From da5d13e6b5a7ea3b284ba122ce1525f3e4a0df97 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Mon, 16 Jan 2023 22:06:53 +0800 Subject: [PATCH 01/24] update the QPA categories I started writing up how to use them, and realised I had overthought things. --- cif_pow.dic | 638 ++++++++++++++++++++++++++++++++++------------------ 1 file changed, 422 insertions(+), 216 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index a1f5c8d..fb5c541 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -14,7 +14,7 @@ data_CIF_POW _dictionary.title CIF_POW _dictionary.class Instance _dictionary.version 2.5.0 - _dictionary.date 2023-01-10 + _dictionary.date 2023-01-16 _dictionary.uri https://raw.githubusercontent.com/COMCIFS/Powder_Dictionary/master/cif_pow.dic _dictionary.ddl_conformance 3.11.10 @@ -130,7 +130,7 @@ save_PD_BLOCK ; _pd_block.id is used to assign a unique ID code to a data block. This code is then used for references between different blocks - (see _pd_block_diffractogram.id, _pd_qpa_ext_std.block_id + (see _pd_block_diffractogram.id, _pd_qpa_external_std.block_id and _pd_phase.block_id). Note that a data block may contain only a single diffraction @@ -647,11 +647,11 @@ save_pd_calib.std_internal_mass_percent _definition.id '_pd_calib.std_internal_mass_percent' _definition_replaced.id 1 - _definition_replaced.by '_pd_qpa_int_std.mass_percent' + _definition_replaced.by '_pd_qpa_internal_std.mass_percent' _definition.update 2023-01-06 _description.text ; - This item is deprecated. Please see _pd_qpa_int_std.mass_percent. + This item is deprecated. Please see _pd_qpa_internal_std.mass_percent. Per cent presence of the internal standard specified by the data item _pd_calib.std_internal_name expressed as 100 times @@ -673,11 +673,11 @@ save_pd_calib.std_internal_mass_percent_su _definition.id '_pd_calib.std_internal_mass_percent_su' _definition_replaced.id 1 - _definition_replaced.by '_pd_qpa_int_std.mass_percent_su' + _definition_replaced.by '_pd_qpa_internal_std.mass_percent_su' _definition.update 2023-01-06 _description.text ; - This item is deprecated. Please see _pd_qpa_int_std.mass_percent_su. + This item is deprecated. Please see _pd_qpa_internal_std.mass_percent_su. Standard uncertainty of _pd_calib.std_internal_mass_percent. ; @@ -5865,8 +5865,8 @@ save_pd_phase_mass.percent Total mass of the phase expressed as a percentage of the total mass of the specimen. - If _pd_qpa_int_std.mass_percent or _pd_qpa_ext_std.k_factor is - present, the values given are assumed to be in absolute terms. + If _pd_qpa_internal_std.mass_percent or _pd_qpa_external_std.k_factor + is present, the values given are assumed to be in absolute terms. The value of the mass percent given to the internal standard represents the total crystalline contribution of that standard. @@ -7466,18 +7466,114 @@ save_pd_proc.number_of_points save_ -save_PD_QPA_EXT_STD +save_PD_QPA_CALIB_FACTOR - _definition.id PD_QPA_EXT_STD + _definition.id PD_QPA_CALIB_FACTOR _definition.scope Category - _definition.class Loop - _definition.update 2023-01-06 + _definition.class Set + _definition.update 2023-01-15 + _description.text +; + This category gives the value of the calibration constant by which the + calculated intensity or scale factor associated with the given phase is + divided in order to allow quantitative phase analysis to be undertaken. + Further normalisation may be necessary, and can be indicated. + + For example, if quantification was undertaken using RIR values, those + values can be recorded with _pd_qpa_calib_factor.value +; + _name.category_id PD_GROUP + _name.object_id PD_QPA_CALIB_FACTOR + _category_key.name '_pd_qpa_calib_factor.phase_id' + +save_ + +save_pd_qpa_calib_factor.phase_id + + _definition.id '_pd_qpa_calib_factor.phase_id' + _definition.update 2023-01-15 + _description.text +; + The phase (see _pd_phase.id) to which the calibration factor applies. +; + _name.category_id pd_qpa_calib_factor + _name.object_id phase_id + _name.linked_item_id '_pd_phase.id' + _type.purpose Link + _type.source Related + _type.container Single + _type.contents Text + +save_ + +save_pd_qpa_calib_factor.special_details + + _definition.id '_pd_qpa_calib_factor.special_details' + _definition.update 2023-01-15 _description.text ; - This category identifies the external standard used for - quantitative phase analysis. Loops may be used for calibration - information that differs by detector channel, otherwise only a - single value should be recorded per diffractogram. + Description of calibration factor details that require additional detail, + or cannot otherwise be recorded using other PD_QPA_CALIB_FACTOR data items. +; + _name.category_id pd_qpa_calib_factor + _name.object_id special_details + _type.purpose Describe + _type.source Recorded + _type.container Single + _type.contents Text + +save_ + +save_pd_qpa_calib_factor.value + + _definition.id '_pd_qpa_calib_factor.value' + _definition.update 2023-01-15 + _description.text +; + A calibration value by which a calculated intensity or scale factor + associated with the given phase is divided by in the process of quantitative + phase analysis. + + The type of calibration factor, and hence the correction quantitative phase + analysis equation, is given in _pd_qpa_calib_factor.type. +; + _name.category_id pd_qpa_calib_factor + _name.object_id value + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.value_su + + _definition.id '_pd_qpa_calib_factor.value_su' + _definition.update 2023-01-14 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.value. +; + _name.category_id pd_qpa_calib_factor + _name.object_id value_su + _name.linked_item_id '_pd_qpa_calib_factor.value' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + +save_PD_QPA_EXTERNAL_STD + + _definition.id PD_QPA_EXTERNAL_STD + _definition.scope Category + _definition.class Set + _definition.update 2023-01-15 + _description.text +; + This category identifies the external diffractogram used for + quantitative phase analysis. Quantification by external standard is typically carried out using the O'Connor and Raven algorithm in conjunction with whole- @@ -7490,18 +7586,14 @@ save_PD_QPA_EXT_STD Chapter 3.9 of International Tables, Vol. H, and references therein. ; _name.category_id PD_GROUP - _name.object_id PD_QPA_EXT_STD - - loop_ - _category_key.name - '_pd_qpa_ext_std.detector_id' - '_pd_qpa_ext_std.block_id' + _name.object_id PD_QPA_EXTERNAL_STD + _category_key.name '_pd_qpa_external_std.diffractogram_id' save_ -save_pd_qpa_ext_std.block_id +save_pd_qpa_external_std.diffractogram_block_id - _definition.id '_pd_qpa_ext_std.block_id' + _definition.id '_pd_qpa_external_std.diffractogram_block_id' _definition.update 2023-01-09 _description.text ; @@ -7512,8 +7604,8 @@ save_pd_qpa_ext_std.block_id Further references to additional phases present are given in that data block. ; - _name.category_id pd_qpa_ext_std - _name.object_id block_id + _name.category_id pd_qpa_external_std + _name.object_id diffractogram_block_id _name.linked_item_id '_pd_block.id' _type.purpose Link _type.source Assigned @@ -7522,31 +7614,28 @@ save_pd_qpa_ext_std.block_id save_ -save_pd_qpa_ext_std.detector_id +save_pd_qpa_external_std.diffractogram_id - _definition.id '_pd_qpa_ext_std.detector_id' - _definition.update 2016-10-18 + _definition.id '_pd_qpa_external_std.diffractogram_id' + _definition.update 2023-01-15 _description.text ; - A code which identifies the detector or channel number to which - the external standard data applies. Note that this code should - match a detector from _pd_meas.detector_id and may be omitted if - only one detector is used. + The diffractogram (see _pd_diffractogram.id) which is being used to + calculate the diffractometer constant. ; - _name.category_id pd_qpa_ext_std - _name.object_id detector_id - _name.linked_item_id '_pd_meas.detector_id' + _name.category_id pd_qpa_external_std + _name.object_id diffractogram_id + _name.linked_item_id '_pd_diffractogram.id' _type.purpose Link - _type.source Assigned + _type.source Related _type.container Single - _type.contents Code - _enumeration.default . + _type.contents Text save_ -save_pd_qpa_ext_std.k_factor +save_pd_qpa_external_std.k_factor - _definition.id '_pd_qpa_ext_std.k_factor' + _definition.id '_pd_qpa_external_std.k_factor' _definition.update 2023-01-06 _description.text ; @@ -7567,7 +7656,7 @@ save_pd_qpa_ext_std.k_factor Refinement Procedure in Assaying Powdered Mixtures. Powder Diffraction, 3(1), 2-6. doi:10.1017/s0885715600013026 ; - _name.category_id pd_qpa_ext_std + _name.category_id pd_qpa_external_std _name.object_id k_factor _type.purpose Measurand _type.source Derived @@ -7577,32 +7666,32 @@ save_pd_qpa_ext_std.k_factor save_ -save_pd_qpa_ext_std.k_factor_su +save_pd_qpa_external_std.k_factor_su - _definition.id '_pd_qpa_ext_std.k_factor_su' + _definition.id '_pd_qpa_external_std.k_factor_su' _definition.update 2022-12-01 _description.text ; - Standard uncertainty of _pd_qpa_ext_std.k_factor. + Standard uncertainty of _pd_qpa_external_std.k_factor. ; - _name.category_id pd_qpa_ext_std + _name.category_id pd_qpa_external_std _name.object_id k_factor_su - _name.linked_item_id '_pd_qpa_ext_std.k_factor' + _name.linked_item_id '_pd_qpa_external_std.k_factor' _units.code none _import.get [{'file':templ_attr.cif 'save':general_su}] save_ -save_pd_qpa_ext_std.phase_id +save_pd_qpa_external_std.phase_id - _definition.id '_pd_qpa_ext_std.phase_id' + _definition.id '_pd_qpa_external_std.phase_id' _definition.update 2022-12-03 _description.text ; The phase (see _pd_phase.id) used as the external standard. ; - _name.category_id pd_qpa_ext_std + _name.category_id pd_qpa_external_std _name.object_id phase_id _name.linked_item_id '_pd_phase.id' _type.purpose Link @@ -7612,9 +7701,9 @@ save_pd_qpa_ext_std.phase_id save_ -save_pd_qpa_ext_std.phase_name +save_pd_qpa_external_std.phase_name - _definition.id '_pd_qpa_ext_std.phase_name' + _definition.id '_pd_qpa_external_std.phase_name' _definition.update 2023-01-07 _description.text ; @@ -7622,7 +7711,7 @@ save_pd_qpa_ext_std.phase_name quantitative phase analysis. This should match the value given in _pd_phase.name in the data block containing the calibration diffractogram. ; - _name.category_id pd_qpa_ext_std + _name.category_id pd_qpa_external_std _name.object_id phase_name _type.purpose Describe _type.source Assigned @@ -7631,16 +7720,16 @@ save_pd_qpa_ext_std.phase_name save_ -save_pd_qpa_ext_std.special_details +save_pd_qpa_external_std.special_details - _definition.id '_pd_qpa_ext_std.special_details' + _definition.id '_pd_qpa_external_std.special_details' _definition.update 2023-01-03 _description.text ; Description of external standard details that cannot otherwise be recorded using other PD_QPA_EXT_STD data items ; - _name.category_id pd_qpa_ext_std + _name.category_id pd_qpa_external_std _name.object_id special_details _type.purpose Describe _type.source Recorded @@ -7649,36 +7738,48 @@ save_pd_qpa_ext_std.special_details save_ -save_PD_QPA_INT_STD +save_PD_QPA_INTERNAL_STD - _definition.id PD_QPA_INT_STD + _definition.id PD_QPA_INTERNAL_STD _definition.scope Category _definition.class Set - _definition.update 2023-01-06 + _definition.update 2023-01-16 _description.text ; This category identifies the internal standard used for quantitative phase analysis. - Quantification by internal standard is typically carried out - using the Hill and Howard algorithm in conjunction with whole- - pattern Rietveld modelling, with the results being scaled to - match the included internal standard. The use of an internal - standard allows for the calculation of absolute mass fractions, - giving an indication of amorphous content. + Quantification by internal standard can be carried out by a variety + of different methods, including the Reference Intensity Ratio or the + Hill & Howard algorithm in conjunction with whole-pattern Rietveld + modelling. + + In general, the use of an internal standard converts relative phase + mass percentages into absolute mass percentage, allowing determination + of the 'unknown' (or 'amorphous', 'noncrystalline', or 'unanalysed') + fraction of the specimen. + + This can be done as + + W~p~^abs.^ = W~p~^rel.^ * (W~s~^known^ / 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. For a review on quantitative phase analysis, see Chapter 3.9 of International Tables, Vol. H, and references therein. ; _name.category_id PD_GROUP - _name.object_id PD_QPA_INT_STD + _name.object_id PD_QPA_INTERNAL_STD save_ -save_pd_qpa_int_std.block_id +save_pd_qpa_internal_std.block_id - _definition.id '_pd_qpa_int_std.block_id' - _definition.update 2023-01-09 + _definition.id '_pd_qpa_internal_std.block_id' + _definition.update 2023-01-16 _description.text ; Identifies the _pd_block.id of the phase used as an internal @@ -7687,9 +7788,9 @@ save_pd_qpa_int_std.block_id The data block containing the crystallographic information for this phase will be identified with a _pd_block.id code matching the - code in _pd_qpa_int_std.block_id + code in _pd_qpa_internal_std.block_id ; - _name.category_id pd_qpa_int_std + _name.category_id pd_qpa_internal_std _name.object_id block_id _name.linked_item_id '_pd_block.id' _type.purpose Link @@ -7699,24 +7800,23 @@ save_pd_qpa_int_std.block_id save_ -save_pd_qpa_int_std.mass_percent +save_pd_qpa_internal_std.mass_percent - _definition.id '_pd_qpa_int_std.mass_percent' + _definition.id '_pd_qpa_internal_std.mass_percent' _alias.definition_id '_pd_calib_std_internal_mass_%' - _definition.update 2023-01-03 + _definition.update 2023-01-16 _description.text ; - Per cent presence of the internal standard specified by the - data item _pd_calib.std_internal_name expressed as 100 times - the mass of standard added divided by the sum of the mass of - standard added and the original sample mass. + Per cent presence of the internal standard specified by the data item + _pd_qpa_internal_std.phase_name expressed as 100 times the mass of + standard added divided by the sum of the mass of standard added and the + original sample mass. - This value does not take into account the crystallinity of the - internal standard. That is, if 1 g of a 90% crystalline internal - standard is added to 3 g of sample, the - _pd_calib.std_internal_mass_percent is 25%. + This value does not take into account the crystallinity of the internal + standard. That is, if 1 g of a 90% crystalline internal standard is added + to 3 g of sample, the _pd_qpa_internal_std.mass_percent is 25%. ; - _name.category_id pd_qpa_int_std + _name.category_id pd_qpa_internal_std _name.object_id mass_percent _type.purpose Measurand _type.source Derived @@ -7726,32 +7826,32 @@ save_pd_qpa_int_std.mass_percent save_ -save_pd_qpa_int_std.mass_percent_su +save_pd_qpa_internal_std.mass_percent_su - _definition.id '_pd_qpa_int_std.mass_percent_su' - _definition.update 2023-01-03 + _definition.id '_pd_qpa_internal_std.mass_percent_su' + _definition.update 2023-01-16 _description.text ; - Standard uncertainty of _pd_qpa_int_std.mass_percent. + Standard uncertainty of _pd_qpa_internal_std.mass_percent. ; - _name.category_id pd_qpa_int_std + _name.category_id pd_qpa_internal_std _name.object_id mass_percent_su - _name.linked_item_id '_pd_qpa_int_std.mass_percent' + _name.linked_item_id '_pd_qpa_internal_std.mass_percent' _units.code none _import.get [{'file':templ_attr.cif 'save':general_su}] save_ -save_pd_qpa_int_std.phase_id +save_pd_qpa_internal_std.phase_id - _definition.id '_pd_qpa_int_std.phase_id' - _definition.update 2022-12-03 + _definition.id '_pd_qpa_internal_std.phase_id' + _definition.update 2023-01-16 _description.text ; The phase (see _pd_phase.id) used as the internal standard. ; - _name.category_id pd_qpa_int_std + _name.category_id pd_qpa_internal_std _name.object_id phase_id _name.linked_item_id '_pd_phase.id' _type.purpose Link @@ -7761,17 +7861,17 @@ save_pd_qpa_int_std.phase_id save_ -save_pd_qpa_int_std.phase_name +save_pd_qpa_internal_std.phase_name - _definition.id '_pd_qpa_int_std.phase_name' - _definition.update 2023-01-07 + _definition.id '_pd_qpa_internal_std.phase_name' + _definition.update 2023-01-16 _description.text ; Identifies the name of the material used as an internal standard for quantitative phase analysis. This should match the value given in _pd_phase.name in the data block containing the calibration diffractogram. ; - _name.category_id pd_qpa_int_std + _name.category_id pd_qpa_internal_std _name.object_id phase_name _type.purpose Describe _type.source Assigned @@ -7780,16 +7880,16 @@ save_pd_qpa_int_std.phase_name save_ -save_pd_qpa_int_std.special_details +save_pd_qpa_internal_std.special_details - _definition.id '_pd_qpa_int_std.special_details' - _definition.update 2023-01-03 + _definition.id '_pd_qpa_internal_std.special_details' + _definition.update 2023-01-16 _description.text ; Description of internal standard details that cannot otherwise - be recorded using other PD_QPA_INT_STD data items + be recorded using other PD_QPA_INTERNAL_STD data items ; - _name.category_id pd_qpa_int_std + _name.category_id pd_qpa_internal_std _name.object_id special_details _type.purpose Describe _type.source Recorded @@ -7798,62 +7898,55 @@ save_pd_qpa_int_std.special_details save_ -save_PD_QPA_RIR +save_PD_QPA_OVERALL - _definition.id PD_QPA_RIR + _definition.id PD_QPA_OVERALL _definition.scope Category _definition.class Set - _definition.update 2023-01-06 + _definition.update 2023-01-16 _description.text ; - This category identifies the reference intensity ratio used for - quantitative phase analysis. - - The reference intensity ratio (RIR) is an instrument-independent phase - constant developed for use in quantitative phase analysis and is - defined as the ratio of the most intense peak of phase, p, to the - most intense peak of a reference material, s. - - The generally accepted reference material is corundum due to its - relatively simple diffraction pattern, stability, and availability - as a highly crystalline and pure single phase. Additionally, the - unknown and reference materials are generally accepted to be mixed - in a 50:50 mass ratio. If corundum is used, the RIR equates to I/Ic - (or 'I over I corundum') for the phase; these are the most commonly - reported values in the literature. - - When applied in conjunction with the matrix-flushing method, quantitative - phase analysis is able to be undertaken without the presence of a - reference material. In this case, the sum of the mass fractions is - normalised to 100%. + This category gives the overall information about the quantitative phase + analysis methodology applied to a given diffractogram. +; + _name.category_id PD_GROUP + _name.object_id PD_QPA_CALIB_FACTOR + _category_key.name '_pd_qpa_overall.diffractogram_id' - The weight fraction of phase p, W_p, is given by +save_ - W_p = [I_p / (RIR_p * I_p,rel)] / Sum_k[I_k / (RIR_k * I_k,rel)] +save_pd_qpa_overall.diffractogram_id - where I_p is the intensity of the analyte peak of phase p, I_P,rel - is the ratio between the analyte peak and the most intense peak for - phase p, and RIR_p is the reference intensity ratio for phase p. - The sum is taken over all phases present in the specimen. + _definition.id '_pd_qpa_overall.diffractogram_id' + _definition.update 2023-01-16 + _description.text +; + A diffractogram ID code (see _pd_diffractogram.id) identifying the + diffractogram to which the quantitative phase analysis information relates. - For a review on quantitative phase analysis, see Chapter 3.9 of - International Tables, Vol. H, and references therein. + The diffractogram will be identified by a _pd_diffractogram.id code matching + the code in _pd_qpa_overall.diffractogram_id. ; - _name.category_id PD_GROUP - _name.object_id PD_QPA_RIR + _name.category_id pd_qpa_overall + _name.object_id diffractogram_id + _name.linked_item_id '_pd_diffractogram.id' + _type.purpose Link + _type.source Related + _type.container Single + _type.contents Word save_ -save_pd_qpa_rir.special_details +save_pd_qpa_overall.special_details - _definition.id '_pd_qpa_rir.special_details' - _definition.update 2023-01-03 + _definition.id '_pd_qpa_overall.special_details' + _definition.update 2023-01-16 _description.text ; - Description of RIR details that cannot otherwise - be recorded using other PD_QPA_RIR data items. + Description of overall QPA details that require additional detail, + or cannot otherwise be recorded using other PD_QPA_OVERALL data items. ; - _name.category_id pd_qpa_rir + _name.category_id pd_qpa_overall _name.object_id special_details _type.purpose Describe _type.source Recorded @@ -7862,101 +7955,213 @@ save_pd_qpa_rir.special_details save_ -save_pd_qpa_rir.std_block_id +save_pd_qpa_overall.method - _definition.id '_pd_qpa_rir.std_block_id' - _definition.update 2023-01-09 + _definition.id '_pd_qpa_overall.method' + _definition.update 2023-01-16 _description.text ; - Identifies the _pd_block.id of the diffractogram used to determine - the reference intensity ratio. + The type of quantification method applied to the given diffractogram. - Further references to additional phases present are given in - that data block. + This data item allows the origin of the values of _pd_phase_mass.percent + to be determined. Additionally, it allows for the proper interpretation + 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 + + For a review on quantitative phase analysis, see Chapter 3.9 of + International Tables, Vol. H, and references therein. ; - _name.category_id pd_qpa_rir - _name.object_id std_block_id - _name.linked_item_id '_pd_block.id' - _type.purpose Link - _type.source Assigned + _name.category_id pd_qpa_overall + _name.object_id method + _type.purpose State + _type.source Recorded _type.container Single - _type.contents Text + _type.contents Code -save_ + loop_ + _enumeration_set.state + _enumeration_set.detail + RIR +; + For an RIR value made with reference to corundum, see the state + 'I/Ic'. -save_pd_qpa_rir.std_phase_id + Quantitative phase analysis was undertaken following the Reference + Intensity Ratio methodology [1-3]. - _definition.id '_pd_qpa_rir.std_phase_id' - _definition.update 2022-12-03 - _description.text + _pd_qpa_calib_factor.value should be defined for each phase. Its value + corresponds to the value C~p~, below. + + The method of determining the RIR value, and the particular standard + against which it was calculated should be given in the + _pd_qpa_calib_factor.special_details for each phase. + + The relative weight fraction of phase p, W_p, is given by + + W~p~ = [(I~p~/I~p,rel~) / C~p~] / Sum[(I~k~/I~k,rel~) / C~k~, k=1:P] + + where I~p~ is the intensity of the analyte peak of phase p, I~P,rel~ + is the ratio between the analyte peak and the most intense peak for + phase p, and C~p~ is the reference intensity ratio for phase p. + The sum is taken over all phases present in the specimen. + + [1] Hubbard, C. R., Evans, E. H. & Smith, D. K. (1976). J. Appl. + Crystallogr. 9, 169-174. + + [2] Hubbard, C. R. & Snyder, R. L. (1988). Powder Diffr. 3, 74-77. + + [3] Snyder, R. L. & Bish, D. L. (1989). In Modern Powder Diffraction, + edited by D. L. Bish & J. E. Post, pp. 101-142. Washington DC: + Mineralogical Society of America. ; - The phase (see _pd_phase.id) used as the internal standard in - the determination of the reference intensity ratio. + I/Ic ; - _name.category_id pd_qpa_rir - _name.object_id phase_id - _name.linked_item_id '_pd_phase.id' - _type.purpose Link - _type.source Related - _type.container Single - _type.contents Text + A Reference Intensity Ratio in the specific case where the RIR value + was determined using corundum (\a-alumina) as the standard, and the + mass ratio of the standard and analyte phases was 50:50. +; + DDM +; + Quantitative phase analysis was undertaken following the Direct + Derivation Method [1-6]. -save_ + _pd_qpa_calib_factor.value should be defined for each phase. Its value + corresponds to the value C~p~, below. -save_pd_qpa_rir.value + The relative weight fraction of phase p, W_p, is given by - _definition.id '_pd_qpa_rir.value' - _definition.update 2023-01-03 - _description.text + W~p~ = (I~p~ / C~p~) / Sum(I~k~ / C~k~, k=1:P) + + where I~p~ is the integrated, Lp-normalised intensity of the analyte + phase over the entire diffractogram. The sum is taken over all phases + present. C~p~ is given by + + C~p~ = (1/M~p~) * Sum(n~i,p~^2^, i=1:N~p~) + + where M~p~ is the chemical formula weight of phase p, n~i,p~ is the + number of electrons belonging to the i^th^ atom of phase p, and N~p~ is + the number of atoms in the formula unit of phase p. + + [1] Toraya, H. (2016). J. Appl. Crystallogr. 49, 1508-1516. + [2] Toraya, H. (2017). J. Appl. Crystallogr. 50, 820-829. + [3] Toraya, H. (2017). J. Appl. Crystallogr. 50, 665-665. + [4] Toraya, H. (2018). J. Appl. Crystallogr. 51, 446-455. + [5] Toraya, H. (2019). J. Appl. Crystallogr. 52, 520-531. + [6] Toraya, H. & Omote, K. (2019). J. Appl. Crystallogr. 52, 13-22. ; - The value of the reference intensity ratio to be used in - quantitative phase analysis, as described by Hubbard et al., 1976, - Hubbard & Snyder, 1988, and Snyder & Bish, 1989. + ZMV +; + Quantitative phase analysis was undertaken following the ZMV + algorithm [1] in conjunction with Rietveld [2] refinements. + + _pd_qpa_calib_factor.value can be defined, if desired, for each phase, + but can be otherwise be calculated from the phases' crystal structure + details. Its value corresponds to the value C~p~, below. - The weight fraction of phase p, W_p is given by + The relative weight fraction of phase p, W~p~, is given by - W_p = [I_p / (RIR_p * I_p,rel)] / Sum_k[I_k / (RIR_k * I_k,rel)] + W~p~ = (S~p~ / C~p~) / Sum(S~k~ / C~k~, k=1:P) - where I_p is the intensity of the analyte peak of phase p, I_P,rel - is the ratio between the analyte peak and the most intense peak for - phase p, and RIR_p is the reference intensity ratio for phase p. - The sum is taken over all phases present in the specimen. + where S~p~ is the Rietveld scale factor of the analyte phase. The sum + is taken over all phases present, and - Hubbard, C. R., Evans, E. H. & Smith, D. K. (1976). The reference - intensity ratio, I/Ic, for computer simulated powder patterns. J. Appl. - Cryst. 9, 169-174. + C~p~ = 1/(Z * M * V)~p~ - Hubbard, C. R. & Snyder, R. L. (1988). RIR - measurement and use in - quantitative XRD. Powder Diffr. 3, 74-77. + where 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, all of phase p. - Snyder, R. L. & Bish, D. L. (1989). In Modern Powder Diffraction, edited - by D. L. Bish & J. E. Post, pp. 101-142. Washington DC: Mineralogical - Society of America. + [1] Hill,R.J. & Howard, C.J. (1987). J. Appl. Crystallogr. 20, 467-474. + [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. ; - _name.category_id pd_qpa_rir - _name.object_id value - _type.purpose Measurand - _type.source Derived - _type.container Single - _type.contents Real - _units.code none + PONKCS +; + Quantitative phase analysis was undertaken following the Partial Or No + Known Crystal Structure methodology [1]. -save_ + _pd_qpa_calib_factor.value should be defined for each phase. Its value + corresponds to the value C~p~, below. -save_pd_qpa_rir.value_su + The relative weight fraction of phase p, W~p~, is given by - _definition.id '_pd_qpa_rir.value_su' - _definition.update 2023-01-03 - _description.text + W~p~ = (S~p~ / C~p~) / Sum(S~k~ / C~k~, k=1:P) + + where S~p~ is the Rietveld scale factor of the analyte phase. The sum + is taken over all phases present, and + + C~p~ = (W~s~/W~p~) * (S~p~/S~s~) * (1/(ZMV)~s~) + + where W is the weight fraction, 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. The subscript p + denotes the analyte phase, and s denotes the standard phase. + + Once a particular phase has been calibrated, it's value of C~p~ is + consistent with ZMV valuesand can be used in conjunction with the ZMV + algorithm with normal, crystalline phases to quantify relative phase + fractions in mixtures containing this phase. + + If any phase in an analysis of a diffractogram uses the PONKCS + approach, the entire quantification is to be marked as 'PONKCS', and + all phases should define _pd_qpa_calib_factor.value. + + [1] Scarlett, N.V.Y. & Madsen, I.C. (2006). Powder Diffr. 21, 278-284. ; - Standard uncertainty of _pd_qpa_rir.value. + absorption_diffraction ; - _name.category_id pd_qpa_rir - _name.object_id value_su - _name.linked_item_id '_pd_qpa_rir.value' - _units.code none + Quantitative phase analysis was undertaken following the + absorption-diffraction methodology methodology [1]. - _import.get [{'file':templ_attr.cif 'save':general_su}] + _pd_qpa_calib_factor.value should be defined for each phase. Its value + corresponds to the value C~p~, below. In addition, + _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs + must be given for the specimen in each diffractogram. + + The absolute weight fraction of phase p, W_p, is given by + + W~p~ = [I~p~ / C~p~] * \mu^*^~m~ + + where I~p~ is the intensity of the analyte peak, \mu^*^~m~ is the mass + absorption coefficient of the entire specimen, and C~p~ is a previously + determined calibration constant. + + [1] Klug, H.P. & Alexander, L.E. (1974). X-Ray Diffraction Procedures: + For Polycrystalline and Amorphous Materials. New York: Wiley. +; + external_standard +; + Quantitative phase analysis was undertaken following the external + standard methodology [1] to quantify absolute phase fractions taken + from Rietveld [2] refinements. + + _pd_qpa_calib_factor.value can be defined for each phase, but data + items from the PD_QPA_EXTERNAL_STANDARD category should preferentially + used. In addition, _pd_char.mass_atten_coef_mu_calc or + _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each + diffractogram. + + The absolute weight fraction of phase p, W~p~, is given by + + W~p~ = [S~p~ / C~p~] * \mu^*^~m~ + + where S~p~ is the Rietveld scale factor of the analyte phase, and + \mu^*^~m~ is the mass absorption coefficient of the entire specimen. + C~p~ is given as + + C~p~ = K /(Z * M * V)~p~ + + where 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, all of phase p, + and K is the previously determined diffractometer constant. + + [1] O'Connor, B. H. & Raven, M. D. (1988). Powder Diffr. 3, 2-6. + [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. +; + other +; + Please give details in _pd_qpa_overall.special_details. +; save_ @@ -8427,7 +8632,7 @@ save_ Deprecated _pd_refln.wavelength_id after consultation with PDDMG. ; - 2.5.0 2023-01-10 + 2.5.0 2023-01-16 ; ## Retain above version number and increment date until final ## release @@ -8467,17 +8672,15 @@ save_ Made PD_PHASE a Set category. - Created PD_QPA_EXT_STD and PD_QPA_INT_STD to record quantitative - phase analysis by the external and internal standard approaches. - - Created PD_QPA_RIR to record quantitative phase analysis by - the reference intensity ratio approach. + Created PD_QPA_EXTERNAL_STD and PD_QPA_INTERNAL_STD to record + quantitative phase analysis by the external and internal standard + approaches. Changed _pd_meas.step_count_time and _pd_meas.time_of_flight from Integer to Real. - Update definitions of _pd_phase.name, _pd_qpa_ext_std.phase_name, and - _pd_qpa_int_std.phase_name to better represent their contents. + Update definitions of _pd_phase.name, _pd_qpa_external_std.phase_name, + and _pd_qpa_internal_std.phase_name to better represent their contents. Created PD_AMORPHOUS. @@ -8489,4 +8692,7 @@ save_ Updated data items to hold block ID values to be of type Link, and to link them formally to _pd_block.id + + Created PD_QPA_OVERALL to record details about the overall quantitative + phase analysis method. ; From 6d6766626e9d380a3255a7777ae4b50f75db7f4c Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Mon, 16 Jan 2023 22:40:09 +0800 Subject: [PATCH 02/24] force checks to run --- cif_pow.dic | 1 - 1 file changed, 1 deletion(-) diff --git a/cif_pow.dic b/cif_pow.dic index fb5c541..489d87f 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7897,7 +7897,6 @@ save_pd_qpa_internal_std.special_details _type.contents Text save_ - save_PD_QPA_OVERALL _definition.id PD_QPA_OVERALL From a1634f603e4b5f757278194565979e3abfe78a73 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Mon, 16 Jan 2023 22:40:52 +0800 Subject: [PATCH 03/24] Revert "force checks to run" This reverts commit 6d6766626e9d380a3255a7777ae4b50f75db7f4c. --- cif_pow.dic | 1 + 1 file changed, 1 insertion(+) diff --git a/cif_pow.dic b/cif_pow.dic index 489d87f..fb5c541 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7897,6 +7897,7 @@ save_pd_qpa_internal_std.special_details _type.contents Text save_ + save_PD_QPA_OVERALL _definition.id PD_QPA_OVERALL From 39b227f8571538a6c601c6492affe145dc15fefa Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Mon, 16 Jan 2023 22:44:56 +0800 Subject: [PATCH 04/24] Fix alphabetical order and incorrect type contents --- cif_pow.dic | 36 ++++++++++++++++++------------------ 1 file changed, 18 insertions(+), 18 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index fb5c541..661ff9a 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7933,24 +7933,6 @@ save_pd_qpa_overall.diffractogram_id _type.purpose Link _type.source Related _type.container Single - _type.contents Word - -save_ - -save_pd_qpa_overall.special_details - - _definition.id '_pd_qpa_overall.special_details' - _definition.update 2023-01-16 - _description.text -; - Description of overall QPA details that require additional detail, - or cannot otherwise be recorded using other PD_QPA_OVERALL data items. -; - _name.category_id pd_qpa_overall - _name.object_id special_details - _type.purpose Describe - _type.source Recorded - _type.container Single _type.contents Text save_ @@ -8165,6 +8147,24 @@ save_pd_qpa_overall.method save_ +save_pd_qpa_overall.special_details + + _definition.id '_pd_qpa_overall.special_details' + _definition.update 2023-01-16 + _description.text +; + Description of overall QPA details that require additional detail, + or cannot otherwise be recorded using other PD_QPA_OVERALL data items. +; + _name.category_id pd_qpa_overall + _name.object_id special_details + _type.purpose Describe + _type.source Recorded + _type.container Single + _type.contents Text + +save_ + save_PD_SPEC _definition.id PD_SPEC From fe96c637aa58bf615f08256c59229f3e443fa76e Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Wed, 18 Jan 2023 20:52:00 +0800 Subject: [PATCH 05/24] remove _*.phase_name data items where the name can be found via _*.phase_id links --- cif_pow.dic | 46 +++------------------------------------------- 1 file changed, 3 insertions(+), 43 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 661ff9a..b273dd6 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7701,25 +7701,6 @@ save_pd_qpa_external_std.phase_id save_ -save_pd_qpa_external_std.phase_name - - _definition.id '_pd_qpa_external_std.phase_name' - _definition.update 2023-01-07 - _description.text -; - Identifies the name of the material used as an external standard for - quantitative phase analysis. This should match the value given in - _pd_phase.name in the data block containing the calibration diffractogram. -; - _name.category_id pd_qpa_external_std - _name.object_id phase_name - _type.purpose Describe - _type.source Assigned - _type.container Single - _type.contents Text - -save_ - save_pd_qpa_external_std.special_details _definition.id '_pd_qpa_external_std.special_details' @@ -7807,9 +7788,8 @@ save_pd_qpa_internal_std.mass_percent _definition.update 2023-01-16 _description.text ; - Per cent presence of the internal standard specified by the data item - _pd_qpa_internal_std.phase_name expressed as 100 times the mass of - standard added divided by the sum of the mass of standard added and the + Per cent presence of the internal standard expressed as 100 times the mass + of standard added divided by the sum of the mass of standard added and the original sample mass. This value does not take into account the crystallinity of the internal @@ -7861,25 +7841,6 @@ save_pd_qpa_internal_std.phase_id save_ -save_pd_qpa_internal_std.phase_name - - _definition.id '_pd_qpa_internal_std.phase_name' - _definition.update 2023-01-16 - _description.text -; - Identifies the name of the material used as an internal standard for - quantitative phase analysis. This should match the value given in - _pd_phase.name in the data block containing the calibration diffractogram. -; - _name.category_id pd_qpa_internal_std - _name.object_id phase_name - _type.purpose Describe - _type.source Assigned - _type.container Single - _type.contents Text - -save_ - save_pd_qpa_internal_std.special_details _definition.id '_pd_qpa_internal_std.special_details' @@ -8679,8 +8640,7 @@ save_ Changed _pd_meas.step_count_time and _pd_meas.time_of_flight from Integer to Real. - Update definitions of _pd_phase.name, _pd_qpa_external_std.phase_name, - and _pd_qpa_internal_std.phase_name to better represent their contents. + Update definitions of _pd_phase.name to better represent their contents. Created PD_AMORPHOUS. From b90d74d8cbc2af35d42e0d9c734c542bf8bb021b Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Sun, 22 Jan 2023 14:44:44 +0800 Subject: [PATCH 06/24] reorder `_pd_qpa_overall.method` enumeration to be alphabetical but with 'other' still at the end --- cif_pow.dic | 165 ++++++++++++++++++++++++++-------------------------- 1 file changed, 82 insertions(+), 83 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 40a5087..49650e1 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -14,7 +14,7 @@ data_CIF_POW _dictionary.title CIF_POW _dictionary.class Instance _dictionary.version 2.5.0 - _dictionary.date 2023-01-18 + _dictionary.date 2023-01-22 _dictionary.uri https://raw.githubusercontent.com/COMCIFS/Powder_Dictionary/master/cif_pow.dic _dictionary.ddl_conformance 3.11.10 @@ -7482,11 +7482,8 @@ save_PD_QPA_CALIB_FACTOR ; This category gives the value of the calibration constant by which the calculated intensity or scale factor associated with the given phase is - divided in order to allow quantitative phase analysis to be undertaken. + divided by in order to allow quantitative phase analysis to be undertaken. Further normalisation may be necessary, and can be indicated. - - For example, if quantification was undertaken using RIR values, those - values can be recorded with _pd_qpa_calib_factor.value ; _name.category_id PD_GROUP _name.object_id PD_QPA_CALIB_FACTOR @@ -7907,7 +7904,7 @@ save_ save_pd_qpa_overall.method _definition.id '_pd_qpa_overall.method' - _definition.update 2023-01-16 + _definition.update 2023-01-22 _description.text ; The type of quantification method applied to the given diffractogram. @@ -7932,44 +7929,26 @@ save_pd_qpa_overall.method loop_ _enumeration_set.state _enumeration_set.detail - RIR + absorption_diffraction ; - For an RIR value made with reference to corundum, see the state - 'I/Ic'. - - Quantitative phase analysis was undertaken following the Reference - Intensity Ratio methodology [1-3]. + Quantitative phase analysis was undertaken following the + absorption-diffraction methodology methodology [1]. _pd_qpa_calib_factor.value should be defined for each phase. Its value - corresponds to the value C~p~, below. - - The method of determining the RIR value, and the particular standard - against which it was calculated should be given in the - _pd_qpa_calib_factor.special_details for each phase. - - The relative weight fraction of phase p, W_p, is given by - - W~p~ = [(I~p~/I~p,rel~) / C~p~] / Sum[(I~k~/I~k,rel~) / C~k~, k=1:P] + corresponds to the value C~p~, below. In addition, + _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs + must be given for the specimen in each diffractogram. - where I~p~ is the intensity of the analyte peak of phase p, I~P,rel~ - is the ratio between the analyte peak and the most intense peak for - phase p, and C~p~ is the reference intensity ratio for phase p. - The sum is taken over all phases present in the specimen. + The absolute weight fraction of phase p, W_p, is given by - [1] Hubbard, C. R., Evans, E. H. & Smith, D. K. (1976). J. Appl. - Crystallogr. 9, 169-174. + W~p~ = [I~p~ / C~p~] * \mu^*^~m~ - [2] Hubbard, C. R. & Snyder, R. L. (1988). Powder Diffr. 3, 74-77. + where I~p~ is the intensity of the analyte peak, \mu^*^~m~ is the mass + absorption coefficient of the entire specimen, and C~p~ is a previously + determined calibration constant. - [3] Snyder, R. L. & Bish, D. L. (1989). In Modern Powder Diffraction, - edited by D. L. Bish & J. E. Post, pp. 101-142. Washington DC: - Mineralogical Society of America. -; - I/Ic -; - A Reference Intensity Ratio in the specific case where the RIR value - was determined using corundum (\a-alumina) as the standard, and the - mass ratio of the standard and analyte phases was 50:50. + [1] Klug, H.P. & Alexander, L.E. (1974). X-Ray Diffraction Procedures: + For Polycrystalline and Amorphous Materials. New York: Wiley. ; DDM ; @@ -8000,29 +7979,42 @@ save_pd_qpa_overall.method [5] Toraya, H. (2019). J. Appl. Crystallogr. 52, 520-531. [6] Toraya, H. & Omote, K. (2019). J. Appl. Crystallogr. 52, 13-22. ; - ZMV + external_standard ; - Quantitative phase analysis was undertaken following the ZMV - algorithm [1] in conjunction with Rietveld [2] refinements. + Quantitative phase analysis was undertaken following the external + standard methodology [1] to quantify absolute phase fractions taken + from Rietveld [2] refinements. - _pd_qpa_calib_factor.value can be defined, if desired, for each phase, - but can be otherwise be calculated from the phases' crystal structure - details. Its value corresponds to the value C~p~, below. + _pd_qpa_calib_factor.value can be defined for each phase, but data + items from the PD_QPA_EXTERNAL_STANDARD category should preferentially + used. In addition, _pd_char.mass_atten_coef_mu_calc or + _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each + diffractogram. - The relative weight fraction of phase p, W~p~, is given by + The absolute weight fraction of phase p, W~p~, is given by - W~p~ = (S~p~ / C~p~) / Sum(S~k~ / C~k~, k=1:P) + W~p~ = [S~p~ / C~p~] * \mu^*^~m~ - where S~p~ is the Rietveld scale factor of the analyte phase. The sum - is taken over all phases present, and + where S~p~ is the Rietveld scale factor of the analyte phase, and + \mu^*^~m~ is the mass absorption coefficient of the entire specimen. + C~p~ is given as - C~p~ = 1/(Z * M * V)~p~ + C~p~ = K /(Z * M * V)~p~ where 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, all of phase p. + formula weight, and V is the volume of the unit cell, all of phase p, + and K is the previously determined diffractometer constant. - [1] Hill,R.J. & Howard, C.J. (1987). J. Appl. Crystallogr. 20, 467-474. + [1] O'Connor, B. H. & Raven, M. D. (1988). Powder Diffr. 3, 2-6. [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. +; + I/Ic +; + A Reference Intensity Ratio (RIR) in the specific case where the RIR + value was determined using corundum (\a-alumina) as the standard, and + the mass ratio of the standard and analyte phases was 50:50. + + For a description of the RIR methodology, see the entry for the 'RIR'. ; PONKCS ; @@ -8047,7 +8039,7 @@ save_pd_qpa_overall.method denotes the analyte phase, and s denotes the standard phase. Once a particular phase has been calibrated, it's value of C~p~ is - consistent with ZMV valuesand can be used in conjunction with the ZMV + consistent with ZMV values and can be used in conjunction with the ZMV algorithm with normal, crystalline phases to quantify relative phase fractions in mixtures containing this phase. @@ -8057,54 +8049,61 @@ save_pd_qpa_overall.method [1] Scarlett, N.V.Y. & Madsen, I.C. (2006). Powder Diffr. 21, 278-284. ; - absorption_diffraction + RIR ; - Quantitative phase analysis was undertaken following the - absorption-diffraction methodology methodology [1]. + For an RIR value made with reference to corundum, see the state + 'I/Ic'. + + Quantitative phase analysis was undertaken following the Reference + Intensity Ratio methodology [1-3]. _pd_qpa_calib_factor.value should be defined for each phase. Its value - corresponds to the value C~p~, below. In addition, - _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs - must be given for the specimen in each diffractogram. + corresponds to the value C~p~, below. - The absolute weight fraction of phase p, W_p, is given by + The method of determining the RIR value, and the particular standard + against which it was calculated should be given in the + _pd_qpa_calib_factor.special_details for each phase. - W~p~ = [I~p~ / C~p~] * \mu^*^~m~ + The relative weight fraction of phase p, W_p, is given by - where I~p~ is the intensity of the analyte peak, \mu^*^~m~ is the mass - absorption coefficient of the entire specimen, and C~p~ is a previously - determined calibration constant. + W~p~ = [(I~p~/I~p,rel~) / C~p~] / Sum[(I~k~/I~k,rel~) / C~k~, k=1:P] - [1] Klug, H.P. & Alexander, L.E. (1974). X-Ray Diffraction Procedures: - For Polycrystalline and Amorphous Materials. New York: Wiley. + where I~p~ is the intensity of the analyte peak of phase p, I~P,rel~ + is the ratio between the analyte peak and the most intense peak for + phase p, and C~p~ is the reference intensity ratio for phase p. + The sum is taken over all phases present in the specimen. + + [1] Hubbard, C. R., Evans, E. H. & Smith, D. K. (1976). J. Appl. + Crystallogr. 9, 169-174. + + [2] Hubbard, C. R. & Snyder, R. L. (1988). Powder Diffr. 3, 74-77. + + [3] Snyder, R. L. & Bish, D. L. (1989). In Modern Powder Diffraction, + edited by D. L. Bish & J. E. Post, pp. 101-142. Washington DC: + Mineralogical Society of America. ; - external_standard + ZMV ; - Quantitative phase analysis was undertaken following the external - standard methodology [1] to quantify absolute phase fractions taken - from Rietveld [2] refinements. + Quantitative phase analysis was undertaken following the ZMV + algorithm [1] in conjunction with Rietveld [2] refinements. - _pd_qpa_calib_factor.value can be defined for each phase, but data - items from the PD_QPA_EXTERNAL_STANDARD category should preferentially - used. In addition, _pd_char.mass_atten_coef_mu_calc or - _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each - diffractogram. + _pd_qpa_calib_factor.value can be defined, if desired, for each phase, + but can be otherwise be calculated from the phases' crystal structure + details. Its value corresponds to the value C~p~, below. - The absolute weight fraction of phase p, W~p~, is given by + The relative weight fraction of phase p, W~p~, is given by - W~p~ = [S~p~ / C~p~] * \mu^*^~m~ + W~p~ = (S~p~ / C~p~) / Sum(S~k~ / C~k~, k=1:P) - where S~p~ is the Rietveld scale factor of the analyte phase, and - \mu^*^~m~ is the mass absorption coefficient of the entire specimen. - C~p~ is given as + where S~p~ is the Rietveld scale factor of the analyte phase. The sum + is taken over all phases present, and - C~p~ = K /(Z * M * V)~p~ + C~p~ = 1/(Z * M * V)~p~ where 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, all of phase p, - and K is the previously determined diffractometer constant. + formula weight, and V is the volume of the unit cell, all of phase p. - [1] O'Connor, B. H. & Raven, M. D. (1988). Powder Diffr. 3, 2-6. + [1] Hill,R.J. & Howard, C.J. (1987). J. Appl. Crystallogr. 20, 467-474. [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. ; other @@ -8599,7 +8598,7 @@ save_ Deprecated _pd_refln.wavelength_id after consultation with PDDMG. ; - 2.5.0 2023-01-18 + 2.5.0 2023-01-22 ; ## Retain above version number and increment date until final ## release From 4019405011cce8a3a42e5d120e42bab1175e4f35 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Sun, 22 Jan 2023 15:06:07 +0800 Subject: [PATCH 07/24] add individual data items in PD_QPA_CALIB_FACTOR for each method of quantification --- cif_pow.dic | 294 ++++++++++++++++++++++++++++++++++++++++++++++++---- 1 file changed, 276 insertions(+), 18 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 49650e1..8c3ab5b 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7484,6 +7484,10 @@ save_PD_QPA_CALIB_FACTOR calculated intensity or scale factor associated with the given phase is divided by in order to allow quantitative phase analysis to be undertaken. Further normalisation may be necessary, and can be indicated. + + 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. ; _name.category_id PD_GROUP _name.object_id PD_QPA_CALIB_FACTOR @@ -7491,6 +7495,169 @@ save_PD_QPA_CALIB_FACTOR save_ +save_pd_qpa_calib_factor.absorption_diffraction + + _definition.id '_pd_qpa_calib_factor.absorption_diffraction' + _definition.update 2023-01-22 + _description.text +; + A absorption-diffraction calibration value associated with the given phase + which allows quantitative phase analysis to be undertaken. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. +; + _name.category_id pd_qpa_calib_factor + _name.object_id absorption_diffraction + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.absorption_diffraction_su + + _definition.id + '_pd_qpa_calib_factor.absorption_diffraction_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.absorption_diffraction. +; + _name.category_id pd_qpa_calib_factor + _name.object_id absorption_diffraction_su + _name.linked_item_id '_pd_qpa_calib_factor.absorption_diffraction' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + +save_pd_qpa_calib_factor.DDM + + _definition.id '_pd_qpa_calib_factor.DDM' + _definition.update 2023-01-22 + _description.text +; + A Direct-Derivation Methodology (DDM) calibration value associated with the + given phase which allows quantitative phase analysis to be undertaken. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. +; + _name.category_id pd_qpa_calib_factor + _name.object_id DDM + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.DDM_su + + _definition.id '_pd_qpa_calib_factor.DDM_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.DDM. +; + _name.category_id pd_qpa_calib_factor + _name.object_id DDM_su + _name.linked_item_id '_pd_qpa_calib_factor.DDM' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + +save_pd_qpa_calib_factor.external_standard + + _definition.id '_pd_qpa_calib_factor.external_standard' + _definition.update 2023-01-22 + _description.text +; + A external standard calibration value associated with the given phase which + allows quantitative phase analysis to be undertaken. + + If the external standard approach is used, the use of PD_EXTERNAL_STD data + items is preferred. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. +; + _name.category_id pd_qpa_calib_factor + _name.object_id external_standard + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.external_standard_su + + _definition.id '_pd_qpa_calib_factor.external_standard_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.external_standard. +; + _name.category_id pd_qpa_calib_factor + _name.object_id external_standard_su + _name.linked_item_id '_pd_qpa_calib_factor.external_standard' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + +save_pd_qpa_calib_factor.I_over_Ic + + _definition.id '_pd_qpa_calib_factor.I_over_Ic' + _definition.update 2023-01-22 + _description.text +; + A Reference Intensity Ratio (RIR) calibration value associated with the + given phase which allows quantitative phase analysis to be undertaken. + + This ratio must have been calculated with respect to corundum; for other + reference materials, please use _pd_qpa_calib_factor.RIR. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. +; + _name.category_id pd_qpa_calib_factor + _name.object_id I_over_Ic + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.I_over_Ic_su + + _definition.id '_pd_qpa_calib_factor.I_over_Ic_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.I_over_Ic. +; + _name.category_id pd_qpa_calib_factor + _name.object_id I_over_Ic_su + _name.linked_item_id '_pd_qpa_calib_factor.I_over_Ic' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + save_pd_qpa_calib_factor.phase_id _definition.id '_pd_qpa_calib_factor.phase_id' @@ -7509,6 +7676,94 @@ save_pd_qpa_calib_factor.phase_id save_ +save_pd_qpa_calib_factor.PONKCS + + _definition.id '_pd_qpa_calib_factor.PONKCS' + _definition.update 2023-01-22 + _description.text +; + A PONKCS calibration value associated with the given phase which allows + quantitative phase analysis to be undertaken. + + This value, when coupled with the peak intensities for which it was + calibrated, forms a pseudo-ZMV value, and can also be used in + quantification with the ZMV algorithm. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. +; + _name.category_id pd_qpa_calib_factor + _name.object_id PONKCS + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.PONKCS_su + + _definition.id '_pd_qpa_calib_factor.PONKCS_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.PONKCS. +; + _name.category_id pd_qpa_calib_factor + _name.object_id PONKCS_su + _name.linked_item_id '_pd_qpa_calib_factor.PONKCS' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + +save_pd_qpa_calib_factor.RIR + + _definition.id '_pd_qpa_calib_factor.RIR' + _definition.update 2023-01-22 + _description.text +; + A Reference Intensity Ratio (RIR) calibration value associated with the + given phase which allows quantitative phase analysis to be undertaken. + + This ratio must NOT have been calculated with respect to corundum; for RIR + values calculated with corundum, please use _pd_qpa_calib_factor.I_over_IC. + + Details of the reference material against which this RIR was determined + should be given in _pd_qpa_calib_factor.special_details. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. +; + _name.category_id pd_qpa_calib_factor + _name.object_id RIR + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.RIR_su + + _definition.id '_pd_qpa_calib_factor.RIR_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.RIR. +; + _name.category_id pd_qpa_calib_factor + _name.object_id RIR_su + _name.linked_item_id '_pd_qpa_calib_factor.RIR' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + save_pd_qpa_calib_factor.special_details _definition.id '_pd_qpa_calib_factor.special_details' @@ -7527,21 +7782,24 @@ save_pd_qpa_calib_factor.special_details save_ -save_pd_qpa_calib_factor.value +save_pd_qpa_calib_factor.ZMV - _definition.id '_pd_qpa_calib_factor.value' - _definition.update 2023-01-15 + _definition.id '_pd_qpa_calib_factor.ZMV' + _definition.update 2023-01-22 _description.text ; - A calibration value by which a calculated intensity or scale factor - associated with the given phase is divided by in the process of quantitative - phase analysis. + A ZMV calibration value associated with the given phase which allows + quantitative phase analysis to be undertaken. - The type of calibration factor, and hence the correction quantitative phase - analysis equation, is given in _pd_qpa_calib_factor.type. + If the ZMV value used in the quantification can be derived from the + structural information present with the phase, then this value + does not need to be given. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. ; _name.category_id pd_qpa_calib_factor - _name.object_id value + _name.object_id ZMV _type.purpose Measurand _type.source Derived _type.container Single @@ -7550,17 +7808,17 @@ save_pd_qpa_calib_factor.value save_ -save_pd_qpa_calib_factor.value_su +save_pd_qpa_calib_factor.ZMV_su - _definition.id '_pd_qpa_calib_factor.value_su' - _definition.update 2023-01-14 + _definition.id '_pd_qpa_calib_factor.ZMV_su' + _definition.update 2023-01-22 _description.text ; - Standard uncertainty of _pd_qpa_calib_factor.value. + Standard uncertainty of _pd_qpa_calib_factor.ZMV. ; _name.category_id pd_qpa_calib_factor - _name.object_id value_su - _name.linked_item_id '_pd_qpa_calib_factor.value' + _name.object_id ZMV_su + _name.linked_item_id '_pd_qpa_calib_factor.ZMV' _units.code none _import.get [{'file':templ_attr.cif 'save':general_su}] @@ -7872,6 +8130,9 @@ save_PD_QPA_OVERALL ; This category gives the overall information about the quantitative phase analysis methodology applied to a given diffractogram. + + For a review on quantitative phase analysis, see Chapter 3.9 of + International Tables, Vol. H, and references therein. ; _name.category_id PD_GROUP _name.object_id PD_QPA_CALIB_FACTOR @@ -7915,9 +8176,6 @@ save_pd_qpa_overall.method If 'other' is chosen, further information must be given in _pd_qpa_overall.special_details - - For a review on quantitative phase analysis, see Chapter 3.9 of - International Tables, Vol. H, and references therein. ; _name.category_id pd_qpa_overall _name.object_id method From c533ec95e65ee7f88d9ce468f4a8721f96e36d5d Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Sun, 22 Jan 2023 15:15:38 +0800 Subject: [PATCH 08/24] update description of _pd_qpa_overall.method enumerations --- cif_pow.dic | 41 +++++++++++++++++++++++------------------ 1 file changed, 23 insertions(+), 18 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 8c3ab5b..d2562f7 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8192,12 +8192,12 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the absorption-diffraction methodology methodology [1]. - _pd_qpa_calib_factor.value should be defined for each phase. Its value - corresponds to the value C~p~, below. In addition, + _pd_qpa_calib_factor.absorption_diffraction should be defined for each + phase, which corresponds to C~p~, below. In addition, _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each diffractogram. - The absolute weight fraction of phase p, W_p, is given by + The absolute weight fraction of phase p, W~p~, is given by W~p~ = [I~p~ / C~p~] * \mu^*^~m~ @@ -8213,10 +8213,10 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the Direct Derivation Method [1-6]. - _pd_qpa_calib_factor.value should be defined for each phase. Its value - corresponds to the value C~p~, below. + _pd_qpa_calib_factor.DDM should be defined for each phase, which + corresponds to C~p~, below. - The relative weight fraction of phase p, W_p, is given by + The relative weight fraction of phase p, W~p~, is given by W~p~ = (I~p~ / C~p~) / Sum(I~k~ / C~k~, k=1:P) @@ -8243,9 +8243,9 @@ save_pd_qpa_overall.method standard methodology [1] to quantify absolute phase fractions taken from Rietveld [2] refinements. - _pd_qpa_calib_factor.value can be defined for each phase, but data - items from the PD_QPA_EXTERNAL_STANDARD category should preferentially - used. In addition, _pd_char.mass_atten_coef_mu_calc or + _pd_qpa_calib_factor.external_standard can be defined for each phase, + but data items from the PD_QPA_EXTERNAL_STANDARD category should be + preferentially used. In addition, _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each diffractogram. @@ -8272,6 +8272,9 @@ save_pd_qpa_overall.method value was determined using corundum (\a-alumina) as the standard, and the mass ratio of the standard and analyte phases was 50:50. + _pd_qpa_calib_factor.I_over_Ic should be defined for each phase, which + corresponds to C~p~. + For a description of the RIR methodology, see the entry for the 'RIR'. ; PONKCS @@ -8279,7 +8282,7 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the Partial Or No Known Crystal Structure methodology [1]. - _pd_qpa_calib_factor.value should be defined for each phase. Its value + _pd_qpa_calib_factor.PONKCS should be defined for each phase. Its value corresponds to the value C~p~, below. The relative weight fraction of phase p, W~p~, is given by @@ -8296,10 +8299,12 @@ save_pd_qpa_overall.method formula weight, and V is the volume of the unit cell. The subscript p denotes the analyte phase, and s denotes the standard phase. - Once a particular phase has been calibrated, it's value of C~p~ is - consistent with ZMV values and can be used in conjunction with the ZMV - algorithm with normal, crystalline phases to quantify relative phase - fractions in mixtures containing this phase. + The intensities of the peaks assigned to the PONKCS phase, when taken + in combination with C~p~, act as pseudo-F_squared values. Because of + this, once a particular phase has been calibrated, it's value of C~p~ + is consistent with ZMV values and can be used in conjunction with the + ZMV algorithm with normal, crystalline phases to quantify relative + phase fractions in mixtures containing this phase. If any phase in an analysis of a diffractogram uses the PONKCS approach, the entire quantification is to be marked as 'PONKCS', and @@ -8315,14 +8320,14 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the Reference Intensity Ratio methodology [1-3]. - _pd_qpa_calib_factor.value should be defined for each phase. Its value + _pd_qpa_calib_factor.RIR should be defined for each phase. Its value corresponds to the value C~p~, below. The method of determining the RIR value, and the particular standard against which it was calculated should be given in the _pd_qpa_calib_factor.special_details for each phase. - The relative weight fraction of phase p, W_p, is given by + The relative weight fraction of phase p, W~p~, is given by W~p~ = [(I~p~/I~p,rel~) / C~p~] / Sum[(I~k~/I~k,rel~) / C~k~, k=1:P] @@ -8345,8 +8350,8 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the ZMV algorithm [1] in conjunction with Rietveld [2] refinements. - _pd_qpa_calib_factor.value can be defined, if desired, for each phase, - but can be otherwise be calculated from the phases' crystal structure + _pd_qpa_calib_factor.ZMV can be defined, if desired, for each phase, + but can be otherwise be calculated from the phase's crystal structure details. Its value corresponds to the value C~p~, below. The relative weight fraction of phase p, W~p~, is given by From cea31295ce057b492b6e6916f5309c15a3c31a28 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Sun, 22 Jan 2023 15:38:32 +0800 Subject: [PATCH 09/24] created PD_QPA_INTENSITY_FACTOR --- cif_pow.dic | 116 +++++++++++++++++++++++++++++++++++++++++++++++++++- 1 file changed, 115 insertions(+), 1 deletion(-) diff --git a/cif_pow.dic b/cif_pow.dic index d2562f7..ed94f15 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7980,6 +7980,118 @@ save_pd_qpa_external_std.special_details save_ +save_PD_QPA_INTENSITY_FACTOR + + _definition.id PD_QPA_INTENSITY_FACTOR + _definition.scope Category + _definition.class Loop + _definition.update 2023-01-22 + _description.text +; + This category gives the value of the intensity or scale factor which is + divided by the corresponding calibration factor in order to allow + 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. + + For a review on quantitative phase analysis, see Chapter 3.9 of + International Tables, Vol. H, and references therein. +; + _name.category_id PD_GROUP + _name.object_id PD_QPA_INTENSITY_FACTOR + + loop_ + _category_key.name + '_pd_qpa_intensity_factor.diffractogram_id' + '_pd_qpa_intensity_factor.phase_id' + +save_ + +save_pd_qpa_intensity_factor.diffractogram_id + + _definition.id '_pd_qpa_intensity_factor.diffractogram_id' + _definition.update 2023-01-15 + _description.text +; + The diffractogram (see _pd_diffractogram.id) to which the intensity factor + relates. +; + _name.category_id pd_qpa_intensity_factor + _name.object_id diffractogram_id + _name.linked_item_id '_pd_diffractogram.id' + _type.purpose Link + _type.source Related + _type.container Single + _type.contents Text + +save_ + +save_pd_qpa_intensity_factor.phase_id + + _definition.id '_pd_qpa_intensity_factor.phase_id' + _definition.update 2023-01-22 + _description.text +; + The phase (see _pd_phase.id) to which the intensity factor applies. +; + _name.category_id pd_qpa_intensity_factor + _name.object_id phase_id + _name.linked_item_id '_pd_phase.id' + _type.purpose Link + _type.source Related + _type.container Single + _type.contents Text + +save_ + +save_pd_qpa_intensity_factor.value + + _definition.id '_pd_qpa_intensity_factor.value' + _definition.update 2023-01-22 + _description.text +; + An intensity or scale factor value associated with the given phase and + diffractogram, which, when divided by the appropriate calibration value + defined in _pd_qpa_calib_factor.*, allows quantitative phase analysis to be + undertaken. + + This value is not, in general, transferable between different program types + and versions, as each software package may incorporate different constants + or normalisations into their calculations. However, if all values for a + given diffractogram, or CIF container, are self-consistent, then + quantification is able to be undertaken. + + A description of the associated quantification procedure can be found in + the equivalent enumeration in _pd_qpa_overall.method. +; + _name.category_id pd_qpa_intensity_factor + _name.object_id value + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_intensity_factor.value_su + + _definition.id '_pd_qpa_intensity_factor.value_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_intensity_factor.value. +; + _name.category_id pd_qpa_intensity_factor + _name.object_id value_su + _name.linked_item_id '_pd_qpa_intensity_factor.value' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + save_PD_QPA_INTERNAL_STD _definition.id PD_QPA_INTERNAL_STD @@ -8930,5 +9042,7 @@ save_ Renamed _pd_char.mass_atten_coef_mu_obs to _pd_char.mass_atten_coef_mu_meas. - Updated _pd_phase.name + Updated _pd_phase.name. + + Created PD_QPA_INTENSITY_FACTOR. ; From 4e10daa5a39464c0db600a53bd160eaf20e54f96 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Mon, 23 Jan 2023 19:53:37 +0800 Subject: [PATCH 10/24] add _pd_qpa_internal_std.crystallinity_percent --- cif_pow.dic | 47 +++++++++++++++++++++++++++++++++++++++++++++++ 1 file changed, 47 insertions(+) diff --git a/cif_pow.dic b/cif_pow.dic index d070d8a..f94dbde 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8155,6 +8155,53 @@ save_pd_qpa_internal_std.block_id save_ +save_pd_qpa_internal_std.crystallinity_percent + + _definition.id '_pd_qpa_internal_std.crystallinity_percent' + _definition.update 2023-01-23 + _description.text +; + Per cent crystallinity of the internal standard. + + Materials are rarely 100% crystalline as the crystal structure at the + material's surface is able to relax, and/or contain reaction products. This + thin, disordered surface layer can account for several mass percent of the + standard, and, as such, can affect any resultant quantification based on the + standard. + + Knowledge of the internal standard crystallinity allows for the known mass + addition to be corrected to a crystalline addition, which is the addition + being analysed in a diffraction experiment. +; + _name.category_id pd_qpa_internal_std + _name.object_id crystallinity_percent + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _enumeration.range 0.0:100.0 + _units.code none + +save_ + +save_pd_qpa_internal_std.crystallinity_percent_su + + _definition.id + '_pd_qpa_internal_std.crystallinity_percent_su' + _definition.update 2023-01-23 + _description.text +; + Standard uncertainty of _pd_qpa_internal_std.crystallinity_percent. +; + _name.category_id pd_qpa_internal_std + _name.object_id crystallinity_percent_su + _name.linked_item_id '_pd_qpa_internal_std.crystallinity_percent' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + save_pd_qpa_internal_std.mass_percent _definition.id '_pd_qpa_internal_std.mass_percent' From d16a89a3335d2cd78b07c6a8cb971cd70dde0e6c Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 15:47:39 +0800 Subject: [PATCH 11/24] add _pd_qpa_calib_factor.other to record calib values for non-supported QPA algorithms --- cif_pow.dic | 53 ++++++++++++++++++++++++++++++++++++++++++++++++++--- 1 file changed, 50 insertions(+), 3 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index f94dbde..64463b4 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7659,6 +7659,52 @@ save_pd_qpa_calib_factor.I_over_Ic_su save_ +save_pd_qpa_calib_factor.other + + _definition.id '_pd_qpa_calib_factor.other + _definition.update 2023-01-24 + _description.text +; + A calibration value associated with the given phase which allows + quantitative phase analysis to be undertaken. + + The type of data this value represents must be given in + _pd_qpa_calib_factor.special_details. + + A description of the associated quantification procedure must be given in + _pd_qpa_overall.method. + + When this data item is used in many phases present in the same + diffractogram, the person creating the CIF file must ensure that they are + have consistent definitions. +; + _name.category_id pd_qpa_calib_factor + _name.object_id other + _type.purpose Measurand + _type.source Derived + _type.container Single + _type.contents Real + _units.code none + +save_ + +save_pd_qpa_calib_factor.other_su + + _definition.id '_pd_qpa_calib_factor.other_su' + _definition.update 2023-01-22 + _description.text +; + Standard uncertainty of _pd_qpa_calib_factor.other. +; + _name.category_id pd_qpa_calib_factor + _name.object_id other_su + _name.linked_item_id '_pd_qpa_calib_factor.other' + _units.code none + + _import.get [{'file':templ_attr.cif 'save':general_su}] + +save_ + save_pd_qpa_calib_factor.phase_id _definition.id '_pd_qpa_calib_factor.phase_id' @@ -7792,9 +7838,9 @@ save_pd_qpa_calib_factor.ZMV A ZMV calibration value associated with the given phase which allows quantitative phase analysis to be undertaken. - If the ZMV value used in the quantification can be derived from the - structural information present with the phase, then this value - does not need to be given. + If this value is not given, please ensure the atoms in the unit cell are + given in an ATOM_TYPE list to allow for the correct calculation of + _cell.atomic_mass. A description of the associated quantification procedure can be found in the equivalent enumeration in _pd_qpa_overall.method. @@ -8179,6 +8225,7 @@ save_pd_qpa_internal_std.crystallinity_percent _type.source Derived _type.container Single _type.contents Real + _enumeration.default 100.0 _enumeration.range 0.0:100.0 _units.code none From c7097a4aaa1f12578dc2ec2240b36662de1a0c56 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 21:36:34 +0800 Subject: [PATCH 12/24] update description of _pd_qpa_overall.method enumeration --- cif_pow.dic | 6 ++++-- 1 file changed, 4 insertions(+), 2 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 64463b4..ca0b814 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8400,8 +8400,10 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the absorption-diffraction methodology methodology [1]. - _pd_qpa_calib_factor.absorption_diffraction should be defined for each - phase, which corresponds to C~p~, below. In addition, + _pd_qpa_calib_factor.absorption_diffraction, which corresponds to C~p~, + below should be defined for each phase. _pd_qpa_intensity_factor.value, + which corresponds to I~p~, below, should be defined for each + diffractogram the phase appears in. In addition, _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each diffractogram. From 2b26ddb8b0f0e840edd83d7984dc8e3eb19351b2 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 21:39:08 +0800 Subject: [PATCH 13/24] update description of 'external_standard' in _pd_qpa_overall.method --- cif_pow.dic | 16 ++++++++-------- 1 file changed, 8 insertions(+), 8 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index ca0b814..68a213c 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -14,7 +14,7 @@ data_CIF_POW _dictionary.title CIF_POW _dictionary.class Instance _dictionary.version 2.5.0 - _dictionary.date 2023-01-22 + _dictionary.date 2023-01-24 _dictionary.uri https://raw.githubusercontent.com/COMCIFS/Powder_Dictionary/master/cif_pow.dic _dictionary.ddl_conformance 3.11.10 @@ -8373,7 +8373,7 @@ save_ save_pd_qpa_overall.method _definition.id '_pd_qpa_overall.method' - _definition.update 2023-01-22 + _definition.update 2023-01-24 _description.text ; The type of quantification method applied to the given diffractogram. @@ -8461,17 +8461,17 @@ save_pd_qpa_overall.method The absolute weight fraction of phase p, W~p~, is given by - W~p~ = [S~p~ / C~p~] * \mu^*^~m~ + W~p~ = [I~p~ / C~p~] * \mu^*^~m~ - where S~p~ is the Rietveld scale factor of the analyte phase, and + where I~p~ = S~p~/K, where S~p~ is the Rietveld scale factor of the + analyte phase and K is a previously determined diffractometer constant. \mu^*^~m~ is the mass absorption coefficient of the entire specimen. C~p~ is given as - C~p~ = K /(Z * M * V)~p~ + C~p~ = 1 /(Z * M * V)~p~ where 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, all of phase p, - and K is the previously determined diffractometer constant. + formula weight, and V is the volume of the unit cell, all of phase p. [1] O'Connor, B. H. & Raven, M. D. (1988). Powder Diffr. 3, 2-6. [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. @@ -9071,7 +9071,7 @@ save_ Deprecated _pd_refln.wavelength_id after consultation with PDDMG. ; - 2.5.0 2023-01-22 + 2.5.0 2023-01-24 ; ## Retain above version number and increment date until final ## release From eef0a91413944b1e163c42e585305b897a166542 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 21:46:55 +0800 Subject: [PATCH 14/24] a betterer description of 'external_standard' in _pd_qpa_overall.method --- cif_pow.dic | 9 ++++----- 1 file changed, 4 insertions(+), 5 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 68a213c..072159f 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8461,12 +8461,11 @@ save_pd_qpa_overall.method The absolute weight fraction of phase p, W~p~, is given by - W~p~ = [I~p~ / C~p~] * \mu^*^~m~ + W~p~ = [(S~p~/K) / C~p~] * \mu^*^~m~ - where I~p~ = S~p~/K, where S~p~ is the Rietveld scale factor of the - analyte phase and K is a previously determined diffractometer constant. - \mu^*^~m~ is the mass absorption coefficient of the entire specimen. - C~p~ is given as + where S~p~ is the Rietveld scale factor of the analyte phase, K is a + previously determined diffractometer constant, and \mu^*^~m~ is the + mass absorption coefficient of the entire specimen. C~p~ is given as C~p~ = 1 /(Z * M * V)~p~ From 534b504a60de12272a14049f93844cfc521d3bc0 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 21:48:31 +0800 Subject: [PATCH 15/24] Revert "a betterer description of 'external_standard' in _pd_qpa_overall.method" This reverts commit eef0a91413944b1e163c42e585305b897a166542. --- cif_pow.dic | 9 +++++---- 1 file changed, 5 insertions(+), 4 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 072159f..68a213c 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8461,11 +8461,12 @@ save_pd_qpa_overall.method The absolute weight fraction of phase p, W~p~, is given by - W~p~ = [(S~p~/K) / C~p~] * \mu^*^~m~ + W~p~ = [I~p~ / C~p~] * \mu^*^~m~ - where S~p~ is the Rietveld scale factor of the analyte phase, K is a - previously determined diffractometer constant, and \mu^*^~m~ is the - mass absorption coefficient of the entire specimen. C~p~ is given as + where I~p~ = S~p~/K, where S~p~ is the Rietveld scale factor of the + analyte phase and K is a previously determined diffractometer constant. + \mu^*^~m~ is the mass absorption coefficient of the entire specimen. + C~p~ is given as C~p~ = 1 /(Z * M * V)~p~ From 3bbe1454db3b875a167aa17dad9d71996ae9fe1c Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 21:55:21 +0800 Subject: [PATCH 16/24] enhance description of 'RIR' in _pd_qpa_overall.method --- cif_pow.dic | 14 +++++++++----- 1 file changed, 9 insertions(+), 5 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 68a213c..10170c6 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8539,12 +8539,16 @@ save_pd_qpa_overall.method The relative weight fraction of phase p, W~p~, is given by - W~p~ = [(I~p~/I~p,rel~) / C~p~] / Sum[(I~k~/I~k,rel~) / C~k~, k=1:P] + W~p~ = [I~p~ / C~p~] / Sum[I~k~ / C~k~, k=1:P] - where I~p~ is the intensity of the analyte peak of phase p, I~P,rel~ - is the ratio between the analyte peak and the most intense peak for - phase p, and C~p~ is the reference intensity ratio for phase p. - The sum is taken over all phases present in the specimen. + where I~p~=I~p~^'^/I~p,rel~, where I~p~^'^ is the intensity of the + analyte peak of phase p and I~P,rel~ is the intensity ratio between the + analyte peak and the most intense peak for phase p. The sum is taken + over all phases present in the specimen. C~p~ is the reference + intensity ratio for phase p, must be pre-calculated with a known, + crystalline internal standard, as + + C~p~ = (W~s~/W~p~) * (I~p~^'^/I~s~^'^) * (I~s,rel~/(I~p,rel~) [1] Hubbard, C. R., Evans, E. H. & Smith, D. K. (1976). J. Appl. Crystallogr. 9, 169-174. From c8451826dbebe28a6f37a50210c0871451c189a5 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 22:01:33 +0800 Subject: [PATCH 17/24] added ' --- cif_pow.dic | 2 +- 1 file changed, 1 insertion(+), 1 deletion(-) diff --git a/cif_pow.dic b/cif_pow.dic index 10170c6..7710d42 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7661,7 +7661,7 @@ save_ save_pd_qpa_calib_factor.other - _definition.id '_pd_qpa_calib_factor.other + _definition.id '_pd_qpa_calib_factor.other' _definition.update 2023-01-24 _description.text ; From b6594dac34bfb07357958f4bf6c375506d9e8442 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Tue, 24 Jan 2023 22:05:39 +0800 Subject: [PATCH 18/24] fix ordering --- cif_pow.dic | 2 +- 1 file changed, 1 insertion(+), 1 deletion(-) diff --git a/cif_pow.dic b/cif_pow.dic index 0ef95d0..8575216 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8249,8 +8249,8 @@ save_pd_qpa_internal_std.crystallinity_percent _type.source Derived _type.container Single _type.contents Real - _enumeration.default 100.0 _enumeration.range 0.0:100.0 + _enumeration.default 100.0 _units.code none save_ From c06e58d06569a19301e200d2b74c49fb24af2c25 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Thu, 26 Jan 2023 11:28:07 +0800 Subject: [PATCH 19/24] added description to _pd_qpa_calib_factor.ZMV re information required to calculate it --- cif_pow.dic | 6 +++--- 1 file changed, 3 insertions(+), 3 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 8575216..70d48d4 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -7862,9 +7862,9 @@ save_pd_qpa_calib_factor.ZMV A ZMV calibration value associated with the given phase which allows quantitative phase analysis to be undertaken. - If this value is not given, please ensure the atoms in the unit cell are - given in an ATOM_TYPE list to allow for the correct calculation of - _cell.atomic_mass. + If this value is not given, please ensure that _cell.volume and either + _cell.atomic_mass or the atoms in the unit cell are given in an ATOM_TYPE + list, to allow for the correct calculation of ZMV. A description of the associated quantification procedure can be found in the equivalent enumeration in _pd_qpa_overall.method. From 2ad58063896b1f1b66a01cc23dc6907ca58b5b21 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Thu, 26 Jan 2023 13:16:07 +0800 Subject: [PATCH 20/24] streamline explanations in _pd_qpa_overall.method enumerations --- cif_pow.dic | 69 ++++++++++++++++++++++++++++++----------------------- 1 file changed, 39 insertions(+), 30 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 70d48d4..d1e6e1e 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8424,20 +8424,22 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the absorption-diffraction methodology methodology [1]. - _pd_qpa_calib_factor.absorption_diffraction, which corresponds to C~p~, - below should be defined for each phase. _pd_qpa_intensity_factor.value, - which corresponds to I~p~, below, should be defined for each - diffractogram the phase appears in. In addition, - _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs - must be given for the specimen in each diffractogram. - The absolute weight fraction of phase p, W~p~, is given by W~p~ = [I~p~ / C~p~] * \mu^*^~m~ where I~p~ is the intensity of the analyte peak, \mu^*^~m~ is the mass absorption coefficient of the entire specimen, and C~p~ is a previously - determined calibration constant. + determined calibration constant. Intensities from unknown specimens + must be collected under the same conditions as the calibration was + determined, or normalised to match. + + _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs + must be given for the specimen in each diffractogram. + + The values utilised for I~p~ and C~p~ can be recorded using + _pd_qpa_intensity_factor.value and + _pd_qpa_calib_factor.absorption_diffraction, respectively. [1] Klug, H.P. & Alexander, L.E. (1974). X-Ray Diffraction Procedures: For Polycrystalline and Amorphous Materials. New York: Wiley. @@ -8447,9 +8449,6 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the Direct Derivation Method [1-6]. - _pd_qpa_calib_factor.DDM should be defined for each phase, which - corresponds to C~p~, below. - The relative weight fraction of phase p, W~p~, is given by W~p~ = (I~p~ / C~p~) / Sum(I~k~ / C~k~, k=1:P) @@ -8464,6 +8463,10 @@ save_pd_qpa_overall.method number of electrons belonging to the i^th^ atom of phase p, and N~p~ is the number of atoms in the formula unit of phase p. + The values utilised for I~p~ and C~p~ can be recorded using + _pd_qpa_intensity_factor.value and _pd_qpa_calib_factor.DDM, + respectively. + [1] Toraya, H. (2016). J. Appl. Crystallogr. 49, 1508-1516. [2] Toraya, H. (2017). J. Appl. Crystallogr. 50, 820-829. [3] Toraya, H. (2017). J. Appl. Crystallogr. 50, 665-665. @@ -8477,12 +8480,6 @@ save_pd_qpa_overall.method standard methodology [1] to quantify absolute phase fractions taken from Rietveld [2] refinements. - _pd_qpa_calib_factor.external_standard can be defined for each phase, - but data items from the PD_QPA_EXTERNAL_STANDARD category should be - preferentially used. In addition, _pd_char.mass_atten_coef_mu_calc or - _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each - diffractogram. - The absolute weight fraction of phase p, W~p~, is given by W~p~ = [I~p~ / C~p~] * \mu^*^~m~ @@ -8497,6 +8494,15 @@ save_pd_qpa_overall.method where 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, all of phase p. + _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs + must be given for the specimen in each diffractogram. + + The values utilised for I~p~ and C~p~ can be recorded using + _pd_qpa_intensity_factor.value and + _pd_qpa_calib_factor.external_standard, respectively, however, data + items from the PD_QPA_EXTERNAL_STANDARD category should be + preferentially used. + [1] O'Connor, B. H. & Raven, M. D. (1988). Powder Diffr. 3, 2-6. [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. ; @@ -8506,19 +8512,17 @@ save_pd_qpa_overall.method value was determined using corundum (\a-alumina) as the standard, and the mass ratio of the standard and analyte phases was 50:50. - _pd_qpa_calib_factor.I_over_Ic should be defined for each phase, which - corresponds to C~p~. - For a description of the RIR methodology, see the entry for the 'RIR'. + + The values utilised for I~p~ and C~p~ can be recorded using + _pd_qpa_intensity_factor.value and _pd_qpa_calib_factor.I_over_Ic, + respectively. ; PONKCS ; Quantitative phase analysis was undertaken following the Partial Or No Known Crystal Structure methodology [1]. - _pd_qpa_calib_factor.PONKCS should be defined for each phase. Its value - corresponds to the value C~p~, below. - The relative weight fraction of phase p, W~p~, is given by W~p~ = (S~p~ / C~p~) / Sum(S~k~ / C~k~, k=1:P) @@ -8544,6 +8548,10 @@ save_pd_qpa_overall.method approach, the entire quantification is to be marked as 'PONKCS', and all phases should define _pd_qpa_calib_factor.value. + The values utilised for I~p~ and C~p~ can be recorded using + _pd_qpa_intensity_factor.value and _pd_qpa_calib_factor.PONKCS, + respectively. + [1] Scarlett, N.V.Y. & Madsen, I.C. (2006). Powder Diffr. 21, 278-284. ; RIR @@ -8554,9 +8562,6 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the Reference Intensity Ratio methodology [1-3]. - _pd_qpa_calib_factor.RIR should be defined for each phase. Its value - corresponds to the value C~p~, below. - The method of determining the RIR value, and the particular standard against which it was calculated should be given in the _pd_qpa_calib_factor.special_details for each phase. @@ -8574,6 +8579,10 @@ save_pd_qpa_overall.method C~p~ = (W~s~/W~p~) * (I~p~^'^/I~s~^'^) * (I~s,rel~/(I~p,rel~) + The values utilised for I~p~ and C~p~ can be recorded using + _pd_qpa_intensity_factor.value and _pd_qpa_calib_factor.RIR, + respectively. + [1] Hubbard, C. R., Evans, E. H. & Smith, D. K. (1976). J. Appl. Crystallogr. 9, 169-174. @@ -8588,10 +8597,6 @@ save_pd_qpa_overall.method Quantitative phase analysis was undertaken following the ZMV algorithm [1] in conjunction with Rietveld [2] refinements. - _pd_qpa_calib_factor.ZMV can be defined, if desired, for each phase, - but can be otherwise be calculated from the phase's crystal structure - details. Its value corresponds to the value C~p~, below. - The relative weight fraction of phase p, W~p~, is given by W~p~ = (S~p~ / C~p~) / Sum(S~k~ / C~k~, k=1:P) @@ -8604,6 +8609,10 @@ save_pd_qpa_overall.method where 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, all of phase p. + The values utilised for I~p~ and C~p~ can be recorded using + _pd_qpa_intensity_factor.value and _pd_qpa_calib_factor.ZMV, + respectively. + [1] Hill,R.J. & Howard, C.J. (1987). J. Appl. Crystallogr. 20, 467-474. [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. ; From e327444715b98b430b60675d28cd7900d6a5ffda Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Fri, 27 Jan 2023 21:17:14 +0800 Subject: [PATCH 21/24] finalise description of absorption_diffraction --- cif_pow.dic | 10 ++++++---- 1 file changed, 6 insertions(+), 4 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index d1e6e1e..27bf393 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8430,9 +8430,10 @@ save_pd_qpa_overall.method where I~p~ is the intensity of the analyte peak, \mu^*^~m~ is the mass absorption coefficient of the entire specimen, and C~p~ is a previously - determined calibration constant. Intensities from unknown specimens - must be collected under the same conditions as the calibration was - determined, or normalised to match. + determined calibration constant which depends on the data collection + conditions and the nature of the phase being calibrated. Intensities + from unknown specimens must be collected under the same conditions as + the calibration was determined, or normalised to match. _pd_char.mass_atten_coef_mu_calc or _pd_char.mass_atten_coef_mu_obs must be given for the specimen in each diffractogram. @@ -8442,7 +8443,8 @@ save_pd_qpa_overall.method _pd_qpa_calib_factor.absorption_diffraction, respectively. [1] Klug, H.P. & Alexander, L.E. (1974). X-Ray Diffraction Procedures: - For Polycrystalline and Amorphous Materials. New York: Wiley. + For Polycrystalline and Amorphous Materials. New York: Wiley. pp. + 532-534. ; DDM ; From f61c03b86415f3346876136fdae65e45837a6c96 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Fri, 27 Jan 2023 22:17:27 +0800 Subject: [PATCH 22/24] updated some references --- cif_pow.dic | 14 ++++---------- 1 file changed, 4 insertions(+), 10 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 27bf393..dde016f 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8562,7 +8562,7 @@ save_pd_qpa_overall.method 'I/Ic'. Quantitative phase analysis was undertaken following the Reference - Intensity Ratio methodology [1-3]. + Intensity Ratio methodology [1]. The method of determining the RIR value, and the particular standard against which it was calculated should be given in the @@ -8585,19 +8585,12 @@ save_pd_qpa_overall.method _pd_qpa_intensity_factor.value and _pd_qpa_calib_factor.RIR, respectively. - [1] Hubbard, C. R., Evans, E. H. & Smith, D. K. (1976). J. Appl. - Crystallogr. 9, 169-174. - - [2] Hubbard, C. R. & Snyder, R. L. (1988). Powder Diffr. 3, 74-77. - - [3] Snyder, R. L. & Bish, D. L. (1989). In Modern Powder Diffraction, - edited by D. L. Bish & J. E. Post, pp. 101-142. Washington DC: - Mineralogical Society of America. + [1] Snyder, R. L. (1992). Powder Diffr. 7, 186-192. ; ZMV ; Quantitative phase analysis was undertaken following the ZMV - algorithm [1] in conjunction with Rietveld [2] refinements. + algorithm [1-2] in conjunction with Rietveld [3] refinements. The relative weight fraction of phase p, W~p~, is given by @@ -8616,6 +8609,7 @@ save_pd_qpa_overall.method respectively. [1] Hill,R.J. & Howard, C.J. (1987). J. Appl. Crystallogr. 20, 467-474. + [1] Bish,D.L. & Howard, S.A. (1988). J. Appl. Crystallogr. 21, 86-91. [2] Rietveld, H. M. (1969). J. Appl. Crystallogr. 2, 65-71. ; other From 4cc3e2c06f252335a9533af5666ef0ce75907821 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Thu, 2 Feb 2023 21:48:43 +0800 Subject: [PATCH 23/24] remove reference to "or CIF container" --- cif_pow.dic | 4 ++-- 1 file changed, 2 insertions(+), 2 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index dde016f..a9e41f7 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -8130,8 +8130,8 @@ save_pd_qpa_intensity_factor.value This value is not, in general, transferable between different program types and versions, as each software package may incorporate different constants or normalisations into their calculations. However, if all values for a - given diffractogram, or CIF container, are self-consistent, then - quantification is able to be undertaken. + given diffractogram are self-consistent, then quantification is able to be + undertaken. A description of the associated quantification procedure can be found in the equivalent enumeration in _pd_qpa_overall.method. From a4387fb5377fe0a9579a928b205fe51f0f670294 Mon Sep 17 00:00:00 2001 From: rowlesmr Date: Thu, 2 Feb 2023 21:52:49 +0800 Subject: [PATCH 24/24] fix dates to avoid clash with core --- cif_pow.dic | 4 ++-- 1 file changed, 2 insertions(+), 2 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index a9e41f7..9d93889 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -14,7 +14,7 @@ data_CIF_POW _dictionary.title CIF_POW _dictionary.class Instance _dictionary.version 2.5.0 - _dictionary.date 2023-01-24 + _dictionary.date 2023-01-29 _dictionary.uri https://raw.githubusercontent.com/COMCIFS/Powder_Dictionary/master/cif_pow.dic _dictionary.ddl_conformance 3.11.10 @@ -9112,7 +9112,7 @@ save_ Deprecated _pd_refln.wavelength_id after consultation with PDDMG. ; - 2.5.0 2023-01-24 + 2.5.0 2023-01-29 ; ## Retain above version number and increment date until final ## release