Author Topic: Not sure what's happening  (Read 1968 times)

tony14

  • Guest
Not sure what's happening
« on: February 05, 2019, 02:38:31 PM »
After my last batch (20ppm; 10mA; 20 drops electrolyte; 3 drops Golden Syrup 50:50; 25degC; 30mins stirred) The batch looked clear in torchlight (wide beam) and stirrer turned off when I spent some 1 hour on the Forum.

I then noticed it was full of wispy 'strands' like cobwebs, with a definite deposit on the bottom. (AG2O?) (There is a label under base)
These 'strands' were very pretty, looked almost solid and very, very, very slowly dispersing. Hard to photo but images attached.
Should this happen?
I'll recheck in the morning.
I never let previous batches sit for such a time and looked with the torch, just filtered and decanted into another container.

tony

Offline Neofizz

  • Expert
  • Participant
  • ***
  • Posts: 1127
  • Likes: 65
Re: Not sure what's happening
« Reply #1 on: February 05, 2019, 03:03:53 PM »
I'm not sure if this is what is happening but you should remove the electrodes as soon as the run is done. Otherwise, you have a battery now that will do it's thing which could cause some problems. This could be why you are seeing what you are seeing.
"Be kinder than necessary, for everyone you meet is fighting some kind of battle."

tony14

  • Guest
Re: Not sure what's happening
« Reply #2 on: February 05, 2019, 03:29:23 PM »
This could be why you are seeing what you are seeing.
The cell was o/c so no current flowing, but, yes, I normally remove electrodes and lid it. Think it was Gene said the oxide minute. a mirror-finish but what's in the bottom isn't and white. Think it never reduced properly but it's first time left for so long before decanting.

Just given it a stir and perfectly clear? It does reflect the torch at 90degs to the beam, one can see the actual torch LED's path in the beam in the solution - er (hopefully) colloid?

tony

tony14

  • Guest
Re: Not sure what's happening
« Reply #3 on: February 06, 2019, 03:04:32 AM »
This could be why you are seeing what you are seeing.

Just given it a stir and perfectly clear? It does reflect the torch at 90degs to the beam, one can see the actual torch LED's path in the beam in the solution  suspension? - er (hopefully) colloid?

This morning it was perfectly clear and on shining the torch the beam was quite noticeable 90deg, 1nm > colloid < 1000nm? When decanted there was no deposit in the jar base - it was the LABEL - stuck under, refracting somehow! It's removed.

My guess is that full reduction never happened. When stirring ceased reduction continued and possibly due to temp increasing up container vertically, reduction occurred upwards producing the whispers??

Again, to my ageing mind, (still trying to understand the mix of: small +Agions; large -AgNS; unprecipitated Ag2O; ? -- have to re-read) the unreduced +Ag ions, surrounded by the mixture take a path 'forced' by something or thermally carried by the liquid? When each one finds sugar (?) it  reduces to a -AgNS clump that disperses due to like charges so the whisper is just the path of reduction?

It's sort of like learning transistor theory - an electron moves leaving a hole and the hole actually moves slower than the electron that left it - yeah, mate!

Has anybody seen these 'whispers' in a solution carrying no current? What are they? And is it safe to use?

tony

tony14

  • Guest
Re: Not sure what's happening
« Reply #4 on: February 06, 2019, 08:51:43 AM »

Quote
What is an AgNS? What is a -AgNS?  These are meaningless terms with no relevance to chemistry of silver nanoparticles.  There is no nitrogen or sulfur in the process.
Sorry, I was reading a paper about nanoparticles in Pseudomonas aeruginosa and they used these terms. I just carried them over without thinking. [Probably my age? :-)]

Quote
What is your electrode spacing, and what was your voltage?

Electrode spacing was/is @ 37mm. Electrode voltage I call Vcell was 13v. This wasn't set. I use a constant current generator set to 10mA and initially wasn't concerned about the electrode voltage providing > 10v. I check the constant current generator and it is correct. Electrode voltage does however matter even with a constant current generator as I note below.

Just ran again but set electrode voltage to 17v (was 13v) by changing depth of cathode. The constant current generator open-circuit voltage is 19v and when shorted is 10mA. 

Parameters: DW 1000ml; 20 drops Electrolyte made as per your instructions; Reducer: 3 drops Golden Syrup 50:50 in DW; Temperature: 25C; 30mins timed; daylight but no direct sunlight (not in fluro-lit room)

Removed electrodes, lidded then waited, still as before on stirrer. Colour now different,  still yellow but ‘seems’ shinier? Don’t know how to put it?  It just stayed very clear even though the ‘whispery’ batch did also.

No laser yet but torch showed I had been making big-particle stuff if my Tyndall interpretation correct? (Overcooked?)

So I’m guessing it’s what should be made, @ 20ppm, 14Nm? So, it’s even important when using a constant current generator to have a high voltage. Why?  High voltage at a constant current= increased density of current that helps any slow reduction process?

Should I junk the batch already made? Thanks, WG.

tony
« Last Edit: February 06, 2019, 11:40:27 AM by tony14 »

tony14

  • Guest
Re: Not sure what's happening
« Reply #5 on: February 06, 2019, 12:32:28 PM »
Quote
Why?  High voltage at a constant current= increased density of current that helps any slow reduction process?
No, current density depends only on current.  Voltage is what drives the newly created silver hydroxide out of the anode by attracting OH ions into the anode.

It sounds like your setup is correct, although I would use more golden syrup.  More does not hurt.

If you continue to have trouble (whisps), I would check the purity of your distilled water, and verify the purity of your anode.

Thanks WG. Makes sense. Distilled water is steam distilled and anode is 1oz ingot 99.99 stamped. Always flame it. Holding Ag wire, 2mm also 99.99. Changed from flat brass strip to silver cathode as round hole easier to make.

tony

tony14

  • Guest
Re: Not sure what's happening
« Reply #6 on: February 06, 2019, 01:27:09 PM »
It sounds like it is down to your distilled water.  I bought a gallon of distilled water from my local grocery store 2 weeks ago, and it would not make good colloidal silver.  It had very high Tyndall, and did not reduce properly.  I made another batch with a different brand of DW, and it was perfect.  I went back to the DW that did not work properly, and again the batch turned out very bad.  So it always pays to check with a different source of distilled water.

Fascinating! The distilled water measures 0ppm/pH 7.5 (not totally sure, calibration)/0 uS/cm. I only got it because it said 'steam distilled.' Change supply tomorrow and hope laser arrives. White light still shows a mild Tyndall in this latest batch but nowhere near as bad as the first batches where electrode voltage was 13v.

Thanks WG.

tony

tony14

  • Guest
Re: Not sure what's happening
« Reply #7 on: February 10, 2019, 03:22:23 AM »
Good luck.  Let us know your results.
I used the last litre to make a batch at 5mA; 17v; 20ppm; 20 drops; 4 drops GS; 25C; 60mins and no different than before except the anode & cathode deposits seemed much thicker and looked 'liquid,' lots of hydrogen (H?) bubbles.

I checked the dropper as advised on the Forum and surprised a 'cooking' teaspoon was filled with 45 drops! So my 20 drops excessive will use 10 drops in future. Electrolyte made as per advice.

Got different DW and made a batch of 1L 20ppm.  As temp here had fallen I heated it to 30C and used 10 drops electrolyte; 4 drops GS. Had to readjust the cathode depth to get 17v (was 18v - less conductive).  10mA. (CC) Cathode 'bubbling' seemed far less than before and there was no 'stream' of bubbles from the twirling base magnet. All my previous runs had a streamer from the twirling magnet like individual small bubbles that meandered to the surface at the spot where slight cavitation appeared sometimes. Final product as before, very golden-looking yellow. Laser not here yet and confused when using white light, get 'bluish' emission in the jar.

Next run no different so I waited about an hour then ran again. Temp fallen to 22C being the only difference. Think I have 40ppm? Image attached, still trying to find best way of photoing using old Kodak C633.

Going to try cinnamon. See post Silver Forum.

tony

tony14

  • Guest
Re: Not sure what's happening
« Reply #8 on: February 12, 2019, 08:06:05 AM »
Good luck.  Let us know your results.

Apologies, a bit lengthy: All 20ppm batches made so far I have thought good. They are very clear, yellow, and maybe 'too' yellow - shine like gold, taste like water. Then the laser arrived and everything awry, shows a noticeable Tyndall!!

Equipment: DC variable constant current (CC) source with mA display + 24v DC mains powerpack supply for it (Manufacturer assures pure DC not PWM.) 2 Multimeters (confirm each other & DC mA on display true) Magnetic stirrer/hotplate (don't use hotplate yet - tried it and 1L water over desk. :-) duh!) 2mm dia K; 1oz Ag ingot both certified .9999; holding jig is a PVC lid, electrodes 37mm apart.

Components: Electrolyte: made by heating baking soda in heatproof glass pan for @ 1 hour, cool, measure 10gm, dissolve into 100ml DW.

Reducer: Golden Syrup 50:50 with DW (2 tablespoons of each); Calibrate dropper - 45 drops into teaspoon/5 =9 drops/litre (started with 20d/L until calibration)

Cleaning with DW, fingers always kept away from things.

Method history: Temp always @ 24C; Initially used 1L DW, 10mA 30mins; ingot 50% in; adjust K depth for Vcell=17v (I originally used a brass strip K, 3mm wide and got Vcell-12v. In this condition at 10mA there were wisps flooding from A so I reduced K depth until they went and it seemed 17v Vcell optimum so I always set K depth for this. Open circuit CC generator is 19v.)
=========
Last run: 0.6L DW (steamed, stirred) TDS ppm=0; pH=7.8; temp=24.7C; Slight Tyndall in daylight;
Add electrolyte, 6 drops & 1d GS; - Tyndall unchanged.

Insert, connect-up electrodes, ingot 7/8 immersed, start & time for 18mins, raise/lower K for 17v Vcell. (10d electrolyte for 1L 6d for .6L) Only viewed action bubbles swirling around.
Very clear result - no cloudiness but Tyndall getting stronger.
Remove electrodes, lid on, ingot face white oxide, edges black oxide, K plateout negligible - faint black when wiped with paper towel.

Tyndall slowly increases. Image taken @ 1/2 hour wait. Tyndall is brighter than image achievable.

NOTE: I did one run prior to the above everything exactly same but reducer added AFTER 18mins. At 18mins the Tyndall was noticeable but got much stronger after adding the GS.

I'm doing something wrong, where? Some batches made under fluro at evening, others day in relatively shaded room.

Any advice please? I must be doing something soppy :-( [Oz Gravity? UK MOD did tell me Oz mV different to UK mV?? Nah! Got something wrong, can't see it.]

Just batched as above, 200ml; 20ppm; 10mA; 17v; 6 mins; 2d electrolyte; raised temp to 40C at start. GS smeared on tissue - guess, added after run. End of run slight Tyndall but after adding GS, 1/2 hr later Tyndall quite noticeable as yellow appeared.

tony


Offline kephra

  • The older I get, the better I was
  • Administrator
  • Participant
  • *****
  • Posts: 8883
  • Likes: 286
  • Illegitimi Non Carborundum
    • My World As I See It
Re: Not sure what's happening
« Reply #9 on: February 12, 2019, 11:16:18 AM »
Tony,

Your Colloidal Silver actually looks quite useable.  The object is to minimize the Tyndall effect, but its almost impossible to eliminate it entirely. 
There is the unknown and the unknowable.  It's a wise man who knows the difference.

tony14

  • Guest
Re: Not sure what's happening
« Reply #10 on: February 13, 2019, 01:24:58 AM »
Tony,

Your colloidal silver actually looks quite useable.  The object is to minimize the Tyndall effect, but its almost impossible to eliminate it entirely.

Thanks, Kephra. [Goes cross-eyed - :-) ]

Fascinating!
Yesterday, when I made a 1L batch, (ionic,) no GS, very slight Tyndall,  I immediately decanted 125ml into a cloudy-clear plastic container used to infuse into dog ears and 200ml into a brown spray container from "My Colloidal Silver." [The latter was some months old and was always clear, TDS 20ppm[?] and thrown away to decant.]
Both containers washed thoroughly before decanting. The brown one sits on the table and gets sunlight through the window, although not directly. The clear one sits in a wool bag on a shelf out of light but not dark.

Both had gone very light yellow BUT, the clear bottle ionic-now-Colloidal Silver mix [?] showed virtually no Tyndal but the brown bottle contents showed Tyndall as seen in all my batches? Go figure?

Tyndall: when I red-laser view this as being 'good' I see almost 'stranded' multiple red micro-diameter beams that sparkle as larger particles move in and out. Beams are subjectively distinct.
As the particle diameter increases it 'seems' many more micro-beams are produced that coalesce such that the total reflection seems to be one beam of greater intensity. I thought this bad but to me, it makes sense in that the micro-beams accumulate on incidence with a larger particle so make Tyndall stronger. Only a subjective concept.

So far the dog's been drinking Colloidal Silver for 4 days and I have been washing her ears out with it. She still shakes her head but no exudate or debris is apparent when cleaning the ears. Just need to check it's not building-up inside so a vet visit needed.

Thanks again Kephra.

tony