First independent Isotopic results [UPDATE#2 - Second Earthtech Ni Isotopic report agrees with University of Missouri results]

Without too much comment so that you can all see it fast - the very first isotopic data sent to us of one of the independent testing parties.

Note we do not know which sample is what - but there is

- a sample of GS3 fuel

- a sample of GS3 ash

- a sample of GS2 ash

Ash samples were fully extracted and mixed before sample selection

before all the data is in and the index key is released - see what you think is what.

https://goo.gl/6bvbjl

UPDATE#1 - MURR, University of Missouri isotopic analysis of Ni and Li

The analysis is for Parkhomov Ni and LiAlH4 as well GS2 Ash and GS3 Fuel/Ash (which contained Parkhomov Ni) and was conducted at http://acg.missouri.edu

Results are

https://goo.gl/mfcNMf

We thank the University of Missouri for conducting this Assay.

We know from previous EDX that Parkhomov LiAlH4 contains Chlorine, but in terms of 7Li and 6Li, both US sourced and Parkhomov LiAlH4 both have near-natural isotopic ratios as given on wikipedia.

Both were 7Li 92.6 : 6Li 7.4 to 1dp

Here are the testers comments:

"Attached is a spreadsheet with isotopic results and approximate elemental concentrations.

The basic message of the results is that, to the ability of our quadrupole ICP-MS to measure, the Li isotope ratios are effectively the same in all four samples that contain major amounts of Li.  We do not have a “natural” Li standard with certified isotope ratios, and since Li is a light element, the ratios can vary a bit in nature.  Thus I had to assume a natural 7Li/6Li ratio in the standard and compare its isotope ratios with those from the samples, keeping the Li in the standard and sample solutions at an approximately constant concentration.  Effectively, it appears that (7Li/6Li) in all samples is a bit higher than the standard.

Also, the Ni in all samples appears to be isotopically natural.  All ratios measured are within one standard deviation of natural Ni, except for one (61Ni/58Ni) measurement in Vial 46, run 2, which was within two standard deviations of the natural ratio.

Please keep in mind that the elemental concentrations were measured without internal standard and may only be considered approximate.

Below are some method notes:

1. The LiAlH4 sample (52.2 mg) was reacted with 1 mL ultrapure water (H2O).  The resulting suspension of white solids was dissolved by adding 1 mL of conc. HNO3 (Optima grade).
   
   
2. To the aliquots of samples in brown vials (approx. 30 mg each) was added 1 mL of H2O, since they were thought to contain LiAlH4.  No reaction was observed.  2 mL of HNO3 was added and samples warmed to 90C for 30 minutes to digest solids.
   
   
3. The sample Vial 38 still contained fine greyish solids after digestion.  It was heated for a longer period of time (about 1 hour) at 90C and no progress was seen in the dissolution of the solids.  The supernatant solution was analyzed regardless.
   
   
4. The Ni carbonyl sample (112.2 mg) was digested in 2 mL HNO3, warming to 90C to speed the reaction.
   
   
5. All samples were diluted with water and the exact mass of solution measured.
   
   
6. Further dilutions were performed as needed using 3% HNO3, in order to make the concentrations of Li or Ni approximately equivalent to the concentrations in the standards.  Separate standards containing Li and Ni were prepared at varying concentrations.
   
   
7. The isotope ratios were measured using bracketing standards in several separate analyses using a PerkinElmer NexION 300X:
   
   Ni isotopes were measured at ~250 ppb Ni in KED (Kinetic Energy Discrimination) mode.
   
   Li isotopes in LiAlH4 were first measured at 1 ppm Li in standard mode, with the deflector lens detuned to keep the signal measurable by the pulse counting detector.
   
   Li isotopes were measured in LiAlH4 and the Vial 34, 38, 46 samples at 100 ppb Li in standard mode, with the nebulizer gas flow detuned slightly to keep the signal measurable by the pulse counting detector.  Consistent results were obtained for the LiAlH4 sample using both methods.
   
   
8. The general order of the analysis was standard-sample-standard-sample-standard-….  Each analysis consisted of 10 separate measurements of the signal at each mass.

The mass bias for each ratio was determined in each analysis of bracketing standard.  The average mass bias was used to correct the bracketed sample signals.  Each sample was run at least twice."

UPDATE#2 - Second Earthtech Ni Isotopic report agrees with University of Missouri results

https://goo.gl/tCMZ4g

Due to the unusual results from the first isotopic study by Earthtechs (ET) testing partners, where both Lithium and some Ni isotopes were studies, Earthtech commissioned another study from the independent testing lab. A separate portion of the blind samples sent was taken.

This time the results match those found at the university of Missouri (UOM), i.e. that Nickel was essentially natural isotopic ratio in all samples, fuel or ash.

The Independent testing lab said that trying to test for Li isotopes at the same time as some Ni isotopes most probably resulted in the unexpected results.

For the MFMP this is an easier result to understand, since whilst we still do not know which sample is which, the difference between UOM and ET did not inspire confidence in comparing analysis between different labs and techniques and also, was quite unexpected given the very short events that occurred in the GS3 runs.