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Am I Done For? (Manske)

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aliendreamtime

aliendreamtime

Rising Star
Hi,
A friend of a friend used salt with the anti caking agent calcium silicate for a manske precip.

A concentrated vinegar/harmala extraction was made by boiling and immediately basifying 5 seperate washes of whole rue seeds. The precipitates were collected by decanting, combined, washed with water to pH ~8 and acidified with vinegar. Solids were decanted and the final solution was filtered once with an exceptional coffee filter.

A saturated salt solution (equal to the volume of the harmala/vinegar solution) was prepared and added to the harmala/vinegar.

After cooling to room temp and now in the fridge for a few hours...no precipitate.

Turns out the salt ingredients include calcium silicate.

Should he re-basify to recover harmalas and try again with pure NaCl?

Can I try adding more NaCl, maybe that's the problem?

Input is appreciated, thanks folks!
 
AFAIK the anti caking agent is harmless and present in low concentration anyway.

Give it some time. Or stir the cooled solution, taking care to slide the stirring implement firmly against the container walls, that usually helps to create nucleation sites.

If nothing works, boil the solution again until it has reduced to half its original volume and then let it cool again.
 
Thanks Pitubo,

Based on the Tao of Rue, dilute solutions = bigger crystals so he was going for that. I'll pass on the message, maybe update on the results.

Is is possible that Ca2SiO4 appreciably reduces NaCl solubility in water? Seems doubtful.

Thanks again!
 
Thanks for the help pitubo!

He took your initial advice and reduced to about 1/2 volume (final volume was slightly less than half the original volume) and allowed to cool. That produced plenty of precipitate in the form of red/br needles and flakes.

On the second Manske he added 10g NaCl / 100ml harmaloid solution to about 475ml harmaloid solution. However, a white precipitate formed after dissolving the NaCl in the harmaloid solution, which was filtered. More hot water was dded to the filtered precipitate, but no dissolution occurred. He thought that perhaps the solution was not hot enough when addding the salt, causing early precipitation. After filtration, the particulate appeared to be white/grey and maybe 1/20th the size of salt granules (quite fine, like silt).

Based on the solubility of the anti-caking agent in the salt (Ca2SiO4, being 0.01% solubility according to Wikipedia) I gather that:

0.01%/100 = a factor of 0.0001. 0.0001 x 1L would give a solubility in g/L of 0.1g/L (100mg/L).

Compar that with with NaCl solubility of 359g/1000g water (given that 1,000 ml H2O = 1,000 mg H20) having a solubility of 359g/1000g x 100 = 35.9%. So we can be sure Ca2SiO4 is quite insoluble compared to a readily soluble salt like NaCl (0.01% compared with 35.9%). I think the amount of Ca2SiO4 in solution probably precipitates before the harmalas or NaCl, which would explain the fine, greyish precipitate, or may not fully dissolve entierely to begin with, if using 10g salt/100ml solution (package doesnt say how much Ca2SiO4/g NaCl).

Conclusion: If using salt with the anti-caking agent Ca2SiO4, one would need to filter the solution subsequent to adding the salt, prior to cooling as there will be some CaSiO4 precipitate in the vessel prior to precipitation of harmine/harmaline after cooling. Na4SiO4 is fairly soluble (22g/L @ 25C), so it shouldnt be preipitating I think.

Comments anyone?
 
You could make a saturated salt solution and let the less soluble impurities precipitate on slight cooling. Then decant or filter.

Personally, I prefer to use dishwasher salt, as it is usually much more pure than table salt. The only downside is the bigger chunks dissolving slower.

Oddly, wikipedia states that dishwasher salt contains 5% additives such as anti-caking agents. It gives no references for that claim and it sounds not very sensible to me. This link does state that dishwasher salt is more pure than table salt. The products that I find at my local supermarkets are very pure and cheap.
 
pitubo said:
You could make a saturated salt solution and let the less soluble impurities precipitate on slight cooling. Then decant or filter.

Personally, I prefer to use dishwasher salt, as it is usually much more pure than table salt. The only downside is the bigger chunks dissolving slower.

Oddly, wikipedia states that dishwasher salt contains 5% additives such as anti-caking agents. It gives no references for that claim and it sounds not very sensible to me. This link does state that dishwasher salt is more pure than table salt. The products that I find at my local supermarkets are very pure and cheap.
Click to expand...

Pickling salt works pretty well also. Apparently iodide makes for a cloudy pickling solution & anti-caking agents make for dark pickles so both are left out.
 
concombres said:
pitubo said:
You could make a saturated salt solution and let the less soluble impurities precipitate on slight cooling. Then decant or filter.

Personally, I prefer to use dishwasher salt, as it is usually much more pure than table salt. The only downside is the bigger chunks dissolving slower.

Oddly, wikipedia states that dishwasher salt contains 5% additives such as anti-caking agents. It gives no references for that claim and it sounds not very sensible to me. This link does state that dishwasher salt is more pure than table salt. The products that I find at my local supermarkets are very pure and cheap.
Click to expand...

Pickling salt works pretty well also. Apparently iodide makes for a cloudy pickling solution & anti-caking agents make for dark pickles so both are left out.
Click to expand...

I concur. I use Morton's Canning and pickling salt. I got a 4 pound box for like 5 bucks at walmart.

8)
 
The Grateful One said:
concombres said:
pitubo said:
You could make a saturated salt solution and let the less soluble impurities precipitate on slight cooling. Then decant or filter.

Personally, I prefer to use dishwasher salt, as it is usually much more pure than table salt. The only downside is the bigger chunks dissolving slower.

Oddly, wikipedia states that dishwasher salt contains 5% additives such as anti-caking agents. It gives no references for that claim and it sounds not very sensible to me. This link does state that dishwasher salt is more pure than table salt. The products that I find at my local supermarkets are very pure and cheap.
Click to expand...

Pickling salt works pretty well also. Apparently iodide makes for a cloudy pickling solution & anti-caking agents make for dark pickles so both are left out.
Click to expand...

I concur. I use Morton's Canning and pickling salt. I got a 4 pound box for like 5 bucks at walmart.

8)
Click to expand...

Makes extraction seem inconspicuous as well 😁
It looks completely normal to have some extraction items like:
Pickling salt, pickling lime, jars, pressure cooker, different powdered acids, etc. Due to the fact it all fits together in a single nice category like canning/pickling.
 
I've recently run into a similar issue, mine isn't from salt I would suspect. I reduced my liquid by a 1/3, filtered added pickling salt and left to cool. Now I have a yellowish tinged sludge formed on the bottom and a gelatinous layer on top maybe 1/8 inch thick.

It all came from the same batch so I'm not understanding what it is. I'm gonna reheat and dissolve again to see what happens. Does ph cause this? Wreaks of vinegar so I'm sure it's acidity is good. Used 10g salt per 100ml. Did I reduce it too much? The other batches (done in 1/3s) where fine and ended up with 25g of hcl xtals.

Again not sure what's going on with this one, only thing I done differently was reduced it before adding salt.

Any thoughts or ideas?
 
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