Sciencemadness Discussion Board - How is amalgamated Al supposed to look like?

How is amalgamated Al supposed to look like?

KidCurry - 2-8-2005 at 04:10

Tried amalgamating Al with Hg2Cl2 in boiling water a week ago, but it didn't turn to a grey slush with Al bits in it (like all the pictures in the Rhodium archive). The aluminium just became slightly less shiny, and the water became a bit clouded. Does this mean the amalgamation failed?

Organikum - 2-8-2005 at 11:49

The Al becomes dull grey. The amalgamation is ok when the overall surface is equally dull.

KidCurry - 2-8-2005 at 12:51

This is what it looked like (looks quite dull).
But theoretically it's reducing power was minimal, and the reduction of nitrostyrene failed. Some of the aluminium reacted tho with the aid of external heating, but a very strange brown guck with tar formed when basifying after 2 hours. The IPA and water layer didn't separate either. I can't think of anything that could have gone wrong except the amalgamation. It's really a straight forward reaction. How long does it usually take to amalgamate for example 20g of Aluminium? SWIM boiled the Al for about 30 minutes and thenlet it stand for another 30.

[Edited on 2-8-2005 by KidCurry]

[Edited on 2-8-2005 by KidCurry]

[Edited on 2-8-2005 by KidCurry]

al.jpg - 100kB

bio2 - 2-8-2005 at 13:40

........ How long does it usually take to amalgamate for example 20g of Aluminium? SWIM boiled the Al for about 30 minutes and thenlet it stand for another 30. ........

It takes only 10-30 minutes to amalgamate any amount at ambient temperature. Boiling would be almost instant. Either the Al is no good or not enough HgCl2 perhaps.

Make sure no coating and clean Al surface. Dissolve a little in 5% NaOH and see what residue there is left. Should only be a little black residue (Fe) and a very little white (Si)
in the almost clear solution.

KidCurry - 2-8-2005 at 13:45

It was amalgamated with Hg2Cl2, hence the boiling since the low solubility. Will check out what happens when the aluminium reacts KOH (no NaOH avaible).

bio2 - 2-8-2005 at 13:46

In the picture it seems the Al is folded too tightly. Both the amalgam solution and the substrate being reduced must contact the entire surface area for the time required for the thickness Al used.

If you rinsed it, this is not required, it has to stay out of air contact until use!

Fleaker - 2-8-2005 at 14:06

Bio, I don't think they add silicon or iron to aluminum for use in foil production. Most alloys for extrusion and rolling don't have silicon (which is added to improve its qualities in castings) in them because it makes them more brittle.

KidCurry - 2-8-2005 at 14:23

Bio2: I think you've found the problem. Unfolded one of the unreacted bits of aluminium, and it looked nearly intact inside. :/ Better luck next time.

Rosco Bodine - 2-8-2005 at 14:58

You need to be using the highly soluble

Mercuric Chloride for amalgamation ,

not the difficulty soluble mercurous salt .

Mercuric nitrate should work well too .
Dissolve a little mercury in a slight excess amount of moderately concentrated nitric acid , do this outdoors or in a fume hood . Dilute and decant and save the mercuric nitrate solution and use it directly for the amalgamation . Never tried it this way , but can't see any reason why it shouldn't work fine .

KidCurry - 2-8-2005 at 15:12

The mercurous salt works fine for amalgamation according to very reliable sources (including prominent members of The Hive). Just takes a little bit longer. Obviously some of the aluminium was amalgamated, the problem is probably as bio2 said that the Al was folded hardly minimising contact area. HgCl2 & co are highly toxic, and hard to get where SWIM live so I'll rather avoid them if I can.

[Edited on 2-8-2005 by KidCurry]

KidCurry - 3-8-2005 at 01:12

This is what's left after letting a piece of aluminium stand in a solution of KOH overnight. Some black/brown solids and it has a yellowish tint. Maybe the aluminium was bad too?

alkoh.jpg - 92kB

KidCurry - 3-8-2005 at 06:12

SWIM was at the store, and checked out the different brand of aluminium foil. The same brand that made the pie form SWIM tried to amalgamated claimed that their foil was an alloy. So SWIM bought another brand of foil, dissolved it in aqueos KOH and it left nothing but a clears olution. SWIM tried amalgamation, worked flawless. SWIM will try the reduction another day!

[Edited on 3-8-2005 by KidCurry]

Bullshit!

KidCurry - 3-8-2005 at 07:36

The amalgamated aluminium doesn't react either. Something is seriously wrong here. SWIM tried starting the reaction with heat, doesn't work. :mad:

Tacho - 3-8-2005 at 08:41

1- a spatula tip of Hg2Cl2 (calomel) in a test tube.

2- add 1ml HCl 37%

3- add 1ml H2O2 as concentrated as you can get. I used 30%, but I gess 10% would work

4- Put a cottom plug on top of the tube -heat on a small flame, don't boil it - a vigorous reaction (bubbling) takes place - be carefull with the spray (mist) comming from it, it has very poisonous mercuric chloride in it, hence the cottom plug.

5- the crystal clear solution left (no calomel precipitate) is a mecuric chloride solution. Insert a piece of clean copper wire in the solution(thanks Polverone). It should come out silvery because it's coated with Hg.

6- Use "as is" diluted in water or neutralize first and get rid of the excess H2O2 with manganese dioxide. I use my marvelous catalyst to do it. Don't forget the cottom plug here.

I never amalgamated al, but I made zinc amalgam very successfully.

I hate working with mercury salts. I have no intention of working with them again. I don't care what people say, everything just feels dirty and contaminated. Are you sure your reduction won't take place with plain HCl + zinc powder in GAA? Try it in small scale. You may be surprised.

And please stop writing in "SWIM" fashion. This is not that forum.

Organikum - 3-8-2005 at 09:05

The Al in the picture looks much too shiny for my taste. Check your Al and your mercury salt.

My Al wire amalgamates nicely with elemental mercury alone overnight, with any salt in minutes.

Is the Al pure?
Is it clean?
Have you done the right incantations?
Did you do your sacrifice?

questions over questions....

KidCurry - 3-8-2005 at 09:20

Organikum: The new Al was clean, looked much more amalgamated (with grey slush).

When the reaction didn't start, I took all the Al I hadn't added together with the reaction solution + the aluminium in it and put it in a large plastic bottle and shook it like hell. And it worked! The Al started to react, and the deep red/orange solution turned to grey and heated up just like it should.

Tacho: Zn/HCl would certainly reduce it, but I wanted to try something I haven't done before. (Also the addition of zinc is quite tedious when reducing more than 5g).

Organikum - 3-8-2005 at 11:04

hehe...
I once did something similar, filling some shit to react into a plastic bottle and shake the hell outa it. Did react. Got hot. Just the fucking PET bottle didn´t like the heat and started shrinking like PET bottles do when heated. Was quite the disaster...

Just an anecdote.

KidCurry - 3-8-2005 at 13:18

Organikum

This was made of PE-HD so the heat wasn't really a problem even tho it got so hot it couldn't be held with bare hands. But it payed off:

succ.jpg - 108kB

bio2 - 3-8-2005 at 22:17

.........Bio, I don't think they add silicon or iron to aluminum for use in foil production. .......

It is not intentionally added but all 99%+ Al (including foil) has Si and Fe as the main impurity. Check material web for alloy compositions.

Kid Curry try making methoxide or the ethoxide with the Al so not to waste the precursors. This is what I did when having trouble finding good Al.

Add 20ml/g MeOH anhydrous to the Al amalgamated in just enough MeOH 2% HgCl2 to cover or 15-25mg/g if it needs more than 2ml/g to cover and it should react almost right away and when slows then reflux until all dissolved. They say a crystal of I2 is needed but mine reacts w/o any catalyst. Just make sure the alcohol is really dry (anhydrous) or the Al just reacts with the water incompletely.

12AX7 - 4-8-2005 at 05:23

Actually foil has about 1% Fe and 1.5% Si, IIRC. Helps with the rolling or something, and you can't blame them, that's a lot of rolling from a foot thick billet

The real pure stuff is aluminum wire, either 99% or 99.99% (1199 alloy). Mine forms crystals on the surface like lead of similar purity.

Tim

Al alloys

bio2 - 4-8-2005 at 16:12

Al foil is series 1000 alloy which is 99+% depending on the particular alloy.
http://www.matweb.com/search/GetComposition.asp has some good info.
Granted, the word foil sure doesn't mean its 1100 H-14. H-19.

Surprisingly, to me anyway, the common soft Al is usually 1000 series alloy which is all 99% or better.

Everything you ever wanted to know about aluminum is here
http://www.aluminum.org/template.cfm?Section=Aluminum_Associ...

This is some stuff I compiled to use in the quest for the good shit.
......................................
The 1xxx series represents the commercially pure aluminum, ranging from the
baseline 1100 (99.00% min. Al) to relatively purer 1050/1350 (99.50% min. Al)
and 1175 (99.75 % min. Al).Some,like 1350 which is used especially for
electrical applications,have relatively tight controls on those impurities that
might lower electrical conductivity.

Subcategory: 1000 Series Aluminum; Aluminum Alloy; Metal; Nonferrous Metal
Close Analogs:

Composition Notes:
The aluminum content for unalloyed aluminum not made by a refining process is the difference between 100.00 percent and the sum of all other analyzed metallic elements present in amounts of 0.010 percent of more each, expressed to the second decimal before determining the sum. For alloys and unalloyed aluminum not made by a refining process, when the specified maximum limit is 0.XX, an observed value or a calculated value greater than 0.005 but less than 0.010% is rounded off and shown as " less than 0.01%".
Composition information provided by the Aluminum Association and is not for design.

Key Words: Aluminium 1110; AA1110
Component Wt. %
Al Min 99.1
B Max 0.02
Cr Max 0.01
Cu Max 0.04

Component Wt. %
Fe Max 0.8
Mg Max 0.25
Mn Max 0.01

Component Wt. %
Other, each Max 0.03
Si Max 0.3
V+Ti Min 0.03

Subcategory: 1000 Series Aluminum; Aluminum Alloy; Metal; Nonferrous Metal
Close Analogs:

Composition Notes:
0.0008% max Be for welding electrode and filler wire only.
The aluminum content for unalloyed aluminum not made by a refining process is the difference between 100.00 percent and the sum of all other analyzed metallic elements present in amounts of 0.010 percent of more each, expressed to the second decimal before determining the sum. For alloys and unalloyed aluminum not made by a refining process, when the specified maximum limit is 0.XX, an observed value or a calculated value greater than 0.005 but less than 0.010% is rounded off and shown as " less than 0.01%".
Composition information provided by the Aluminum Association and is not for design.

Key Words: Aluminium 1188; AA1188
Component Wt. %
Al Min 99.88
Cu Max 0.005
Fe Max 0.06
Ga Max 0.03

Component Wt. %
Mg Max 0.01
Mn Max 0.01
Other, each Max 0.01
Si Max 0.06

Component Wt. %
Ti Max 0.01
V Max 0.05
Zn Max 0.03

I350 H19 SOLID
Construction
Conductors are aluminum alloy 1350-H19, 6201-T81, or ACSR conductors, concentrically stranded and covered for weather proofing with polyethylene, high-density polyethylene (HID) or crosslinked polyethylene (XLP).

Application
Covered Line Wire is used primarily for overhead secondary distribution lines. It is not an electrically insulated conductor and is treated as bare conductor when installed.

Type XHHW
Building Wire - Aluminum Conductor - Type XHHW

Construction
Compact stranded 8000 Series aluminum alloy conductor, black abrasion, heat and moisture resistant crosslinked polyethylene insulation.

Application
Type XHHW is intended for use as general purpose wiring in air, conduit or other recognized raceways for services, feeders and branch circuit wiring as specified in the National Electric Code at a maximum conductor temperature of 90°C in dry locations and 75°C in wet locations.
Subcategory: 1000 Series Aluminum; Aluminum Alloy; Metal; Nonferrous Metal
The 8xxx series is used for those alloys with lesser used alloying elements such
as Fe,Ni and Li.Each is used for the particular characteristics it provides the
alloys: Fe and Ni provide strength with little loss in electrical conductivity and so
are used in a series of alloys represented by 8017 for conductors.Li in alloy 8090
provides exceptionally high strength and modulus, and so this alloy is used for
aerospace applications where increases in stiffness combined with high strength
reduces component

Key Words: Aluminium 8017-H12; AA8017-H12
Component Wt. %
Al Max 98.6
B Max 0.04
Cu 0.1 - 0.2
Fe 0.55 - 0.8

Component Wt. %
Li Max 0.003
Mg 0.01 - 0.05
Other, each Max 0.03

Component Wt. %
Other, total Max 0.1
Si Max 0.1
Zn Max 0.05
Close Analogs:

Composition Notes:
The aluminum content for unalloyed aluminum not made by a refining process is the difference between 100.00 percent and the sum of all other analyzed metallic elements present in amounts of 0.010 percent of more each, expressed to the second decimal before determining the sum. For alloys and unalloyed aluminum not made by a refining process, when the specified maximum limit is 0.XX, an observed value or a calculated value greater than 0.005 but less than 0.010% is rounded off and shown as " less than 0.01%".
Composition information provided by the Aluminum Association and is not for design.

Key Words: Aluminium 1350-H19; Electrical Conductor Grade (EC); UNS A91350; NF A5/L (France); AA1350-H19, BS1E (UK); DIN E-Al99.5
Component Wt. %
Al Min 99.5
B Max 0.05
Cr Max 0.01
Cu Max 0.05

Component Wt. %
Fe Max 0.4
Ga Max 0.03
Mn Max 0.01
Other, each Max 0.03

Component Wt. %
Other, total Max 0.1
Si Max 0.1
V+Ti Min 0.02
Zn Max 0.05

Universal Wire Works Alloy 1100 (AMS 4180) Aluminum Alloy Filler Metal
Subcategory: 1000 Series Aluminum; Aluminum Alloy; Metal; Nonferrous Metal
Component Wt. %
Al 99.9
Cu Max 0.02
Mn 0.05
Si+Fe Max 0.02
Zn 0.1

Material Notes:
Alloy 1100 is virtually pure aluminum designed to weld grades 1100 and 3003 aluminum sheets, plates, bars, e

Subcategory: 6000 Series Aluminum Alloy; Aluminum Alloy; Metal; Nonferrous Metal
Close Analogs:

Composition Notes:
Aluminum content reported is calculated as remainder.
Composition information provided by the Aluminum Association and is not for design.
panels with high dent resistance; and 6101and 6201 for high strength electrical
bus and electrical conductor wire, respectively.

Key Words: UNS A96201; Aluminium 6201-T81; AA6201-T81
Component Wt. %
Al 97.3 - 98.9
B Max 0.06
Cr Max 0.03
Cu Max 0.1

Component Wt. %
Fe Max 0.5
Mg 0.6 - 0.9
Mn Max 0.03
Other, each Max 0.03

Component Wt. %
Other, total Max 0.1
Si 0.5 - 0.9
Zn Max 0.1

resonance - 4-9-2005 at 17:03

what could a brown residue be that was left from aluminium welding/filler rod ???

12AX7 - 4-9-2005 at 17:09

Iron (oxide?), silicon, ?

Tim

bio2 - 6-9-2005 at 02:10

Silicon leaves a white residue when the Al is dissolved in NaOH solution. Fe leaves a black residue that oxidizes to brownish red within a day or so if left in the solution.

Look up the welding alloy composition for other metals as there are many, many types with only the 99% or better grades being suitable for reduction use.

resonance - 7-9-2005 at 20:27

Quote:

Originally posted by resonance
what could a brown residue be that was left from aluminium welding/filler rod ???

after getting hold of the technical papers for these rods, it seems the brown residue is magnesium

12AX7 - 8-9-2005 at 08:17

Wouldn't that just form Mg(OH)2?

FWIW, Mg in small amounts (up to maybe 5%) is in solid solution with the alpha aluminum.

Tim

MostlyAir - 16-12-2011 at 12:36

Quote: Originally posted by Tacho

1- a spatula tip of Hg2Cl2 (calomel) in a test tube.

2- add 1ml HCl 37%

3- add 1ml H2O2 as concentrated as you can get. I used 30%, but I gess 10% would work

4- Put a cottom plug on top of the tube -heat on a small flame, don't boil it - a vigorous reaction (bubbling) takes place - be carefull with the spray (mist) comming from it, it has very poisonous mercuric chloride in it, hence the cottom plug.

5- the crystal clear solution left (no calomel precipitate) is a mecuric chloride solution. Insert a piece of clean copper wire in the solution(thanks Polverone). It should come out silvery because it's coated with Hg.

6- Use "as is" diluted in water or neutralize first and get rid of the excess H2O2 with manganese dioxide. I use my marvelous catalyst to do it. Don't forget the cottom plug here.

I cam across this website yesterday while searching for a way to turn about a gram or so of the Hg2Cl2 I had into at least a half a gram of HgCl2 (the way more soluble mercury salt I could use). I know this is a very old post, but I am presently attempting this reaction (http://www.sciencemadness.org/talk/viewthread.php?tid=4248&a...), with slight modifications (because I don't have the chemicals is their concentration, as suggested), and am hoping for some feedback.

Here's what I did:

In a test tube, I placed 800mg of Hg2Cl2, 1mL of HCL (only 29%) and 8mL of H202 (3% from a drug store), then capped it off with a cotton ball as advised. I increased the H202 amount because I figured it would be necessary to offset the low concentration of the solution. Then I placed the test tube in a water bath on my hot plate stirrer and heated it up to about 85C.

The white Hg2Cl2 powder is at the bottom of the tube, and lots of tiny, very small bubbles are rising out of it (I'm hoping as a result of the reaction, and not merely the heat from the water bath). That said, these bubbles are hardly "vigorous" and it has been an hour so far and it hardly seems like any of the calomel has reacted or reduced.

Is the procedure doomed because of the lower concentrations of HCL & Hydrogen Peroxide? Or do I just need to be patient? Should I adjust the amounts of the reagents? Or should I just wait until next week when I can try to acquire some real Hydrogen Peroxide (which I really would rather not do because it's such a pain to order and pickup). Thanks for all your help!

EDIT/UPDATE:

I was patient, and waited over 6 hours for this to process. During this time, I added another 1mL of HCL (29%) and another 12 mL of H2O2 (3%) in 3 different additions of 4 mL as the reaction bubbling slowed.

After 6 hours, the Hg2Cl2 didn't fully disolve but the H2O2 bubbles were gone again and I was tired of waiting...and I only needed about 400-500mg of HgCl2 for my reaction anyway, so I decided to use the tube's contents (now about 20mL of mostly acidic water and a little of the original Hg2Cl2 on the bottom).

The Al amalgam was a success within 5 minutes of me adding the tube's contents down the condenser. Too much of a success actually (I got a manageable, but frightening reflux up the condensor in about 10 minutes). Ultimately though, my patience paid off and I was able to achieve my goals with only the chemicals on hand. Just thought I'd share it with you in case 3% Hydrogen Peroxide is all you have at the moment...

[Edited on 17-12-2011 by MostlyAir]