Are there reserves of SRM's 1871 through 1875 (any or all)?
If so, is there any consideration of making these available?
And who would be the primary NIST contact for these glasses?
Finally, are glasses K373 through K377 (with U) available or documented by NIST?
Thanks in advance.
I looked into SRM-1871 to SRM-1875 at https://www.nist.gov/srm. They have all been discontinued and are out-of-stock. The certificates can be viewed here: https://www.evernote.com/shard/s23/sh/15b5752e-cc21-7ffa-76bb-5f899dfe78bf/db6a20766a2b0eff03b30baeaa187191 (https://www.evernote.com/shard/s23/sh/15b5752e-cc21-7ffa-76bb-5f899dfe78bf/db6a20766a2b0eff03b30baeaa187191). They consist of glasses engineered by Doug Blackburn and D. Kauffman numbered (K456, K493, K523), (K453, K491, K968), (K458, K489, K963), (K495, K490, K546) and (K496, K499, K1013). I believe that both Blackburn and Kauffman were long gone by the time I arrived at NIST in 2004. It is possible that some of these glasses remain in a drawer somewhere. I'll look around. Alternatively, a microanalysis standard vendor might have shards they might sell. As for a contact, I'm probably about as good as it gets. The original contacts have all retired.
Here is the compositional data I have on the K373-K377 glasses (except K374 for which I have no data)
NIST GLASS K 373
CATION NUMBER ANION NUMBER WT PCT COMPOUND WT PCT ELEMENT AT PCT ELEMENT
Na 11 2 8 1 14.06 10.4304 10.3462
Si 14 1 8 2 68.13 31.8484 25.8555
Zn 30 1 8 1 6.15 4.9407 1.7236
Ba 56 1 8 1 11.59 10.3803 1.7241
U 92 3 8 8 0.063 0.0534 0.0051
AVERAGE ATOMIC NUMBER 22.4626
WEIGHT PERCENT OXIDE TOTAL 99.993
WEIGHT PERCENT ELEMENT TOTAL 99.993
ATOMIC PERCENT ELEMENT TOTAL 100
WEIGHT PERCENT OXYGEN 42.3397
ATOM PERCENT OXYGEN 60.3455
NIST GLASS K 375
CATION NUMBER ANION NUMBER WT PCT COMPOUND WT PCT ELEMENT AT PCT ELEMENT
Na 11 2 8 1 14.05 10.423 10.3429
Si 14 1 8 2 68.09 31.8297 25.8506
Zn 30 1 8 1 6.15 4.9407 1.7242
Ba 56 1 8 1 11.58 10.3714 1.7233
U 92 3 8 8 0.13 0.1102 0.0106
AVERAGE ATOMIC NUMBER 22.5302
WEIGHT PERCENT OXIDE TOTAL 100
WEIGHT PERCENT ELEMENT TOTAL 100
ATOMIC PERCENT ELEMENT TOTAL 100
WEIGHT PERCENT OXYGEN 42.3249
ATOM PERCENT OXYGEN 60.3484
NIST GLASS K 376
CATION NUMBER ANION NUMBER WT PCT COMPOUND WT PCT ELEMENT AT PCT ELEMENT
Na 11 2 8 1 13.99 10.3785 10.3367
Si 14 1 8 2 67.72 31.6568 25.8049
Zn 30 1 8 1 6.12 4.9166 1.7222
Ba 56 1 8 1 11.54 10.3356 1.7237
U 92 3 8 8 0.63 0.5342 0.0514
AVERAGE ATOMIC NUMBER 23.0501
WEIGHT PERCENT OXIDE TOTAL 100
WEIGHT PERCENT ELEMENT TOTAL 100
ATOMIC PERCENT ELEMENT TOTAL 100
WEIGHT PERCENT OXYGEN 42.1783
ATOM PERCENT OXYGEN 60.3611
NIST GLASS K 377
CATION NUMBER ANION NUMBER WT PCT COMPOUND WT PCT ELEMENT AT PCT ELEMENT
Na 11 2 8 1 13.91 10.3192 10.3237
Si 14 1 8 2 67.28 31.4511 25.7523
Zn 30 1 8 1 6.08 4.8845 1.7186
Ba 56 1 8 1 11.47 10.2729 1.7209
U 92 3 8 8 1.26 1.0685 0.1033
AVERAGE ATOMIC NUMBER 23.6903
WEIGHT PERCENT OXIDE TOTAL 100
WEIGHT PERCENT ELEMENT TOTAL 100
ATOMIC PERCENT ELEMENT TOTAL 100
WEIGHT PERCENT OXYGEN 42.004
ATOM PERCENT OXYGEN 60.3812
I received a small amount of K-373 and K-375 from John Rutledge a few years ago. They are super beam sensitive materials. Check out the TDI curve on this one:
(https://smf.probesoftware.com/gallery/395_15_10_21_9_13_03.png)
That's an exponential fit in log space! A *double* exponential extrapolation to zero time (15 keV, 30 nA, 5 um beam). Amazingly it is within 5-6% accuracy even with a > 300% TDI correction. Here is K-373 (analyzed only for Na):
St 172 Set 1 K-0373 NBS glass, Results in Elemental Weight Percents
ELEM: Na Si Zn Ba U O
TYPE: ANAL SPEC SPEC SPEC SPEC SPEC
BGDS: MAN
TIME: 30.00 --- --- --- --- ---
BEAM: 30.29 --- --- --- --- ---
ELEM: Na Si Zn Ba U O SUM
10 11.152 31.850 4.940 10.380 .054 42.340 100.716
11 11.916 31.850 4.940 10.380 .054 42.340 101.480
12 10.119 31.850 4.940 10.380 .054 42.340 99.683
AVER: 11.062 31.850 4.940 10.380 .054 42.340 100.627
SDEV: .902 .000 .000 .000 .000 .000 .902
SERR: .521 .000 .000 .000 .000 .000
%RSD: 8.16 .00 .00 .00 .00 .00
PUBL: 10.430 31.850 4.940 10.380 .054 42.340 99.994
%VAR: 6.06 .00 .00 .00 .00 .00
DIFF: .632 .000 .000 .000 .000 .000
STDS: 301 --- --- --- --- ---
STKF: .0510 --- --- --- --- ---
STCT: 2939.1 --- --- --- --- ---
UNKF: .0541 --- --- --- --- ---
UNCT: 3115.2 --- --- --- --- ---
UNBG: 27.8 --- --- --- --- ---
ZCOR: 2.0456 --- --- --- --- ---
KRAW: 1.0599 --- --- --- --- ---
PKBG: 112.89 --- --- --- --- ---
TDI%: 332.567 --- --- --- --- ---
DEV%: .5 --- --- --- --- ---
TDIF: LOG-LOG --- --- --- --- ---
TDIT: 53.67 --- --- --- --- ---
TDII: 2781. --- --- --- --- ---
TDIL: 7.93 --- --- --- --- ---
And K-375:
St 173 Set 1 K-0375 NBS glass, Results in Elemental Weight Percents
ELEM: Na Si Zn Ba U O
TYPE: ANAL SPEC SPEC SPEC SPEC SPEC
BGDS: MAN
TIME: 30.00 --- --- --- --- ---
BEAM: 30.30 --- --- --- --- ---
ELEM: Na Si Zn Ba U O SUM
13 10.600 31.830 4.940 10.370 .110 42.320 100.170
14 10.594 31.830 4.940 10.370 .110 42.320 100.164
15 11.802 31.830 4.940 10.370 .110 42.320 101.372
AVER: 10.998 31.830 4.940 10.370 .110 42.320 100.569
SDEV: .696 .000 .000 .000 .000 .000 .696
SERR: .402 .000 .000 .000 .000 .000
%RSD: 6.32 .00 .00 .00 .00 .00
PUBL: 10.420 31.830 4.940 10.370 .110 42.320 99.990
%VAR: 5.55 .00 .00 .00 .00 .00
DIFF: .578 .000 .000 .000 .000 .000
STDS: 301 --- --- --- --- ---
STKF: .0510 --- --- --- --- ---
STCT: 2939.1 --- --- --- --- ---
UNKF: .0538 --- --- --- --- ---
UNCT: 3095.4 --- --- --- --- ---
UNBG: 27.9 --- --- --- --- ---
ZCOR: 2.0465 --- --- --- --- ---
KRAW: 1.0532 --- --- --- --- ---
PKBG: 111.97 --- --- --- --- ---
TDI%: 308.933 --- --- --- --- ---
DEV%: .7 --- --- --- --- ---
TDIF: LOG-LOG --- --- --- --- ---
TDIT: 52.67 --- --- --- --- ---
TDII: 2714. --- --- --- --- ---
TDIL: 7.91 --- --- --- --- ---
Well that explains why K373 through K377 were not assigned SRM numbers.
The homogeneity of K series glasses were documented in Special Publication 260-65 (attached).
Final documentation of SRM 1871 through 1875 in a later SP260-112 also attached now.
Quote from: crystalgrower on October 19, 2021, 06:40:34 AM
Well that explains why K373 through K377 were not assigned SRM numbers.
The homogeneity of SRM 1871-1875 were documented in Special Publication 260-65 (attached).
I do not know how I found out about them. It might have been a personal communication with Dale Newbury.
Here is the data I have on them:
St 172 K-0373 NBS glass
TakeOff = 40.0 KiloVolt = 15.0 Density = 5.000 Type = glass
from John Rutledge
Elemental Composition
Average Total Oxygen: .000 Average Total Weight%: 99.994
Average Calculated Oxygen: .000 Average Atomic Number: 16.339
Average Excess Oxygen: .000 Average Atomic Weight: 22.802
ELEM: Na Si Zn Ba U O
XRAY: ka ka ka la ma ka
ELWT: 10.430 31.850 4.940 10.380 .054 42.340
KFAC: .0508 .2498 .0408 .0789 .0004 .2264
ZCOR: 2.0527 1.2752 1.2100 1.3161 1.2878 1.8698
AT% : 10.345 25.859 1.723 1.723 .005 60.343
St 173 K-0375 NBS glass
TakeOff = 40.0 KiloVolt = 15.0 Density = 5.000 Type = glass
from John Rutledge
Elemental Composition
Average Total Oxygen: .000 Average Total Weight%: 99.990
Average Calculated Oxygen: .000 Average Atomic Number: 16.380
Average Excess Oxygen: .000 Average Atomic Weight: 22.813
ELEM: Na Si Zn Ba U O
XRAY: ka ka ka la ma ka
ELWT: 10.420 31.830 4.940 10.370 .110 42.320
KFAC: .0508 .2496 .0408 .0788 .0009 .2262
ZCOR: 2.0531 1.2752 1.2097 1.3160 1.2877 1.8709
AT% : 10.341 25.856 1.724 1.723 .011 60.346
OK, I also did a search on K-0373 and got this link:
https://www.2spi.com/catalog/standards/aweb/tayl-gls.html
OK, I remember now that NIST could not send them to me because they contain uranium and would therefore it would require an "act of congress" to get them out the door. But apparently they are available commercially.
Speaking of beam sensitive glasses from NIST, here is a look at the NIST SRM 1718 glass:
https://smf.probesoftware.com/index.php?topic=912.msg5904#msg5904
All these high Na glasses I think were made to study as possible materials for storing nuclear waste...
Nuclear waste...a science where no number of projections ever reach the reality. The only way to know something was to make it and then see what actually happened. The glasses had to be fusible at a reasonable temperature hence the Na.
I worked at AECL when they were testing borosilicate glass for the underground repository. Problem was not measuring leach rate in the presence of B...it was the heat generated by decaying fuel. it was the Devonian water that had saturated the Precambrian granite that stopped the project.
More recently, something similar with monazite as a storage material has evolved. Major accumulation of Po-210 in warehouses has been recorded. I tried a different matrix for 0.5% U and the Ce+3 spontaneously changed to Ce+4 some 10 years later. You just can;t win.
There are thousands of K-glasses and only a handful are SRMs (SRM being a NIST-held trademark). Most of the tabulated compositions are based on the raw ingredients. We would need to evaluate them by microprobe for homogeneity and by another methods for composition. This is so time consuming that only a handful were ever turned into SRM. The utility of most of the K-glasses is only in as much as the actual composition matches the input raw materials - a good assumption in most cases but only an assumption.
Still, I have found some of them to be very helpful in studying TDI effects for Na, Si and other major elements.
Attached below (please login to see attachments), is a poster of TDI measurements from the MRM 2012 on K-1718, K-412 and nepheline (my preferred primary standard for Na).