Author Topic: Dis ASM, he mighty pow'ful magic! (or ... have I witnessed a reverse reaction) (Read 21050 times)

nathanrobo · « **Reply #30 on:** January 15, 2013, 01:09:41 AM »

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Now, ask me if I'm short of soap!
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Julian... r u short of soap?

K.H · « **Reply #31 on:** January 15, 2013, 07:16:05 AM »

Have you checked the methanol?

Julian · « **Reply #32 on:** January 15, 2013, 11:26:21 AM »

Quote from: K.H on January 15, 2013, 07:16:05 AM

Have you checked the methanol?

It's on the list of things to check, but I've no reason to suspect it ... newish drum from known supplier, well sealed, stored in warm dry garage, and has not given any problems in the past.

Julian · « **Reply #33 on:** January 15, 2013, 03:10:24 PM »

Ok, checked my Methanol (gave me the opportunity of some photos for the wiki page I started many months ago!)

Methanol SG is 0.805 @ 10.2°C.

My chart only goes down to 11°C, but that gives 98%. At a lower temperature the purity would be higher so at a guess it must be around 98-99%.

julesandtash · « **Reply #34 on:** January 15, 2013, 03:38:11 PM »

I suspect that if you methanol was bad, the Dr Pepper sample would have behaved in the same way as the full batch.

Something has got to be happening in the processor that shouldn't be. Is the circulation OK (not a partially blocked pump or similar).

Julian · « **Reply #35 on:** January 15, 2013, 04:06:44 PM »

No blockages. I've got a pressure gauge on the pump discharges (where they are common) and any blockages down stream show up on the gauge. And besides I'm overly cautious of what I put in the processor. The oil is either visibly clear or is filtered through landscaping fabric ... not sure of the micron size but it's quite fine.

The Dr Pepper was only a small sample ... ½ a jam jar, so that could be a reason in it's self, but after some thought the major differences between the Dr Pepper and the batch is copper and temperature. Dr pepper saw no copper, the batch saw lots. The batch was processed at around 60°C and the Dr Pepper was probably down to around 30 - 40°C by the time I tested it.

Anyone else using ASM with a copper processor and pipe work?

julesandtash · « **Reply #36 on:** January 15, 2013, 04:26:02 PM »

Afraid not, mine is stainless steel with iron pipework and fittings. I would not have thought that copper would have that much effect but I guess anything is possible. Maybe try a doctor pepper with a piece of copper in the jar?

Julian · « **Reply #37 on:** January 15, 2013, 04:51:56 PM »

That was exactly my intention. Got ideas for a series of Dr Peppers which I'll post for comments shortly.

william crosby · « **Reply #38 on:** January 15, 2013, 05:50:07 PM »

Julian

you mention copper and asm.I noticed something very strange with the barrel pump i made from copper the asm turned it jet black.Could this be some sort of reaction.

Julian · « **Reply #39 on:** January 15, 2013, 06:04:51 PM »

If I was anything of a chemist I'd stand a fighting chance of answering that and solving the problem I have!

As far as I know when copper oxidises it goes that nice verdigris colour, and that I assume is a reaction with Oxygen.

I guess it's quite possible some alternative reaction happens with ASM. Me thinks an experiment of copper in a high concentration of ASM is called for. I'll pickle and wash the copper first to make sure it's clean.

1958steveflying · « **Reply #40 on:** January 15, 2013, 06:37:53 PM »

Quote from: Julian on January 15, 2013, 06:04:51 PM

If I was anything of a chemist I'd stand a fighting chance of answering that and solving the problem I have!

As far as I know when copper oxidises it goes that nice verdigris colour, and that I assume is a reaction with Oxygen.

I guess it's quite possible some alternative reaction happens with ASM. Me thinks an experiment of copper in a high concentration of ASM is called for. I'll pickle and wash the copper first to make sure it's clean.

Surely it is not the effect of ASM on copper you are looking for but the effect of copper on your reaction using ASM.
ASM at the end of the day is the same as Sodium hydroxide in methanol but without the water. Perhaps if you email Graham Laming he may know.

1958steveflying · « **Reply #41 on:** January 15, 2013, 06:45:26 PM »

Just read this
"Conventional sodium methylate manufacturing processes typically employ mercury-sodium amalgam in the electrolysis process, which could potentially contaminate suppliers’ grades with trace quantities of mercury. In contrast, the unique manufacturing process for DuPont™ Sodium Methylate in the U.S. incorporates innovative technology that virtually eliminates traces of mercury and enhances product purity"

Could our ASM have traces of Mercury that maybe gives rise to problems?

Julian · « **Reply #42 on:** January 15, 2013, 07:17:59 PM »

Quote from: 1958steveflying on January 15, 2013, 06:37:53 PM

Quote from: Julian on January 15, 2013, 06:04:51 PM
If I was anything of a chemist I'd stand a fighting chance of answering that and solving the problem I have!

As far as I know when copper oxidises it goes that nice verdigris colour, and that I assume is a reaction with Oxygen.

I guess it's quite possible some alternative reaction happens with ASM. Me thinks an experiment of copper in a high concentration of ASM is called for. I'll pickle and wash the copper first to make sure it's clean.

Surely it is not the effect of ASM on copper you are looking for but the effect of copper on your reaction using ASM.
ASM at the end of the day is the same as Sodium hydroxide in methanol but without the water. Perhaps if you email Graham Laming he may know.

Good point, the Dr Pepper with added copper should highlight any problems, but as ASM is the major change to test it directly with copper can't do any harm, especially in the light of what William says above.

Julian · « **Reply #43 on:** January 17, 2013, 08:02:48 PM »

Looks like I might have some bio at last!

I filled the process with water, heated and circulated in an attempt to remove any residual soap. Rinsed out the Methoxide mixer with fresh Methanol. Dried 80 ltrs. of really good oil to over 100°C and processed using a two stage titrated process which gave a 3/27 with colour but no dropout after half an hour of the second stage. Recovered just over 5 ltrs of Methanol and the Glycerin is settling as I type. I'll drain the lower pipe work later and settle further over night ready for an acid wash tomorrow.

So, Dr Peppers I intend to do are as follows ...

1) The oil I used today with ASM from drum 1.
2) The oil used in the previous failed batches with NaOH, titrated.
3) The oil used in the previous failed batches with ASM from drum 1 and several pieces of pickled Copper
4) The oil I used today with ASM from drum 2( (subject to friends daughter drinking enough pop to get me another test bottle!)

Can anyone think of any other meaningful test that can be carried out?

1958steveflying · « **Reply #44 on:** January 17, 2013, 08:17:56 PM »

Quote from: Julian on January 17, 2013, 08:02:48 PM

Looks like I might have some bio at last!

Dried 80 ltrs. of really good oil to over 100°C and processed using a two stage titrated process which gave a 3/27 with colour but no dropout after half an hour of the second stage.

What were the numbers Julian.
1, Ml of ASM stage 1
2, Ml of ASM stage 2
3, Methanol amount for each stage.
And was this fresh Meth and fresh ASM ?

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Dis ASM, he mighty pow'ful magic! (or ... have I witnessed a reverse reaction)