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> *On
Behalf Of *Matthew Rowles
*Sent:* torsdag 14. april 2022 09:03
*To:* Jonathan WRIGHT <wri...@esrf.fr>
*Cc:* RIETVELD_L Distribution List <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
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> <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
>
>
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