Hi Holger There is a good paper by Ian Madsen, Nikki Scarlett, and Arnt Kern about the quantification of amorphous materials - https://doi.org/10.1524/zkri.2011.1437
On the RR, I'll let the CPD know! Matthew On Thu, 14 Apr 2022 at 16:51, Holger Kletti <holger.kle...@uni-weimar.de> wrote: > an actual RR on amourphous contents like thos on crystalline mixtureswould > really be appriciable, i don't know any publications therewith. The problem > seems to exist as can be seen here, but also with internal standard method, > as in personal discussions the question on achieved negative amorphous > contents (internal as well as external standard method) arises from time to > time. And not alway this can be solved just by variation of background > polynoms or other structure related parameters. > > So if "anyone" would initiate such a RR i would like to join it .... > > Holger > Am 14.04.2022 um 09:49 schrieb Julian Richard Tolchard: > > I confess that this discussion seems to validate my personal choice to > treat Rietveld quantification (and especially amorphous quant) as something > lying between a quantificational and semi-quantificational technique. > > > > Has anyone done a proper round-robin on amorphous quant (by any methods > actually)? There have been some RR’s for crystalline mixtures I know, but I > can’t remember seeing one for crystalline+amorphous samples. > > > > > > jools > > > > *From:* rietveld_l-requ...@ill.fr <rietveld_l-requ...@ill.fr> > <rietveld_l-requ...@ill.fr> *On Behalf Of *Matthew Rowles > *Sent:* torsdag 14. april 2022 09:03 > *To:* Jonathan WRIGHT <wri...@esrf.fr> <wri...@esrf.fr> > *Cc:* RIETVELD_L Distribution List <rietveld_l@ill.fr> <rietveld_l@ill.fr> > *Subject:* Re: NIST SRM656 Analysis > > > > Hi Jon > > > > The data is put on an absolute scale through the external standard > approach. The calculations assume that the QPA for corundum in NIST > SRSM676a is 99.02 wt%. This scaling factor is then applied to the silicon > nitride pattern. > > > > re surface roughness: The samples were backpacked against a glass surface, > and the powders used as-received. I've never measured the particle size > distribution of either (any!) SRM, but the certificates describe 676a as > "fully disaggregated" and "grains are sub-micrometer in size and equi-axial > in shape" and the 656 certificate has a particle size distribution by laser > scattering, with 100% less than 5 um. In our other work, we aim to > micronise to less than 10 um. Our grinding checks show that we get 100 vol% > <15 um and 95 vol% <6 um. > > > > I've never used the Pitschke or Suortti roughness corrections available in > Topas, and have no intuition as to the magnitude of their correction or > what "proper" values should be. > > > > > > Matthew > > > > > > On Wed, 13 Apr 2022 at 18:11, Jonathan WRIGHT <wri...@esrf.fr> wrote: > > Maybe a silly question: are you assuming you have the data on an absolute > scale > in order to do these calculations? Do things like surface roughness > somehow not > matter? > > Best > > Jon > > > > > On 13/04/2022 11:56, Matthew Rowles wrote: > > Thanks Tony > > > > When I add the absorption edge correction to the silicon nitride model > (and add > > beta-silicon nitride), it becomes -2.8 wt% amorphous; up a little due to > the > > added correction and down a little due to the extra phase. > > > > If I change your al-SN thermals from 1 to those given in ICSD 77811, I > get +4.8 > > wt% amorphous. Your atoms were already neutral, so I left them as-is. > > > > If I make all the Si-nitride phases' thermal parameters == 0, then I can > get up > > to 8.5 wt% amorphous. > > > > In all of this, corundum is staying as charged atoms, with Al and O beqs > fixed > > at 0.334 and 0.278. > > > > I'll have to have a go at applying the absorption edge correction; I > always > > forget which parameter is which thing and have to rederive my > understanding of > > it everytime... > > > > > > Thanks > > > > Matthew > > > > On Wed, 13 Apr 2022 at 13:58, iangie <ian...@126.com <mailto: > ian...@126.com>> wrote: > > > > Dear Matthew, > > > > I tried your data and get ~-1% amorphous. My .pro is in below link. > > > > https://www.dropbox.com/s/xuw13c91l9gq5m5/ROW.pro?dl=0 > <https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fwww.dropbox.com%2Fs%2Fxuw13c91l9gq5m5%2FROW.pro%3Fdl%3D0&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216257549%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=fQatqp0bH0nfkYmTd8bWQkEALCntqGFYjYoSOXMt5ng%3D&reserved=0> > > <https://www.dropbox.com/s/xuw13c91l9gq5m5/ROW.pro?dl=0 > <https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fwww.dropbox.com%2Fs%2Fxuw13c91l9gq5m5%2FROW.pro%3Fdl%3D0&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216267509%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=5LLaS0ghYvZKqLDm%2FSkFKRH6ltta7LOvKEb84CZnD8A%3D&reserved=0> > > > > > > I normally do not refine Beq, which I believe gives biggest source > of error > > in QPA... > > > > > > Cheers! > > > > -- > > > > *Dr. Xiaodong (Tony) Wang* > > *Senior Research Infrastructure Specialist (XRD)* > > Central Analytical Research Facility (CARF) | Queensland > University of > > Technology > > *Address:* Level 6, P Block, Gardens Point campus, 2 George St > Brisbane QLD 4000 > > *Tel:*+61 7 3138 1904 | *Mob:*0452 571 680 > > *Email:* tony <mailto:stephen.blank...@qut.edu.au>. > > <mailto:stephen.blank...@qut.edu.au>w...@qut.edu.au > > <mailto:stephen.blank...@qut.edu.au> | *Web:* > www.qut.edu.au/ife/carf > <https://eur03.safelinks.protection.outlook.com/?url=http%3A%2F%2Fwww.qut.edu.au%2Fife%2Fcarf&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216267509%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=F5DERNblJYX%2BaKhoCgJTNNBWTVeMLjChU5oceqBomIg%3D&reserved=0> > > <http://www.qut.edu.au/ife/carf > <https://eur03.safelinks.protection.outlook.com/?url=http%3A%2F%2Fwww.qut.edu.au%2Fife%2Fcarf&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216277469%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=5KO9AzzM8vBK5DcbiOXLSR%2Bpu6G1kh3LFoTJEFx2ENI%3D&reserved=0> > > > > > > > > At 2022-04-13 13:00:44, "Matthew Rowles" <rowle...@gmail.com > > <mailto:rowle...@gmail.com>> wrote: > > > > Hi all > > > > Thanks to those that have replied off-list. > > > > I've managed to jiggle things around and get various answers. If > you > > want an answer between -14 and +6 wt% amorphous, I can make it > happen. I > > can either use charged atoms or not, or use thermal parameters > or not. > > Combining those between the corundum and Si3N4, you get the > following: > > > > > > image.png > > This is using the scattering factors defined with 11 gaussians. > > > > If you use the ones defined by 9 gaussians, you get > > image.png > > > > The structures I used are below. In the certificate for 656, the > > structures are referenced, but those structures have no thermal > > parameters. Does anyone know what was used in the NIST > determination? > > > > > > > > phase_name "Aluminium_oxide_alpha_10425_icsd" > > Hexagonal( 4.759355, 12.99231) > > space_group "R -3 c H" > > site Al1 num_posns 12x 0 y 0 z 0.14772 occ Al+3 1. beq > 0.318 > > site O1 num_posns 18x 0.3064 y 0 z 0.25 occ O-2 1. beq > 0.334 > > > > phase_name "ALPHA_Marchand_ICSD_26191" > > Hexagonal( 7.75411, 5.62034) > > space_group "P31c" 'atom positions from Marchand. Thermals from > ICSD 77811 > > site Si1 num_posns 6x 0.0806 y 0.5095 z 0.3020 occ Si+4 1 beq > 0.25 > > site Si2 num_posns 6x 0.1675 y 0.2560 z 0.0070 occ Si+4 1 beq > 0.29 > > site N1 num_posns 2x 0 y 0 z 0 occ N 1. beq > 0.88 > > site N2 num_posns 2x =1/3; y =2/3; z 0.3500 occ N 1. beq > 0.46 > > site N3 num_posns 6x 0.0390 y 0.3860 z 0.0310 occ N 1. beq > 1.06 > > site N4 num_posns 6x 0.3190 y 0.3210 z 0.2660 occ N 1. beq > 0.17 > > > > phase_name "BETA_Billy_ICSD_35566" > > Hexagonal( 7.60633, 2.90778) > > space_group "P 63/m" ' structure from Billy, thermals from ICSD > 170004 > > site Si1 num_posns 6x 0.2323 y 0.4096 z 0.25 occ Si+4 1 beq > 0.231 > > site N1 num_posns 2x =1/3; y =2/3; z 0.25 occ N 1 beq > 0.326 > > site N2 num_posns 6x 0.3337 y 0.0323 z 0.25 occ N 1 beq > 0.314 > > > > > > > > > > > > > > On Tue, 12 Apr 2022 at 17:13, Matthew Rowles <rowle...@gmail.com > > <mailto:rowle...@gmail.com>> wrote: > > > > Hi all > > > > I've collected some more data, and am still getting spurious > > results, and by spurious, I mean -5 wt% amorphous in > SRM-alpha-656 > > when quantified by the external method against SRM 676a. > > > > We had some SRM-656alpha (couldn't find any of the > beta) stored in a > > drying oven, and some SRM676a stored in a cupboard. I > collected some > > data using a D8 with Ni-filtered Cu and a lynx-eye detector > (0.25° > > fixed divergence, 250 mm radius, 2x2.5° sollers). The > patterns were > > collected consecutively (using the same program), with a > single peak > > from SRM1976 (b, I think), acting as an intensity calibrant > (the > > intensity didn't appreciably change), collected before, > after, and > > between. > > > > Does anybody want to have a look at the data and see what > I'm doing > > wrong? Data available at: > > > https://raw.githubusercontent.com/rowlesmr/pdCIFplotter/changing-str-to-float-conversion/data/row_Cu_676a.xy > <https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fraw.githubusercontent.com%2Frowlesmr%2FpdCIFplotter%2Fchanging-str-to-float-conversion%2Fdata%2Frow_Cu_676a.xy&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216277469%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=bpmDTHBfC%2BxKNGENBr1Xw4lYUhVLOxqdvi7pzNv9L6g%3D&reserved=0> > > < > https://raw.githubusercontent.com/rowlesmr/pdCIFplotter/changing-str-to-float-conversion/data/row_Cu_676a.xy > <https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fraw.githubusercontent.com%2Frowlesmr%2FpdCIFplotter%2Fchanging-str-to-float-conversion%2Fdata%2Frow_Cu_676a.xy&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216287428%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=1yKQm%2Ftpm6Wz06p2gvWcFYWTcu1G%2Bc1dbzSQxaQDSuo%3D&reserved=0> > > > > > > > https://raw.githubusercontent.com/rowlesmr/pdCIFplotter/changing-str-to-float-conversion/data/row_Cu_al656.xy > <https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fraw.githubusercontent.com%2Frowlesmr%2FpdCIFplotter%2Fchanging-str-to-float-conversion%2Fdata%2Frow_Cu_al656.xy&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216287428%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=slpXNmyXO1AbhW0Dgvis%2F02k2BB0Yxgh2QLWUu7HKsY%3D&reserved=0> > > < > https://raw.githubusercontent.com/rowlesmr/pdCIFplotter/changing-str-to-float-conversion/data/row_Cu_al656.xy > <https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fraw.githubusercontent.com%2Frowlesmr%2FpdCIFplotter%2Fchanging-str-to-float-conversion%2Fdata%2Frow_Cu_al656.xy&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216287428%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=slpXNmyXO1AbhW0Dgvis%2F02k2BB0Yxgh2QLWUu7HKsY%3D&reserved=0> > > > > > > > > Thanks > > > > Matthew > > > > > > > > > > > > On Wed, 16 Mar 2022 at 21:13, Matthew Rowles < > rowle...@gmail.com > > <mailto:rowle...@gmail.com>> wrote: > > > > Hi List People > > > > Do any of you use NIST SRM656 in your quantitative > analysis > > quality control? > > > > I've recently started at a new lab, and am finding it > impossible > > to make a physically realistic model (in Topas) that > gives > > results anywhere near correct (or at least, close to the > > certificate values). > > > > As an example, using the external std approach with > SRM676, I've > > managed to calculate there is -11 wt% amorphous in the > beta-656 > > standard. > > > > I've tried using the silicon nitride structures given in > the SRM > > certificate, but the papers and the ICSD entries don't > list any > > thermal parameters. > > > > I can get the same results as given on the certificate > using a > > siroquant model, but I don't know the provenance of the > HKL > > files used in the analysis. > > > > > > Thanks in advance > > > > > > Matthew Rowles > > > > > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > Please do NOT attach files to the whole list < > alan.he...@neutronoptics.com> > > Send commands to <lists...@ill.fr> eg: HELP as the subject with no body > text > > The Rietveld_L list archive is on > http://www.mail-archive.com/rietveld_l@ill.fr/ > <https://eur03.safelinks.protection.outlook.com/?url=http%3A%2F%2Fwww.mail-archive.com%2Frietveld_l%40ill.fr%2F&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216287428%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=R7sTNT7bv4AyZJm4sMxNH2KFbpGDV9a73QViQFxYbvo%3D&reserved=0> > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > Please do NOT attach files to the whole list <alan.he...@neutronoptics.com > > > Send commands to <lists...@ill.fr> eg: HELP as the subject with no body > text > The Rietveld_L list archive is on > http://www.mail-archive.com/rietveld_l@ill.fr/ > <https://eur03.safelinks.protection.outlook.com/?url=http%3A%2F%2Fwww.mail-archive.com%2Frietveld_l%40ill.fr%2F&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7Ced6d59fce55f4454e6a408da1de54221%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C0%7C637855168216287428%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=R7sTNT7bv4AyZJm4sMxNH2KFbpGDV9a73QViQFxYbvo%3D&reserved=0> > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > Please do NOT attach files to the whole list <alan.he...@neutronoptics.com> > <alan.he...@neutronoptics.com> > Send commands to <lists...@ill.fr> <lists...@ill.fr> eg: HELP as the subject > with no body text > The Rietveld_L list archive is on > http://www.mail-archive.com/rietveld_l@ill.fr/ > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > Please do NOT attach files to the whole list <alan.he...@neutronoptics.com > > > Send commands to <lists...@ill.fr> eg: HELP as the subject with no body > text > The Rietveld_L list archive is on > http://www.mail-archive.com/rietveld_l@ill.fr/ > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > >
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Please do NOT attach files to the whole list <alan.he...@neutronoptics.com> Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
