Making a small quantity of ferric chloride (III)

Hello to all of you,

I wanted to obtain a small quantity of ferric chloride (III), no ferrous
chloride (II).

To do this, I contacted a concentrated HCL solution with iron powder (not
steel powder) for about 7 days: there was a release of H2 that I could
notice with a flame. When calculating my quantities, I used an excess HCL
(about 35% excess by mass) in an atempt to favor the ferric (III) over the
ferrous (II) chloride. Afetr about 7 days of reaction, I filtered the
solution since there was still a deposit of powder at the bottom of the
beaker (I believe the deposit was iron since the density appeared high based
on the quick settling time after stirring). I got a pale green solution
that I brought up in temperature to 95°C for evaporation. After 4-5 hours
at 95°C, I reduced the liquid volume of the solution by more than 50 %. The
solution was now brown with a bit of a beige deposit. There was probably
still some HCL in the solution during the evaporation based on the strong
and irritant smell of the fumes. After letting the solution cool for a day
on the counter, I obtained large pale green crystals, needle shaped.
Iremoved the crystals from the solution to let them dry in air.

Question 1:
Is this ferrous chloride (II)? My chemical dictionnary would suggest yes
becaus they say that ferrous chloride is green while ferric chloride is
brown. However, ferrous chloride is said to be deliquescent from the same
dictionary, it should therefore dissolve itself in the moisture that it
absorbs from the air, no? Unless tere was not enough time?

Question 2:
If it is ferous chloride, how cam I get ferric chloride? I got the
suggestion to treat the solid crystals (or in solution?) with chlorine, but
I do not have the gas available. Any other alternatives?

Thanks in advance...

"Patrice Nadeau" <[Only registered users see links. ]> wrote in message
news:LXjRb.6740$[Only registered users see links. ].. .
While you do have your excess of HCl ( 3 moles/mole Fe) in solution
do (a) or (b) or......(e)....

a) heat it to 40-50C and bubble slowly air thru it. (Aquarium pump)
FeCl2 + HCl + 1/2 O2 ----> FeCl3 + 1/2 H2O
b) add slowly dilute H2O2 (Peroxide) into the solution
FeCl2 + HCl + 1/2 H2O2 ----> FeCl3 + H2O
c) add Cl2/water solution to it, which you make on the side from diluted
2 HCl + H2O2 ---> Cl2 + 2 H2O
2 FeCl2 + Cl2 ----> 2 FeCl3
d) drip/bubble dilute HNO3 or NOx thru it
FeCl2 + HCl + HNO3 ---> FeCl3 + H2O + NO2
(this might give you NOx contamineed FeCl3, and you may have to
make an addtional work up step to get pure FeCl3)
e) etc......there are dozens of ways to get to FeCl3.....

You should get a clear dark yellow/honey colored liquid. No green.

Explore and enjoy chemistry. -- **** enviros.
hanson

"hanson" <[Only registered users see links. ]> wrote in message news:<ydlRb.28898$[Only registered users see links. ].pas.ear thlink.net>...


A further suggestion, if one simply oxidises the reaction solution (in
step 2) with a slight excess of hydrogen peroxide, one can do away
with nitric acid, bubbling air and heating the solution(in step 1),
perhaps it will take a longer time to dissolve iron in HCl without
heating.

Whenever I prepared copper sulfate from copper turnings and
concentrated sulfuric acid, nothing seemed to happen, even if kept in
a boiling water bath, as I added 33% hydrogen peroxide, the turnings
would immediatly start dissolving and the solution acquired a deep
blue color in 10 minutes with almost no turnings remaining in that
solution.

Hanson wrote
Does this actually occur?

"Mohammed Farooq" <[Only registered users see links. ]> wrote in message
news:66756669.0401270839.15247a92@posting.google.c om...
news:<ydlRb.28898$[Only registered users see links. ].pas.ear thlink.net>...
but
[Hanson]
It seems so to me, as long as HCl is in stochiometric excess
over H2O2, else you'd get HClOx, where x = 1 to 4.
But even then it wouldn't matter, because HClOx, with Fe2+ and
Fe present, will be reduced to the Cl- in the oxidized FeCl3.

>From: "hanson" [Only registered users see links. ]


We used to oxidize FeCl2 with Cl2 ...to regenerate PCB etchants ... quick
reaction ... goes to completion ...quantitative and easily controlled by ORP
....


Be seeing you
In the Village
Number 6

[Only registered users see links. ] (SNUMBER6) wrote:


I've thought about doing this myself, even though dealing with Cl2 is
nasty and FeCl3 solution is not very expensive at RadioShack. How did
you get rid of the copper ion?

Steve Turner

Real address contains worldnet instead of spamnet

>From: Steve Turner [Only registered users see links. ]


Back 25-30 years ago ... We needed an additional source of cheap copper ...and
.... Spent Ferric Etchants were being dumped down the sewers ... to the dismay
of local sewerage authorities ... companies doing this were more than glad all
of a sudden to give us these solutions for free ... or even pay us (less than
the disposal charge ... )

We developed the process to recycle the etchant ... by cementing the copper
with scrap iron ... ( which had the effect of also reducing all the Ferric Ion
present to Ferrous) ... It was this Cu free solution that we oxidized with
Chlorine ... and resold to the customer ... It worked better than the original
....
An astute observer would note that one generates a lot more solution each time
the material is recycled ... so one needed an expanded customer base ... It was
like a pyramid scheme ... leading to the ultimate demise of the process ...




Be seeing you
In the Village
Number 6

"hanson" <[Only registered users see links. ]> wrote in message news:<PpARb.29057$[Only registered users see links. ].pas.eart hlink.net>...

Hanson
I think Hydrogen peroxide is unable to oxidize HCl to OCl- or
chlorite, or perchlorate ion, keeping in mind the chemical properties
of H2O2 and electrode potentials of hydrogen peroxide.
Hypochlorite ion is more powerful oxidizing agent than peroxide ion ,
and both are not compatable with each other, the final reaction being
OCl- +H2O2--> O2 +Cl +H2O. I remember this reaction produces light
when a suitable dye is used.

"Mohammed Farooq" <[Only registered users see links. ]> wrote in message
news:66756669.0401271951.130ae510@posting.google.c om...
news:<PpARb.29057$[Only registered users see links. ].pas.eart hlink.net>...
ferrous
chlorine,
[hanson]
Interesting. When I get back into the labs, I'll asked them to play
with your assertion and find out. Don't hold your breath though.
It'll take time. BTW. What dye did you use and what color of light
did it produce? Gimme some details about this reaction, please.
hanson

"hanson" <[Only registered users see links. ]> wrote in message news:<tsIRb.29877$[Only registered users see links. ].pas.earth link.net>...

Hanson,
The book by Oxtoby et.al "General Chemistry" ,from which I read (two
years back) this chemiluminiscent reaction simply uses the word "dye".
I am afraid I can not name that particular sensitizer that is used to
produce light in peroxide-hypochlorite reaction, however in an amateur
home experiment(two years back) after reading that article I tried
fluorescein, but nothing happened, only oxygen bubbled out
immediately.
After reading this post, I searched ACS monograph "Hydorgen Peroxide"
by Walter J. Schumb, it does discuss this reaction from kinetics point
of view, an interesting point is that oxygen that comes out is from
hydrogen peroxide only not from hypochlorite. Nothing is mentioned
about chemiluminiscence.The relevant article is A.U. Khan and M.
Kasha, J. Amer. Chem. Soc., 1970, 92, 3293

However an excellent demonstration by Leeds University on singlet
oxygen produced by this reaction is here
[Only registered users see links. ]
and a reference in J.Chem. Ed
B.Z. Shakhashiri and L.G. Williams, "Singlet oxygen in aqueous
solution: a lecture demonstration", J. Chem. Educ., 1976, 53, 358.
Do tell us more about your experiment, when you get time to do it.
By the way, Hanson, what is your area of specialization?