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crdatabase
crdatabase

Crystallographic Data Base:

LaTeX Math Block
alignmentcenter
\boxed {\lambda  [Å] = \frac {12.3984}  {E [keV]}}

Inorganic Crystal Structure Database – ICSD 

https://icsd.fiz-karlsruhe.de/search/basic.xhtml

Find your compound and download CIF-file.

Open CIF-file in one of next program to look reflections positions in :

Mercury

Mercury - Crystal Structure Visualisation, Exploration and Analysis Made Easy

https://www.ccdc.cam.ac.uk/Community/csd-community/freemercury/

File -> Open -> Calculate -> Powder pattern... -> Customize... (Change energy...)

Vesta

Vesta is a 3D visualization program for structural models, volumetric data such as electron/nuclear densities, and crystal morphologies.

http://jp-minerals.org/vesta/en/download.html

File -> Open ->Utilities -> Powder diffraction pattern -> Conditions -> (Change energy...)



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lab6
lab6

LaB6 - Lanthanum hexaboride (WAXS, GID)

LaB6 NIST 660c: The certified lattice parameter for a temperature of 22.5 °C is 4.156 826 Å ± 0.000 08 Å [1]

Lanthanum hexaboride (41857 ALDRICH) [2] has the same properties as a LaB6 (NIST Standard) [3], but 10 times cheaper (smile)

LaB6 (P03 info.): d001 = 4.1549 Å,  (4.1569 Å)

Lanthanum hexaboride - powder, 10 μm, 99% 41857 ALDRICH [1]
CAS Number 12008-21-8 Linear Formula LaB6 Molecular Weight 203.77 EC Number 234-531-6 MDL number MFCD00151350 PubChem Substance ID 24854496
Conditionnement - SKU: 241857-25G
T (mp) = 2210 °C
ρ density = 2.61 g/cm3 at 25 °C
Informations Sécurité: Personal Protective Equipment Eyeshields, Gloves, type N95 (US), type P1 (EN143) respirator filter RIDADR NONH

Table 1: LaB6 - Lanthanum hexaboride (WAXS, GID)

LaB6NIST 660c [3]

Cu_Ka (1.54Å)
hkl

2θ, degrees

Q, 1/Å

10021.3581.512
11030.3852.138
11137.4422.618
20043.5073.023
21048.9583.380
21153.9903.702
22063.2204.275
30067.5494.535
31071.7474.780
31175.8465.013
22279.8725.236
32083.8475.450
32187.7945.656
40095.6736.046
41099.6456.232
330103.6636.413
331107.7526.589
420111.9366.760
421116.2486.927
332120.7267.090
422130.4137.405
500135.8057.558
510141.7807.707
511148.6857.854

References:

[1] https://www-s.nist.gov/srmors/certificates/660c.pdf

[2] http://www.sigmaaldrich.com/catalog/product/aldrich/241857?lang=fr&region=FR 

[3] https://www-s.nist.gov/srmors/view_detail.cfm?srm=660c



Figure 1: LaB6 

Figure 2: LaB6 comparing of ALDRICH and NIST in quartz and glass capillary at the ESRF-SNBL (BM01) - 2017.04.27


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silicon
silicon

Silicon standards NIST (WAXS, GID)

Parameters of NIST silicon standards, see Figure 3

Table 2: NIST silicon standards

Si - NIST-640d [3]

Cu_Ka (1.54Å)
hkl

2θ, degrees

Q, 1/Å

1

1

1

28.441

2.004

2

2

0

47.300

3.272

3

1

1

56.119

3.837

4

0

0

69.126

4.627

3

3

1

76.371

5.043

4

2

2

88.024

5.667

5

1

1

94.946

6.011

4

4

0

106.700

6.544

5

3

1

114.082

6.844

6

2

0

127.532

7.317

5

3

3

136.877

7.586

References:

[4] W. Parrish, A. J. C. Wilson, and J. I. Langford, in International Table for X-ray Crystallography, edited by A. J. C. Wilson and E. Prince (Kluwer Academic, Dordrecht, 1999), Sec. 5.2.10.



Figure 3: Copy from W. Parrish, A. J. C. Wilson, and J. I. Langford, in International Table for X-ray Crystallography, edited by A. J. C. Wilson and E. Prince (Kluwer Academic, Dordrecht, 1999), Sec. 5.2.10.

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ceo2
ceo2

CeO2 standards NIST (WAXS, GID)

Parameters of NIST CeO2 standards: 

Lattice parameters:

a = b = c  = 5.411526 Å

alpha = beta = gamma = 90°

Lattice type: F
Space group name: F m -3 m
Space group number: 225

Table : NIST CeOstandards

          CeO2 - NIST-640d [1]



hkl

d, Å

Q, 1/Å

1

1

1

1

3.124342.011044
2

2

0

0

2.705762.322152
3

2

2

0

1.913263.284021
43111.631633.850864
52221.562174.022088
64001.352884.644303
73311.241495.061004
84201.210055.192501
94221.104625.688097
105111.041456.033113
114400.956636.568041

Calibrand file of CeO2_NIST for DPDAK

F

References:

[1] Standard Reference Material 674b







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mica675
mica675

Mica Powder 675 NIST (WAXS, GID)

This Standard Reference Material (SRM) was prepared for use as an external or internal 20 φ (large d-spacing) calibration standard for powder diffractometry. The material is synthetic fluorophlogopite mica and is best suited for reflection diffractometry as pressed samples have a high degree of preferred orientation in which only the 00l reflections have significant intensity. The mica was ground to pass a 75 μm (200 mesh) sieve.

  • CAS Number 12003-38-2

  • Linear Formula Mg3K[AlF2O(SiO3)3]

  • Molecular Weight 421.24

References:

[1] https://www-s.nist.gov/srmors/view_cert.cfm?srm=675

[2] Mica Powder 675 NIST . PDF - LOAD

[3] https://www.sigmaaldrich.com/catalog/product/sial/nist675?lang=de&region=DE


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silverbeh
silverbeh

Silver Behenate (SAXS, GISAXS)

The silver behenate is known silver salts of the long-chain fatty acids.

The long-period spacing of d001=58.378 (8) Å, see Figure 6


Figure 4: Bragg peaks of silver stearate measured by SAXS [6]

References:

[5] N. Blanton, C. L. Barnes and M. Lelental, J. Appl. Cryst. (2000). 33, 172-173

[6] M Nyam-Osor, D V Soloviov, Yu S Kovalev, A Zhigunov, A V Rogachev, O I Ivankov, R V Erhan, A I Kuklin, Journal of Physics: Conference Series, Volume 351, conference 1, 2012,  DOI: 10.1088/1742-6596/351/1/012024

Figure 5: SEM micrographs [5] of silver behenate on a (5 1 0) silicon wafer, 20 000×

Figure 6: Bragg peaks from silver behenate obtained by SAXS [6]


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lupolen
lupolen

Lupolen

Lupolen is a semicrystalline high molecular weight polyethylene produced by BASF. This sample produces a very strong signal, nearly 3 orders of magnitude stronger than pure water. At q=0.03 Å-1, a scattering maximum is observed. This strong signal with a broad peak at a convenient angle can also be easily desmeared when using a slit geometry. It is a solid, so no windows are required and it is not subject to aging. For these reasons, the scattering of Lupolen is widely used as a secondary reference standard. [7]

Lupolen  [7]: d(1st order)= 20.94 nm (from q=0.03 Å-1)

Lupolen (P03 info.): d(1st order) = 36.4 nm ?

References:

[7] T. P. Russell, J. S. Lin, S. Spooner and G. D. Wignall, Intercalibration of small-angle X-ray and neutron scattering data, J. Appl. Cryst. (1988). 21, 629-638 

[8] G. D. Wignall, Instrumental resolution effects in small-angle scattering, J. Appl. Cryst. (1991). 24, 479-484



Figure 7: Scaled SAXS intensity obtained for the Lupolen™ sample of thickness t=3 mm and transmission T=0.37 (exposure time 15 mn) [7].

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collagen
collagen

Collagen

Collagen is the main structural protein in the extracellular space in the various connective tissues in the body. As the main component of connective tissue, it is the most abundant protein in mammals, making 25% to 35% of the whole-body protein content. Collagen consists of amino acids wound together to form triple-helices of elongated fibrils. It is mostly found in fibrous tissues such as tendons, ligaments, and skin. [9]

Collagen: d = 673 Å (or 650 Å)

Many modern laboratory SAXS systems are usually able to resolve the first order reflection of collagen at a scattering q-value of approx. 0.091 nm-1, corresponding to 67 nm d-spacing [10].

 

d, ÅQ, 1/ÅQ, 1/nm
16730.0093360.093361
2336.50.0186720.186722
3224.33330.0280080.280083
4168.250.0373440.373443
5134.60.046680.466804
6112.16670.0560170.560165
796.142860.0653530.653526
884.1250.0746890.746887
974.777780.0840250.840248
1067.30.0933610.933609
1161.181820.1026971.026969
1256.083330.1120331.12033

Calibrand file of Collagen for DPDAK

References:

[9] https://en.wikipedia.org/wiki/Collagen

[10] https://www.anton-paar.com/corp-en/products/applications/collagen-a-validation-sample-for-saxs-systems/

[11] https://www.sciencedirect.com/topics/medicine-and-dentistry/collagen-fibril

[12] https://www.sciencedirect.com/science/article/pii/S1063458407000052#bib21


 

Figure 8 (a)The D-period of collagen fibrils results in visible 67 nm bands when observed by electron microscopy [9,10].


Figure 8 (b):  1D scattering curve of the collagen sample extracted from the 2 D pattern [10].

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argonxrf
argonxrf

Argon (XRF)

line should be defined for the calibration of Fluorescence detector (at He atmosphere in chamber?).

: 2.957

VORTEX_1us_30kev_2048ch_201503.ini (example at ID10, ESRF)

1 at tilt = 0.045°

filename__xiact_0000_0000_0000 (example at ID10, ESRF)

: 2.957 , 197.6 / 15eV/channel

Figure 9: Example of XRF calibration picture in EH1 (ID10, ESRF)

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p03Ecal
p03Ecal

XRF at P03 - energy calibration

Figure 2 - Calibration of the X-ray beam energy

See PDF