SRMs K-373 to K-377 and K-1871 to 1875

[crystalgrower]

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.

[Nicholas Ritchie]

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.  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               

[Probeman]

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:



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     ---     ---     ---     ---     ---

[crystalgrower]

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.

[Probeman]

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.

[Probeman]

Speaking of beam sensitive glasses from NIST, here is a look at the NIST SRM 1718 glass:

https://probesoftware.com/smf/index.php?topic=912.msg5904#msg5904

All these high Na glasses I think were made to study as possible materials for storing nuclear waste...

[crystalgrower]

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.

[Nicholas Ritchie]

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.

[Probeman]

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).