Karin,
Please see:
https://www-s.nist.gov/srmors/certificates/archive/1976.pdf
for a copy of 1976 certificate.
The run time parameters of 0.5 sec count time and a step width of 0.005 degrees are most certainly not optimal. You should fit your profiles to determine their FWHM values and set the step width to obtain a minimum of six points above the FWHM. This is typically 0.01 degrees.
Regards,
Jim
James P. Cline
Ceramics Division
National Institute of Standards and Technology
100 Bureau Dr. stop 8520 [ B113 / Bldg 217 ]
Gaithersburg, MD 20899-8523 USA
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(301) 975 5793
FAX (301) 975 5334
-----Original Message-----
From: Support and use of X-ray diffraction instrumentation [mailto:[log in to unmask]] On Behalf Of Karin Liltorp
Sent: Friday, May 25, 2012 6:18 AM
To: [log in to unmask]
Subject: Re: **JUNK** Re: NIST standard 1976 does not match certified intensities
Dear all,
Again I have to thank you for you enthusiams in trying to solve our problem.Sorry to bother you again - but I really appreciate all the interesting topics that has come up in the discussion. Does any of you have the certificate for the NIST1976 standard? (not a or b - our serial number is A13-B73 (-S) F-Nr 06/10-504)
Below I have added all the information that I have from a run (as I guess my information has not been fulfiling :)) The variations have become smaller by increasing sample time as someone suggested - however, as do not have the right corundum certificate I am still not sure whether the values are OK (and still quite some variations are seen).
Best regards
Karin
Total estimated time: 02.06
Meas delay time: 0
Estimated scantime: 7600 s
Scan mode: step scan
Start position: 24
Increment: 0.005
Steps: 15200
Time pr step: 0.5 s
Motorized slit changer: out
Rotation: On
Generator voltage: 40 kV
Generator current: 40 mA
Theta:
Drive number: 1
Encoder used: No
Position: 12
Oscillation: No
2Theta:
Drive number: 2
Encoder used: No
Position: 24
Oscillation: No
Scintillation counter: Using configured values
Slits: 1.0/1.0/0.1/Ni filter
Results when using the “peak seach” option (EVA) day 1, position 1 in the sampler:
Caption Angle d value Intensity Intensity %
2-Theta ° Angstrom Count %
d=3.47900 25.584 347.900 762 37.9
d=3.47130 25.642 347.130 365 18.2
d=2.82337 31.665 282.337 53 2.6
d=2.55090 35.152 255.090 2009 100
d=2.54463 35.242 254.463 1003 49.9
d=2.37918 37.782 237.918 287 14.3
d=2.37331 37.879 237.331 155 7.7
d=2.16531 41.678 216.531 79 3.9
d=2.08530 43.357 208.530 1007 50.1
d=2.08008 43.471 208.008 524 26.1
d=1.77206 51.531 177.206 39 1.9
d=1.73999 52.553 173.999 535 26.6
d=1.73566 52.694 173.566 263 13.1
Result when using the “area” option in EVA
Obs. Max d (Obs. Max) Max Int. Net Height FWHM Raw Area Net Area
2-Theta ° Angstrom Cps Cps 2-Theta ° Cps x 2-Theta ° Cps x 2-Theta ° %
25.582 347.924 1490 1451 0.051 196.4 132.1 34.17
35.154 255.080 3993 3958 0.053 443.3 386.6
Results when using the “peak seach” option day 2, position 2 in the sampler:
Caption Angle d value Intensity Intensity %
2-Theta ° Angstrom Count %
d=3.47844 25.588 347.844 755 37.1
d=3.47011 25.651 347.011 361 17.7
d=2.55043 35.159 255.043 2035 100
d=2.54412 35.249 254.412 1031 50.7
d=2.37895 37.786 237.895 303 14.9
d=2.37303 37.883 237.303 167 8.2
d=2.08510 43.361 208.510 1032 50.7
d=2.07987 43.476 207.987 527 25.9
d=1.73990 52.556 173.990 506 24.9
d=1.73556 52.697 173.556 285 14
d=1.60141 57.503 160.141 1583 77.8
d=1.59742 57.660 159.742 781 38.4
d=1.51087 61.306 151.087 262 12.9
d=1.50718 61.473 150.718 123 6
d=1.40443 66.525 140.443 299 14.7
d=1.40096 66.712 140.096 162 8
d=1.37375 68.212 137.375 327 16.1
d=1.37031 68.407 137.031 191 9.4
d=1.23909 76.876 123.909 557 27.4
d=1.23600 77.103 123.600 287 14.1
d=1.23417 77.239 123.417 197 9.7
d=1.23107 77.469 123.107 111 5.5
d=1.09903 88.997 109.903 159 7.8
d=1.08265 90.713 108.265 93 4.6
d=1.04266 95.255 104.266 119 5.8
Result when using the “area” option in EVA
Obs. Max d (Obs. Max) Max Int. Net Height FWHM Raw Area Net Area %
2-Theta ° Angstrom Cps Cps 2-Theta ° Cps x 2-Theta ° Cps x 2-Theta °
25.588 347.852 1482 1446 0.054 226.4 134.2 32.24
35.158 255.048 4033 4010 0.104 476 416.3
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