) + + _pd_qpa_overall.method I/Ic + + loop_ + _pd_qpa_intensity_factor.phase_id + _pd_qpa_intensity_factor.value + PHASE_A 242.54(81) + PHASE_B 122.6(12) + PHASE_C 43.02(25) +; + _description_example.detail +; + A diffraction pattern containing three phases (PHASE_1, PHASE_2, and + some NIST SRM646a) has been quantified using the I_over_Ic + specialisation of the RIR algorithm. + + The I/Ic value for each of the phases is specified by the values of + _pd_qpa_calib_factor.I_over_Ic. The intensity factors to which each + of the I/Ic values are applied are given by the values of + _pd_qpa_intensity_factor.value. + + The quantification values given by _pd_phase_mass.percent can now be + confirmed by following the I_over_Ic algorithm detailed in + _pd_qpa_overall.method. +; + save_ save_pd_qpa_intensity_factor.diffractogram_id @@ -11640,6 +12432,54 @@ save_PD_QPA_INTERNAL_STD '_pd_qpa_internal_std.diffractogram_id' '_pd_qpa_internal_std.phase_id' + _description_example.case +; + _pd_diffractogram.id DIFFRACTOGRAM_1 + + loop_ + _pd_phase_mass.phase_id + _pd_phase_mass.percent + _pd_phase_mass.percent_su + PHASE_1 42.81 0.56 + PHASE_2 14.73 0.24 + NIST_ALUMINA_676A 24.76 0.28 + + _pd_qpa_internal_std.mass_percent 25.000 + _pd_qpa_internal_std.mass_percent_su 0.002 + _pd_qpa_internal_std.crystallinity_percent 99.02 + _pd_qpa_internal_std.crystallinity_percent_su 1.11 + _pd_qpa_internal_std.phase_id NIST_ALUMINA_676A + + _pd_qpa_overall.method ZMV +; + _description_example.detail +; + A diffraction pattern containing three phases (PHASE_1, PHASE_2, and + some NIST SRM646a) has been quantified using the ZMV algorithm after + Rietveld refinement. + + The diffraction pattern was collected from a specimen containing + 25.000 +- 0.002 wt% internal standard (i.e. 1 g added to 3 g of unknown + to make a specimen with total weight of 4 g). The internal standard is + known to be 99.02 +- 1.11 % crystalline, and so the reported value of + _pd_phase_mass.percent for the standard is 25.000 * 0.9902 = 24.96 wt%. + + The weight fractions derived from the ZMW algorithm were then scaled as + + W~p~^absolute^ = W~p~^ZMV^ * (W~s~^known^ / W~s~^ZMV^) + + where W is the weight percentage, p is the phase, s is the standard + 'ZMV' is the weight fraction from the ZMV algorithm, and 'known' is the + known addition of standard (_pd_qpa_internal_std.mass_percent). These + are the values reported as _pd_phase_mass.percent. Any difference + between the sum of the _pd_phase_mass.percent values and 100 wt% can + be attributed to unanalysed or amorphous phases. + + The crystal structure of the internal standard is described by the + information linked to the _pd_phase.id data item with the value + 'NIST_ALUMINA_676A'. +; + save_ save_pd_qpa_internal_std.crystallinity_percent @@ -11846,7 +12686,9 @@ save_pd_qpa_overall.method of any _pd_qpa_calib_factor.* value that is given. If 'other' is chosen, further information must be given in - _pd_qpa_overall.special_details + _pd_qpa_overall.special_details. + + See examples in PD_QPA_* as to how this category is used. ; _name.category_id pd_qpa_overall _name.object_id method @@ -12140,6 +12982,34 @@ save_PD_SPEC _name.category_id PD_GROUP _name.object_id PD_SPEC _category_key.name '_pd_spec.id' + _description_example.case +; + _pd_spec.id ABC123_03 + _pd_spec.description 'Iron ore from FeOre Inc. ID number ABC123' + _pd_spec.mount_mode reflection + _pd_spec.mounting 'back-packed powder pellet' + _pd_spec.orientation horizontal + _pd_spec.preparation + ; + 50 g of received sample was homogenised and cone-and-quartered + to obtain a 3 g split. 1 g of \a-alumina was added as an internal + standard. The specimen was micronised for 15 min with 15 ml of + ethanol and dried at 45 \%C. The resulting powder was backpressed + into a holder with a semi-automated press. + ; + _pd_spec.shape flat_sheet + _pd_spec.size_axial 25.0 + _pd_spec.size_equat 25.0 + _pd_spec.size_thick 3.5 +; + _description_example.detail +; + A specimen of iron ore, from FeOre Inc., with an added internal + standard was prepared for analysis. The data were collected in + reflection on an instrument where the incident and diffracted beams + are vertical. The specimen flat, and is 25.0 x 25.0 mm, or it could be + inferred to be 25 mm diameter. The specimen was prepared as described. +; save_ @@ -12160,6 +13030,12 @@ save_pd_spec.description _type.container Single _type.contents Text + loop_ + _description_example.case + 'Grab specimen from goethite bottle from Acme. Lot #1234.' + 'By-product found in corroded pipe threads.' + 'Mystery powder found in back of cupboard.' + save_ save_pd_spec.id @@ -12830,4 +13706,6 @@ save_ Updated descriptions of data items linked to _pd_data.point_id to clarify that identical values refer to the same data point in each disparate loop; they cannot be assigned values independently. + + Added examples to PD_CALIB_INCIDENT_INTENSITY. ;