From 415e78f0cc508e76f1dd3907b75d3b3f53b9a68a Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 15:42:26 +0800 Subject: [PATCH 01/16] pd_calib_d_to_tof: added key --- cif_pd.dic | 4 ++++ 1 file changed, 4 insertions(+) diff --git a/cif_pd.dic b/cif_pd.dic index 2b53f17..62ae2dd 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -2489,6 +2489,8 @@ save_PD_CALIB_D_TO_TOF _description_example.case _description_example.detail ; + _pd_diffractogram.id TOF_DATA_BANK_1 + loop_ _pd_calib_d_to_tof.id _pd_calib_d_to_tof.power @@ -2504,6 +2506,8 @@ save_PD_CALIB_D_TO_TOF + 0.08099 * d_spacing^2^ ; ; + _pd_diffractogram.id TOF_DATA_BANK_2 + loop_ _pd_calib_d_to_tof.id _pd_calib_d_to_tof.power From 572a7188ca18e0ec81bf97c9dd4899604e1a0ff3 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 15:44:28 +0800 Subject: [PATCH 02/16] _pd_calib_incident_intensity: fix typos --- cif_pd.dic | 8 ++++---- 1 file changed, 4 insertions(+), 4 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 62ae2dd..1336734 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -2926,17 +2926,17 @@ save_PD_CALIB_INCIDENT_INTENSITY _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 + _pd_calib_incident_intensity.phase_id SRM1976_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. + SRM1976_15341c3a. ; ; - _pd_instr.id a3643812 - _pd_diffractogram.id WHITE_POWDER + _pd_diffractogram.id WHITE_POWDER + _pd_diffractogram.instr_id a3643812 loop_ _pd_data.point_id From c3d15c7e6bdbae3ac79db78902d3e04b12e159a0 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 15:47:16 +0800 Subject: [PATCH 03/16] PD_CALIB_INCIDENT_INTENSITY: added _audit_dataset.id values --- cif_pd.dic | 7 +++++++ 1 file changed, 7 insertions(+) diff --git a/cif_pd.dic b/cif_pd.dic index 1336734..625dcfd 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -2911,6 +2911,8 @@ save_PD_CALIB_INCIDENT_INTENSITY _description_example.case _description_example.detail ; + _audit_dataset.id b007cf82-6338-4387-9abb-2825c6bf37b6 + _pd_calib_incident_intensity.instr_id a3643812 _pd_calib_incident_intensity.incident_counts 4231 _pd_calib_incident_intensity.special_details 'From beam monitor.' @@ -2935,6 +2937,8 @@ save_PD_CALIB_INCIDENT_INTENSITY SRM1976_15341c3a. ; ; + _audit_dataset.id b007cf82-6338-4387-9abb-2825c6bf37b6 + _pd_diffractogram.id WHITE_POWDER _pd_diffractogram.instr_id a3643812 @@ -2957,6 +2961,9 @@ save_PD_CALIB_INCIDENT_INTENSITY the incident intensity calibration linked to that instrument. The SU values have also been calculated for the _pd_proc.intensity_total values. + + Identical _audit_dataset.id value show that the identical + instrument id values must refer to the same instrument. ; save_ From 25c7a8676af370832e83ffee4a19495c9a1477c9 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 15:49:38 +0800 Subject: [PATCH 04/16] PD_DATA: added _pd_diffractogram.id values --- cif_pd.dic | 10 +++++++++- 1 file changed, 9 insertions(+), 1 deletion(-) diff --git a/cif_pd.dic b/cif_pd.dic index 625dcfd..99b16a1 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -4884,6 +4884,8 @@ save_PD_DATA _description_example.case _description_example.detail ; + _pd_diffractogram.id histogram01 + loop_ _pd_data.point_id _pd_meas.2theta_scan @@ -4909,6 +4911,8 @@ save_PD_DATA with the data name _pd_diffractogram.id given in that data block. ; ; + _pd_diffractogram.id pattern02 + loop_ _pd_data.point_id _pd_meas.time_of_flight @@ -4941,7 +4945,9 @@ save_PD_DATA with the data name _pd_diffractogram.id given in that data block. ; ; - loop_ + _pd_diffractogram.id diffractogram03 + + loop_ _pd_data.point_id _pd_meas.2theta_scan _pd_proc.2theta_corrected @@ -4968,6 +4974,8 @@ save_PD_DATA with the data name _pd_diffractogram.id given in that data block. ; ; + _pd_diffractogram.id rawdata04 + loop_ _pd_data.point_id _pd_meas.2theta_scan From 8a68efdb54479ef0a0f436097d9b79dbd9caec25 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 15:53:40 +0800 Subject: [PATCH 05/16] PD_DIFFRACTOGRAM: added a data_ to be consistent with other example --- cif_pd.dic | 2 ++ 1 file changed, 2 insertions(+) diff --git a/cif_pd.dic b/cif_pd.dic index 99b16a1..851d00b 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -6853,6 +6853,8 @@ save_PD_DIFFRACTOGRAM _description_example.case _description_example.detail ; + data_combined + _diffrn.id highTemp _diffrn.ambient_temperature 1273 _diffrn.ambient_pressure 101.3 From b15eb53f8394d2dd36d228ea4d5b9f31fc55106b Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 15:54:08 +0800 Subject: [PATCH 06/16] _pd_instr: add radiation id --- cif_pd.dic | 8 ++++++-- 1 file changed, 6 insertions(+), 2 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 851d00b..026f7b6 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -7140,6 +7140,7 @@ save_PD_INSTR _pd_instr.dist_mono_spec 402 _pd_instr.dist_src_mono 39 _pd_instr.beam_size_ax 10.5 + _pd_instr.radiation_id Hires_tube _pd_instr.slit_ax_mono_spec 10.0 _pd_instr.slit_eq_mono_spec 0.5 _pd_instr.soller_ax_mono_spec 2.5 @@ -7173,7 +7174,8 @@ save_PD_INSTR 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 Å. + radiation with a wavelength of 1.540596 Å. It is linked to the instrument + through the value of _pd_instr.radiation_id. ; ; _diffrn_radiation.id Cobalt_tube @@ -7197,6 +7199,7 @@ save_PD_INSTR _pd_instr.detector_circle_radius 117.5 _pd_instr.dist_src_spec 117.5 _pd_instr.beam_size_ax 9.8 + _pd_instr.radiation_id Cobalt_tube _pd_instr.slit_ax_src_spec 9.5 _pd_instr.soller_ax_src_spec 5.0 _pd_instr.source_size_ax 8.5 @@ -7223,7 +7226,8 @@ save_PD_INSTR 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. Hölzer et al. Phys. Rev. A 56, 4554. + described by G. Hölzer et al. Phys. Rev. A 56, 4554. It is linked to + the instrument through the value of _pd_instr.radiation_id. ; save_ From 1684d3b8846323a7b5cf520d7f0282bb9b639ede Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 16:01:33 +0800 Subject: [PATCH 07/16] pd_peak: add more tags to properly associate wavelengths and peaks --- cif_pd.dic | 14 ++++++++++++++ 1 file changed, 14 insertions(+) diff --git a/cif_pd.dic b/cif_pd.dic index 026f7b6..e56d489 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -9727,6 +9727,8 @@ save_PD_PEAK _description_example.case _description_example.detail ; + _pd_diffractogram.id PEAKYPLOT + loop_ _pd_peak.id _pd_peak.2theta_centroid @@ -9745,6 +9747,14 @@ save_PD_PEAK uncertainty (eg 1023 ± 7). ; ; + _pd_diffractogram.id PEAKYPLOT + _pd_diffractogram.instr_id Cu_workhorse + + _pd_instr.id Cu_workhorse + _pd_instr.radiation_id Cu_tube + + _diffrn_radiation.id Cu_tube + loop_ _diffrn_radiation_wavelength.id _diffrn_radiation_wavelength.value @@ -9773,6 +9783,10 @@ save_PD_PEAK d-spacing from the data's original 2θ results is given in the final column, which corresponds to 1.540596 Å, as given in the top-most loop. + + The individual data names at the top are to associate the radiation + source with the instrument, and the instrument with the diffractogram, + allowing for the correct wavelength to be specified in the peak loop. ; save_ From 4c1d0154de50f734da65a629dcf42c7eba984c18 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 16:03:36 +0800 Subject: [PATCH 08/16] _pd_peak_overall: add pd diffractogram id --- cif_pd.dic | 5 ++++- 1 file changed, 4 insertions(+), 1 deletion(-) diff --git a/cif_pd.dic b/cif_pd.dic index e56d489..5d27746 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -10163,13 +10163,16 @@ save_PD_PEAK_OVERALL _category_key.name '_pd_peak_overall.id' _description_example.case ; - _pd_peak_overall.id PEAK_GROUP_1 + _pd_diffractogram.id UNKNOWN_PEAKS + + _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. ; + loop_ _pd_peak.id _pd_peak.2theta_centroid From f6ffa39a86bc054785a0f1ecbacaba5e32d57c95 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 17:16:17 +0800 Subject: [PATCH 09/16] pd_phase_mass: update examples One custom was left, and anotated as a summary block. The one with values disributed amongst blocks was labelled as the preferred method. --- cif_pd.dic | 37 +++++++++++++++++++++++-------------- 1 file changed, 23 insertions(+), 14 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 5d27746..6a8f5b3 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -10513,7 +10513,8 @@ save_PD_PHASE_MASS associated with one diffractogram and three phases. Blocks containing information about more than one phase or - diffractogram must set a non-default value for _audit.schema. + diffractogram must set a non-default value for _audit.schema. If a + summary block is desired, this is the method. ; ; data_b1 @@ -10534,23 +10535,34 @@ save_PD_PHASE_MASS ; Identical as previous example, but values distributed amongst blocks so as to maintain the default value of _audit.schema. + This is the preferred methodology. ; ; - _audit.schema Custom + data_b1 + _pd_diffractogram.id ANOTHER_DIFFRACTOGRAM + _pd_phase.id PHASE_1 + + _pd_phase_mass.percent 45.45 + _pd_phase_mass.absolute 30.36 + _pd_phase_mass.original 40.49 + data_b2 _pd_diffractogram.id ANOTHER_DIFFRACTOGRAM + _pd_phase.id PHASE_2 _pd_qpa_internal_std.mass_percent 25.000 - _pd_qpa_internal_std.phase_id PHASE_2 - loop_ - _pd_phase_mass.phase_id - _pd_phase_mass.percent - _pd_phase_mass.absolute - _pd_phase_mass.original - PHASE_1 45.45 30.36 40.49 - PHASE_2 37.42 25.00 0 - PHASE_3 17.13 11.44 15.26 + _pd_phase_mass.percent 37.42 + _pd_phase_mass.absolute 25.00 + _pd_phase_mass.original 0 + + data_b3 + _pd_diffractogram.id ANOTHER_DIFFRACTOGRAM + _pd_phase.id PHASE_3 + + _pd_phase_mass.percent 17.13 + _pd_phase_mass.absolute 11.44 + _pd_phase_mass.original 15.26 ; ; Tabulation of quantitative phase analysis data. @@ -10561,9 +10573,6 @@ save_PD_PHASE_MASS _pd_phase_mass.absolute. We can then calculate the original mass percentages, those present in the sample before adding the internal standard, given by _pd_phase_mass.original. - - Blocks containing information about more than one phase or - diffractogram must set a non-default value for _audit.schema. ; save_ From 1b06b22c01eedc2629b4e726f224caf41a0d69bd Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 17:25:03 +0800 Subject: [PATCH 10/16] _pd_pref_orient_March_Dollase: removed custom Altered exapmle with only a single row of values to assign as if were Set datanames --- cif_pd.dic | 32 ++++++++++++++++++-------------- 1 file changed, 18 insertions(+), 14 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 6a8f5b3..297cf64 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -10997,32 +10997,36 @@ save_PD_PREF_ORIENT_MARCH_DOLLASE _description_example.case _description_example.detail ; - _audit.schema Custom + data_p1 + _pd_diffractogram.id DIFFPAT_1 + _pd_phase.id PHASE_1 loop_ _pd_pref_orient_March_Dollase.id - _pd_pref_orient_March_Dollase.diffractogram_id - _pd_pref_orient_March_Dollase.phase_id _pd_pref_orient_March_Dollase.hkl _pd_pref_orient_March_Dollase.r _pd_pref_orient_March_Dollase.r_su - 1 DIFFPAT_1 PHASE_1 [ 1 0 4 ] 0.79 0.12 - 2 DIFFPAT_1 PHASE_2 [ 0 0 1 ] 0.66 0.15 + 1 [ 1 0 4 ] 0.79 0.12 + + data_p2 + _pd_diffractogram.id DIFFPAT_1 + _pd_phase.id PHASE_2 + + _pd_pref_orient_March_Dollase.id 1 + _pd_pref_orient_March_Dollase.hkl [ 0 0 1 ] + _pd_pref_orient_March_Dollase.r 0.66(15) ; ; - Showing a fully qualified reporting of the preferred-orientation - corrections for a phase with a _pd_phase.id of 'PHASE_1' a phase - with a _pd_phase.id of 'PHASE_2', both belonging to a diffractogram - with a _pd_diffractogram.id of 'DIFFPAT_1. + Reporting the preferred-orientation corrections for phases PHASE_1 + and PHASE_2, both from diffractogram DIFFPAT_1. The first phase has the preferred-orientation direction of 104, with a March r parameter value of 0.79 with a standard uncertainty of 0.12. - The second phase has the preferred-orientation direction of 001, with a - March r parameter value of 0.66 with a standard uncertainty of 0.15. - - As information about more than one phase is present in the data block - _audit.schema takes a non-default value. + The second phase has the preferred-orientation direction of 001, with + a March r parameter value of 0.66 with a standard uncertainty of 0.15. + It is permissible to allocate values to Loop data names as if they + were Set data names if there is only a single row of data. ; ; _pd_diffractogram.id DIFFPAT_A From 327ae1b7065703f5dd2688cbf90e44b67717b075 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 17:49:33 +0800 Subject: [PATCH 11/16] _pd_pref_orient_spherical_harmonics removed custom added extra Also added a geom and a texture index --- cif_pd.dic | 57 +++++++++++++++++++++++++++++++++++++----------------- 1 file changed, 39 insertions(+), 18 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 297cf64..22a169e 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -11326,44 +11326,61 @@ save_PD_PREF_ORIENT_SPHERICAL_HARMONICS _description_example.case _description_example.detail ; - _audit.schema Custom + data_s1 + _pd_diffractogram.id DIFFPAT_A + _pd_phase.id PHASE_A loop_ _pd_pref_orient_spherical_harmonics.id - _pd_pref_orient_spherical_harmonics.phase_id - _pd_pref_orient_spherical_harmonics.diffractogram_id _pd_pref_orient_spherical_harmonics.y_ij _pd_pref_orient_spherical_harmonics.c_ij _pd_pref_orient_spherical_harmonics.c_ij_su - a PHASE_A DIFFPAT_A [0 0] 1.0 . - b PHASE_A DIFFPAT_A [2 0] 1.538 0.013 - c PHASE_B DIFFPAT_A [0 0] 1.0 . - d PHASE_B DIFFPAT_A [4 1] -0.066 0.010 - e PHASE_A DIFFPAT_B [0 0] 1.0 . - f PHASE_A DIFFPAT_B [2 0] 1.630 0.014 + a [0 0] 1.0 . + b [2 0] 1.538 0.013 + + data_s2 + _pd_diffractogram.id DIFFPAT_A + _pd_phase.id PHASE_B + + loop_ + _pd_pref_orient_spherical_harmonics.id + _pd_pref_orient_spherical_harmonics.y_ij + _pd_pref_orient_spherical_harmonics.c_ij + I [0 0] 1.0 + II [4 1] -0.066(10) + + data_s13 + _pd_diffractogram.id DIFFPAT_B + _pd_phase.id PHASE_A + + loop_ + _pd_pref_orient_spherical_harmonics.id + _pd_pref_orient_spherical_harmonics.y_ij + _pd_pref_orient_spherical_harmonics.c_ij + _pd_pref_orient_spherical_harmonics.c_ij_su + q [0 0] 1.0 . + w [2 0] 1.630 0.014 ; ; - Showing a fully qualified reporting of the preferred-orientation - corrections for phases with the _pd_phase.id of 'PHASE_A' and 'PHASE_B' - present in the diffractograms with the _pd_diffractogram.id of - 'DIFFPAT_A' and 'DIFFPAT_B'. + Reporting the preferred-orientation corrections for phases PHASE_A + and PHASE_B, both in diffractograms DIFFPAT_A and DIFFPAT_B. - In diffractogram 'DIFFPAT_A', both 'PHASE_A' and 'PHASE_B' have + In diffractogram DIFFPAT_A, both PHASE_A and PHASE_B have corrections applied, with the non-(0,0) order/term pairs taking the values (2,0) and (4,1), with coefficients of 1.538(13) and -0.066(10), respectively. - In diffractogram 'DIFFPAT_B', only 'PHASE_A' has corrections applied, + In diffractogram DIFFPAT_B, only PHASE_A has corrections applied, with the non-(0,0) order/term pair taking the value (2,0), with a coefficient of 1.630(14). - - As information for more than one phase is contained in the data block, - _audit.schema has non-default value 'Custom'. ; ; _pd_diffractogram.id DIFFPAT_A _pd_phase.id PHASE_A + _pd_pref_orient.geom cap + _pd_pref_orient.spherical_harmonics_texture_index 1.5688 + loop_ _pd_pref_orient_spherical_harmonics.id _pd_pref_orient_spherical_harmonics.y_i @@ -11383,6 +11400,10 @@ save_PD_PREF_ORIENT_SPHERICAL_HARMONICS order/term pairs of (0,0), (2,0), (4,0), and (4, -3), and their magnitudes and standard uncertainties are 1.0, 1.538(13), 0.913(16), and -0.166(10), respectively. + + The correction applied corresponds to the capillary geometry. + The texture index is also given, indicating the severity of the + preferred orientation. ; save_ From 9ef544de6838d3cf6574070706746603b4303b09 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 20:46:49 +0800 Subject: [PATCH 12/16] _pd_qpa_intensity_factor and _pd_qpa_calib_factor: same example But one is a custom schema --- cif_pd.dic | 56 ++++++++++++++++++++++++++++-------------------------- 1 file changed, 29 insertions(+), 27 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 22a169e..2e4c335 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -12701,36 +12701,38 @@ save_PD_QPA_CALIB_FACTOR _description_example.case ; data_phase_A - _pd_phase.id PHASE_A - _pd_qpa_calib_factor.I_over_Ic 3.26 + _pd_phase.id PHASE_A + _pd_qpa_calib_factor.I_over_Ic 3.26 data_phase_B - _pd_phase.id PHASE_B - _pd_qpa_calib_factor.I_over_Ic 4.79 + _pd_phase.id PHASE_B + _pd_qpa_calib_factor.I_over_Ic 4.79 data_phase_C - _pd_phase.id PHASE_C - _pd_qpa_calib_factor.I_over_Ic 1.00 + _pd_phase.id PHASE_C + _pd_qpa_calib_factor.I_over_Ic 1.00 - data_diffractogram_block - _audit.schema Custom - _pd_diffractogram.id UNKNOWN_DIFFRACTOGRAM + data_diffractogram_block_I + _pd_diffractogram.id UNKNOWN + _pd_phase.id PHASE_A - 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_phase_mass.percent 52.02(15) + _pd_qpa_overall.method I/Ic + _pd_qpa_intensity_factor.value 242.54(81) - _pd_qpa_overall.method I/Ic + data_diffractogram_block_II + _pd_diffractogram.id UNKNOWN + _pd_phase.id PHASE_B - 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) + _pd_phase_mass.percent 17.90(15) + _pd_qpa_intensity_factor.value 122.6(12) + + data_diffractogram_block_III + _pd_diffractogram.id UNKNOWN + _pd_phase.id PHASE_C + + _pd_phase_mass.percent 30.08(14) + _pd_qpa_intensity_factor.value 43.02(25) ; _description_example.detail ; @@ -12747,10 +12749,9 @@ save_PD_QPA_CALIB_FACTOR confirmed by following the I/Ic algorithm detailed in _pd_qpa_overall.method. - As there are loops containing data names linked to key data names of - Set categories (_pd_phase_mass.phase_id and - _pd_qpa_intensity_factor.phase_id), the _audit.schema value for the - last block must take the value 'Custom' + This example is the same as for PD_QPA_INTENSITY_FACTOR, but with + values distributed amongst blocks such that a custom _audit.schema + value is not needed. ; save_ @@ -13389,7 +13390,8 @@ save_PD_QPA_INTENSITY_FACTOR confirmed by following the I/Ic algorithm detailed in _pd_qpa_overall.method. - As we are looping data names linked to _pd_phase.id, the _audit.schema + This example is the same as for PD_QPA_CALIB_FACTOR, but as we are + looping data names linked to _pd_phase.id, the _audit.schema is set to Custom. ; From cefe97efb4f8862b4bdcbf03cd86254fd6c5fd63 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 20:57:52 +0800 Subject: [PATCH 13/16] _pd_qpa_internal_std: remove custom --- cif_pd.dic | 31 +++++++++++++++++-------------- 1 file changed, 17 insertions(+), 14 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 2e4c335..931447e 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -13524,24 +13524,27 @@ save_PD_QPA_INTERNAL_STD _description_example.case ; - _audit.schema Custom + data_int_std _pd_diffractogram.id DIFFRACTOGRAM_1 + _pd_phase.id NIST_ALUMINA_676A - loop_ - _pd_phase_mass.phase_id - _pd_phase_mass.absolute - _pd_phase_mass.absolute_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_internal_std.mass_percent 25.000(2) + _pd_qpa_internal_std.crystallinity_percent 99.02(111) + _pd_phase_mass.absolute 24.76(28) _pd_qpa_overall.method ZMV + + data_b1 + _pd_diffractogram.id DIFFRACTOGRAM_1 + _pd_phase.id PHASE_1 + + _pd_phase_mass.absolute 42.81(56) + + data_b1 + _pd_diffractogram.id DIFFRACTOGRAM_1 + _pd_phase.id PHASE_2 + + _pd_phase_mass.absolute 14.73(24) ; _description_example.detail ; From a7eb1c16d8e81041be4bdb49e57eed82c2d4dd3a Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 21:06:37 +0800 Subject: [PATCH 14/16] _pd_qpa_internal_std: added discussion on crystallinity to example and category description --- cif_pd.dic | 30 ++++++++++++++++-------------- 1 file changed, 16 insertions(+), 14 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 931447e..fdad11a 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -13504,12 +13504,13 @@ save_PD_QPA_INTERNAL_STD This can be done as - W~p~^abs.^ = W~p~^rel.^ * (W~s~^known^ / W~s~^rel.^) + W~p~^abs.^ = W~p~^rel.^ * (W~s~^known^ * X~s~ / W~s~^rel.^) where p and s represent the analyte phase and standard phase, respectively, W is the weight fraction, 'abs.' is absolute, 'rel.' is relative, and - 'known' is the known addition. Here, W~s~^rel.^ is the relative amount of - standard as calculated by the quantification algorithm. + 'known' is the known addition. X~s~ is the crystallinity of the internal + standard. Here, W~s~^rel.^ is the relative amount of standard as calculated + by the quantification algorithm. For a review on quantitative phase analysis, see Chapter 3.9 of International Tables, Vol. H, and references therein. @@ -13552,23 +13553,24 @@ save_PD_QPA_INTERNAL_STD some NIST SRM676a) 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.absolute for the standard is: + The diffraction pattern was collected from a specimen with a known + addition of 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.absolute for the standard is: 25.000 * 0.9902 = 24.76 wt%. The weight fractions derived from the ZMV algorithm were then scaled as - W~p~^absolute^ = W~p~^ZMV^ * (W~s~^known^ / W~s~^ZMV^) + W~p~^absolute^ = W~p~^ZMV^ * (W~s~^known^ * X~s~ / 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.absolute. Any difference - between the sum of the _pd_phase_mass.absolute values and 100 wt% can - be attributed to unanalysed or amorphous phases. + 'ZMV' is the weight fraction from the ZMV algorithm, 'known' is the + known addition of standard (_pd_qpa_internal_std.mass_percent), and + X~s~ is the crystallinity of the internal standard. These are the + values reported as _pd_phase_mass.absolute. Any difference between + the sum of the _pd_phase_mass.absolute 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 From 6919ef3242b443bdd1286c4b1be16b9178dfcdef Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 6 Jul 2026 21:18:46 +0800 Subject: [PATCH 15/16] fix layout --- cif_pd.dic | 4 ++-- 1 file changed, 2 insertions(+), 2 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index fdad11a..6273429 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -7174,8 +7174,8 @@ save_PD_INSTR 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 Å. It is linked to the instrument - through the value of _pd_instr.radiation_id. + radiation with a wavelength of 1.540596 Å. It is linked to the + instrument through the value of _pd_instr.radiation_id. ; ; _diffrn_radiation.id Cobalt_tube From d3575a593680cfc87dfbd3e897c9e4dadbf09260 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Tue, 7 Jul 2026 18:52:19 +0800 Subject: [PATCH 16/16] fix duplicate example --- cif_pd.dic | 31 ++++++++++--------------------- 1 file changed, 10 insertions(+), 21 deletions(-) diff --git a/cif_pd.dic b/cif_pd.dic index 9ca79fa..acd99cd 100644 --- a/cif_pd.dic +++ b/cif_pd.dic @@ -10630,31 +10630,20 @@ save_PD_PHASE_MASS This is the preferred methodology. ; ; - data_b1 - _pd_diffractogram.id ANOTHER_DIFFRACTOGRAM - _pd_phase.id PHASE_1 - - _pd_phase_mass.percent 45.45 - _pd_phase_mass.absolute 30.36 - _pd_phase_mass.original 40.49 - - data_b2 + data_all_results + _audit_schema Custom _pd_diffractogram.id ANOTHER_DIFFRACTOGRAM - _pd_phase.id PHASE_2 _pd_qpa_internal_std.mass_percent 25.000 - _pd_phase_mass.percent 37.42 - _pd_phase_mass.absolute 25.00 - _pd_phase_mass.original 0 - - data_b3 - _pd_diffractogram.id ANOTHER_DIFFRACTOGRAM - _pd_phase.id PHASE_3 - - _pd_phase_mass.percent 17.13 - _pd_phase_mass.absolute 11.44 - _pd_phase_mass.original 15.26 + loop_ + _pd_phase_mass.phase_id + _pd_phase_mass.percent + _pd_phase_mass.absolute + _pd_phase_mass.original + PHASE_1 45.45 30.36 40.49 + PHASE_2 37.42 25.00 0 + PHASE_3 17.13 11.44 15.26 ; ; Tabulation of quantitative phase analysis data.