Tuesday, September 24, 2013

Lab Update: Specialty Analytical

More news from Specialty Analytical

Specialty Analytical is analyzing the Mystery Oil from Vector and Newport (maybe Lucienne; see SPR) based on these 12 chemical compounds:

Isocyanato-cyclohexane
Isocyanati-cyclohexane
Butylated hydroxytoluene
2,4,6-trimethyloctane
10-methylnonadecane
6-propyltridecane
Tetratetracontane
Eicosane
Bis-2-ethylhexyldecanedioic acid
Carbonic acid phenyltetradecyl-
Tetramethylheptadecane
Hexadecane-1-ol


This list was supplied by Marty, Lab Director, at Specialty Analytical. 

Specialty Analytical said that all 12 compounds have been sourced and should arrive by weeks' end. The quantitative results should be available by October 7. This means that we will know, with more exactness, what the MO consists of. Thank you for your patience. BHO tests will follow.

Tuesday, September 17, 2013

News from Specialty Analytical

Just finished speaking with the chemist, Marty, at Specialty Analytical.

The TIC (Tentative Individual Compound) summary on the Newport and Vector 'Mystery Oil' (MO) is complete (the .pdf is at the bottom of this post). The TIC is a computer driven search-and-match based on GC/MS analysis and a database of 140,000 compounds. In total, the TIC produced around 460 potentially present compounds in the MO samples.

After reviewing the TIC, Marty is interested in an analytical analysis of 12 out of the 460 compounds found. Two that Marty mentioned specifically are cyclohexane based: isocyanate and isothiocyanate. These and the other 12 compounds produced what he called "a spectra that stands out." The TIC does give, as Marty verified, false-positives; however, for our purpose (identifying the MO in BHO), a manual review of all 460 compounds is not necessary.

With a more analytical/manual approach to Marty's "Big 12", the lab will be able to "positively identify" and give "quantifying amounts" of each as it relates to the MO. Unfortunately, the TIC does not produce this information. Therefore, the accompanying pdf. files are not final, in any respect.

Marty will be sourcing "pure samples" of each of the 12 compounds and then using each as a "standard" to identify and quantify with GC/MS analysis. Once identified and quantified in the MO, according to Marty, we should be able to identify these compounds in BHO.

In 48hrs Marty will have a timeline on acquiring, identifying, and quantifying these compounds.
Thank-you, Marty and the team at Specialty Analytical!

MysteryOil:Chromo.pdf

Saturday, September 14, 2013

Lab Update

Today I spoke with scientists at Specialty Analytical, Steep Hill Halent and Sunrise Analytical. These labs are currently working the MO samples in different ways. I am no chemist, so bare with me.

Specialty Analytical: My conversation with the chemist, AJ, was in regard to his confidence level in the test that Gray Wolf received (Lucienne) and the two that I will receive on Tuesday (Newport and Vector). AJ reiterated that the Tentatively Identified Compound (TIC) summary is based on an automated hit on a library of 100,000+ compounds. He verified that this test, because of its nature to create false-positives, will need "quantitative analysis" by a chemist. The chemist would be looking at those compounds on the TIC list and any compounds with indicating factors that stood out would become a focus (high "response time" etc.) Once a substance is identified as a possible 'suspect', a sample has to be purchased in its most pure form so that it can be used as a reference in both calibrating the GC/MS and then matching it to the 'suspected' compound in the MO. With a chuckle, AJ says that this is where "the real research begins, and where it gets real expensive, too." I look forward to my conversation with him on Tuesday.

Steep Hill Halent: This is a bit more of a 'wild goose chase; but, may yield some interesting results in the end. Travis, the chemist with Steep Hill Halent whose background happens to be in petroleum distillates, is using a combination of GC/MS and HLPC tests. Even though he has no idea what he is looking for 'structurally', (meaning the GC/MS is not calibrated for the MO or any of its compounds) he is able to see "unique peaks" when he runs the MO sample as if it were BHO and he was testing for either specific residual pesticides and solvents, or cannabinoid content (all three are different tests). One "peak" in particular that Travis says is "odd" is showing up clearly in multiple tests and he thinks that it will not interfere with any of the compounds (Cannabinoids, solvents, etc) that the machine is calibrated for. With a BHO sample he thinks he may be able to at least give us a positive identification of this peak in BHO. This will not have established the 'standard' that we are hoping for, of course. But it is fun science and Travis has been very kind to continue to try and educate me along the way. I will be delivering the BHO samples to Travis next week along with the TIC from Specialty Analytical.

Sunrise Analytical: Pat, the chemist with Sunrise, was kind enough to take interest in this project as well. He runs an analytical lab and will be joining the conversation further next week. He has lots to add.

Thank-you to all the chemists for their time and patience.

Wednesday, September 11, 2013

Lab Update

Specialty Analytical in Oregon has both samples of Mystery Oil (Vector and Newport) and is scheduled to deliver LSC results on Tuesday of next week. 

Several scientists have cautioned that the LSC test is merely a guide and provides only clues. My understanding is that an LSC is not definite proof of the compounds or their respective concentration levels (ppm/ppb). However, this test is a necessary first step and the scientist at Steep Hill is excited to have it.

Steep Hill Halent still has its sample of the Newport Mystery Oil and is continuing its investigation using different methods of analysis with GC/MS and HPLC. I expect to hear more from their scientist by weeks' end.

Next week, once the LSC results are in, I will be taking those and several BHO samples to Steep Hill Halent to continue the drive toward developing a 'standard' for testing BHO for Mystery Oil contaminants.

Thank-you again for your interest, your patience, and most of all, for sharing this with your BHO friends/family.

Wednesday, September 4, 2013

News from SteepHill Halent

Today's email communication with the chemist at Steep Hill Halent Laboratories:

Hi <Guys>,

I had a chance to discuss your data with another chemist. It definitely looks like a petroleum product. From the fragmentation in the mass spectrometer, we can say that some of the compounds contain alkane, cycloalkane and aromatic functional groups.

We're keenly interested in helping you learn more about this, but understand that research can be costly and time consuming. To minimize costs, I'd suggest that we can continue by running two of our other routine tests, GC-MS for pesticides, which won't show pesticides, but should give us better signal than the GC-MS residual solvent analysis, and an HPLC potency test, which uses an HPLC-MS using a softer ionization technique, electrspray ionization, than the GC-MS and may allow us to discover the molecular ion, instead of just looking at fragments of ions. The GC-MS test for pesticides is $120 and the HPLC potency is $100. I'd also like to include an hour of consulting time for data analysis at $200 per hour for a total of $420.

The additional routine test should give us some more information without the time and cost associated with developing new methods just for this analysis. If we're able to identify a unique peak using either of these analyses, that coul also be a starting point for verifying products are free of this mystery oil.

Please let me know what you think.

Regards, 
<Chemist>


---
I have ok'd the further testing and the chemist said that he would be performing the tests this week and should have all the information compiled by Tuesday.

I was also assured by one of Steep Hill's founders that it is their strong intention to get to the bottom of this as quickly as time and money would allow.

Thank-you for sharing.

Friday, August 30, 2013

Lab Update

I spoke with Adam, President, at Steep Hill Halent Laboratories in Oakland, Ca.

He assured me that the next step will be pinpointing the exact compounds within the two generalized groupings that the chemist found in his initial GC/MS 'mass fragmentation' analysis. 

Those groups were Linear Alkanes and Aromatic Compounds. 

The chemist working this project--whose background is in petroleum distillates--will be working the Mystery Oil sample on the GC/MS for a second time on Tuesday or Wednesday. And we should know more then.

Sorry for the slow progress; as I indicated originally, the Lab didn't think we would get to the bottom of this overnight.

Thank-you for your continued patience and interest and input! Everyone has been great!

Thursday, August 29, 2013

News from Newport/Keen

EVIDENCE FROM THE SOURCE!

Newport says their cans contain "oils, waxes, charcoal dust, etc." at less than 50ppm. 

I received a follow-up email from Newport/Keen "Near Zero Impurities", Managing Director, Paula Hussain. She states that the cans have 50ppm or less of "oil, wax, charcoal dust etcetera".

However, it is all relative to the amount of BHO that is produced from one can.

From what I know, one can produces around 4grams of BHO.

If each can contains Ms. Hussain's stated ppm of 50, then that leaves .015grams of these "impurities" per 10oz can.

.015 grams of impurities in 4grams of BHO equals 3,750ppm.

IF ALL the impurities are in the end-product, that is high!

Here is her entire response to my question about the 'Mystery Oil'--

"Traditional refineries produced butane propellant with an uncontrolled non-volatile content of impurities including oil, wax substances, charcoal dust etcetera which was not a problem for filling lighters until 1983 when the so-called "flameless" heat-generated turbo lighter was invented in Japan. In order to market this lighter it was established that the non-volatile impurity content of the butane could not exceed fifty parts per one million parts. Our company was assigned this problem which enabled the inventors to market the new product by 1985. Since then numerous diversifications of the concept have appeared. Our exclusive "Near Zero Impurities" has been included on all butane refills that we produce to differentiate our butane refills from all others."

Regards,
Paula Hussain
Managing Director


1 Northbrook Street
Newbury
Berkshire RG14 1DJ
England
Telephone: 44 (0) 1635 34600
Fax: 44 (0) 1635 33360

www.keen-newport.com