What is the most convenient way to prepare ferrous oxide (FeO) in the laboratory?Most economical method to convert potassium oxide to potassium nitride.What does Cobaltous Oxide form with metal oxides?What is the nature of the oxide of boron?What is the most accepted explanation of aurophilicity?What causes the iridescent colour in laboratory grown bismuth?What are the most extreme chemicals?What is the most compact way to store Oxygen?Is to possible to prepare gallium oxide from gallium sulfate against gallium nitrate or ZnO from ZnSO4 against Zn(NO3)2How can copper(II) nitrate hexahydrate be synthesized in the laboratory as well as industrially?What noble metal is most oxidation resistant?
Do other countries guarantee freedoms that the United States does not have?
ESTA declined to the US
Did silent film actors actually say their lines or did they simply improvise “dialogue” while being filmed?
Decode a variable-length quantity
Colleagues speaking another language and it impacts work
Not understanding how the gain works in the 1st stage of an instrumentation amplifier
Where to pee in London?
How do I get the =LEFT function in excel, to also take the number zero as the first number?
In the movie Harry Potter and the Order or the Phoenix, why didn't Mr. Filch succeed to open the Room of Requirement if it's what he needed?
How to avoid ci-driven development..?
Changing headheight pushes footer off page
Secure my password from unsafe servers
Finish the Mastermind
What can make Linux unresponsive for minutes when browsing certain websites?
Is alignment needed after replacing upper control arms?
sytemctl status log output
Is it true that control+alt+delete only became a thing because IBM would not build Bill Gates a computer with a task manager button?
Why do proponents of guns oppose gun competency tests?
Does bottle color affect mold growth?
Does the Voyager team use a wrapper (Fortran(77?) to Python) to transmit current commands?
What word can be used to describe a bug in a movie?
Will a paper be retracted if a flaw in released software code invalidates its central idea?
What does VB stand for?
Why do private jets such as Gulfstream fly higher than other civilian jets?
What is the most convenient way to prepare ferrous oxide (FeO) in the laboratory?
Most economical method to convert potassium oxide to potassium nitride.What does Cobaltous Oxide form with metal oxides?What is the nature of the oxide of boron?What is the most accepted explanation of aurophilicity?What causes the iridescent colour in laboratory grown bismuth?What are the most extreme chemicals?What is the most compact way to store Oxygen?Is to possible to prepare gallium oxide from gallium sulfate against gallium nitrate or ZnO from ZnSO4 against Zn(NO3)2How can copper(II) nitrate hexahydrate be synthesized in the laboratory as well as industrially?What noble metal is most oxidation resistant?
.everyoneloves__top-leaderboard:empty,.everyoneloves__mid-leaderboard:empty,.everyoneloves__bot-mid-leaderboard:empty margin-bottom:0;
$begingroup$
The Wikipedia page for ferrous oxide states that $ceFeO$ can be prepared by the thermal decomposition of iron(II) oxalate, with the following reaction:
$$ceFeC2O4 → FeO + CO2 + CO$$
And that the procedure is conducted under an inert atmosphere to avoid the formation of ferric oxide.
Sicius' Eisengruppe: Elemente der achten Nebengruppe: Eine Reise durch das Periodensystem states that $ceFeC2O4$ should "slowly" be heated in a vacuum and then rapidly cooled down.
Both of these resources, however, omit critical information as to the preparation process. These questions remain:
At which temperature does this reaction really start occurring, and what is the ideal temperature range to carry out this thermal decomposition?
How "fast" should it be cooled down? And what are appropriate methods to do so?
I'd be very thankful for any additional information on the topic.
inorganic-chemistry synthesis metal reference-request decomposition
$endgroup$
add a comment |
$begingroup$
The Wikipedia page for ferrous oxide states that $ceFeO$ can be prepared by the thermal decomposition of iron(II) oxalate, with the following reaction:
$$ceFeC2O4 → FeO + CO2 + CO$$
And that the procedure is conducted under an inert atmosphere to avoid the formation of ferric oxide.
Sicius' Eisengruppe: Elemente der achten Nebengruppe: Eine Reise durch das Periodensystem states that $ceFeC2O4$ should "slowly" be heated in a vacuum and then rapidly cooled down.
Both of these resources, however, omit critical information as to the preparation process. These questions remain:
At which temperature does this reaction really start occurring, and what is the ideal temperature range to carry out this thermal decomposition?
How "fast" should it be cooled down? And what are appropriate methods to do so?
I'd be very thankful for any additional information on the topic.
inorganic-chemistry synthesis metal reference-request decomposition
$endgroup$
4
$begingroup$
If you were an undergrad student, this would qualify as "homework": literature research. Are you? ;-)
$endgroup$
– Karl
Jul 28 at 20:11
add a comment |
$begingroup$
The Wikipedia page for ferrous oxide states that $ceFeO$ can be prepared by the thermal decomposition of iron(II) oxalate, with the following reaction:
$$ceFeC2O4 → FeO + CO2 + CO$$
And that the procedure is conducted under an inert atmosphere to avoid the formation of ferric oxide.
Sicius' Eisengruppe: Elemente der achten Nebengruppe: Eine Reise durch das Periodensystem states that $ceFeC2O4$ should "slowly" be heated in a vacuum and then rapidly cooled down.
Both of these resources, however, omit critical information as to the preparation process. These questions remain:
At which temperature does this reaction really start occurring, and what is the ideal temperature range to carry out this thermal decomposition?
How "fast" should it be cooled down? And what are appropriate methods to do so?
I'd be very thankful for any additional information on the topic.
inorganic-chemistry synthesis metal reference-request decomposition
$endgroup$
The Wikipedia page for ferrous oxide states that $ceFeO$ can be prepared by the thermal decomposition of iron(II) oxalate, with the following reaction:
$$ceFeC2O4 → FeO + CO2 + CO$$
And that the procedure is conducted under an inert atmosphere to avoid the formation of ferric oxide.
Sicius' Eisengruppe: Elemente der achten Nebengruppe: Eine Reise durch das Periodensystem states that $ceFeC2O4$ should "slowly" be heated in a vacuum and then rapidly cooled down.
Both of these resources, however, omit critical information as to the preparation process. These questions remain:
At which temperature does this reaction really start occurring, and what is the ideal temperature range to carry out this thermal decomposition?
How "fast" should it be cooled down? And what are appropriate methods to do so?
I'd be very thankful for any additional information on the topic.
inorganic-chemistry synthesis metal reference-request decomposition
inorganic-chemistry synthesis metal reference-request decomposition
edited Jul 28 at 22:43
andselisk♦
21.9k8 gold badges77 silver badges147 bronze badges
21.9k8 gold badges77 silver badges147 bronze badges
asked Jul 28 at 19:45
HansHans
617 bronze badges
617 bronze badges
4
$begingroup$
If you were an undergrad student, this would qualify as "homework": literature research. Are you? ;-)
$endgroup$
– Karl
Jul 28 at 20:11
add a comment |
4
$begingroup$
If you were an undergrad student, this would qualify as "homework": literature research. Are you? ;-)
$endgroup$
– Karl
Jul 28 at 20:11
4
4
$begingroup$
If you were an undergrad student, this would qualify as "homework": literature research. Are you? ;-)
$endgroup$
– Karl
Jul 28 at 20:11
$begingroup$
If you were an undergrad student, this would qualify as "homework": literature research. Are you? ;-)
$endgroup$
– Karl
Jul 28 at 20:11
add a comment |
2 Answers
2
active
oldest
votes
$begingroup$
In appears that the synthetic procedure for preparation of iron(II) oxide from iron(II) oxalate has been first described by Günther et al. [1] and subsequently summarized in Brauer's Handbook of Preparative Inorganic Chemistry [2, p. 1497]:
Iron (II) Oxide
I.
$$ceunderset143.8FeC2O4 = underset71.8FeO + underset28.0CO + underset44.0CO2$$
Thermal decomposition of $ceFeC2O4$ yields pure $ceFeO$ only under specific conditions.
The decomposition is carried out in a quartz vessel (Fig. 332) whose lower section is kept at $pu850 °C$ by means of an electric furnace.
The joint is surrounded by a water-cooled lead coil or a rubber hose.
The nascent gases should be removed as quickly as possible; for this reason, the reactor is connected to two parallel mercury pumps and a good forepump; the gas is carried into two liquid-nitrogen-cooled traps containing activated charcoal.
Fig. 332. Preparation of iron (II) oxide.
The starting $ceFeC2O4$ $(pu0.5 - 0.8 g.)$ is placed in the small bulb above the quartz vessel, and the water of crystallization is completely vaporized by heating in vacuum for 12 hours at $pu200 °C.$
The bulb is turned in the joint, and the $ceFeC2O4$ drops into the heated lower section of the reactor where it is rapidly decomposed to $ceFeO,$ $ceCO$ and $ceCO2$ (the decomposition is complete in about 20 seconds). The product $ceFeO$ is retained by a quartz wool plug, which must be loose enough to prevent a buildup of pressure during the decomposition.
The furnace is now removed and the hot quartz tube is chilled as rapidly as possible in cold water, since $ceFeO$ is unstable in the range of $pu300-560 °C$ and decomposes according to:
$$ce4 FeO = Fe3O4 + Fe$$
(this decomposition proceeds most rapidly at about $pu480 °C,$ but
ceases below $pu300 °C).$
The above procedure yields a jet-black product, readily soluble in dilute acids; it is rapidly oxidized in air, but does not ignite.
Alternatively, iron(III) oxide can be reduced by iron to iron(II) oxide [2, p. 1498]:
II. The preparation from stoichiometric quantities of commercial $ceFe2O3$ and reduced iron can also be recommended.
The mixture and a few drops of water are sealed into a preevacuated quartz tube, heated for about three days at $pu900 °C,$ and quenched in cold water.
$$ceFe + Fe2O3 ->[pu900 °C] 3 FeO$$
Iron(II) oxide can also be produced from iron(III) oxide reduction by carbon monoxide at the temperature range between $pu500 °C$ and $pu600 °C$ (adapted from [3, p. 415]):
$$
beginalign
ce3 Fe2O3 + CO &->[pu400 °C] 2 Fe3O4 + CO2 \
ceFe2O3 + CO &->[pu500-600 °C] 2 FeO + CO2 \
ceFe2O3 + 3 CO &->[pu700 °C] 2 Fe + 3 CO2
endalign
$$
as well as by thermal decomposition of magnetite [3, p. 415]:
$$ce2 Fe3O4 ->[>pu1538 °C] 6 FeO + O2$$
References
- Günther, P. L.; Rehaag, H. Über Die Thermische Zersetzung von Oxalaten II. Mitteilung. Darstellung von Reinem Ferrooxyd. Z. Anorg. Allg. Chem. 1939, 243 (1), 60–68. https://doi.org/10/cqzgk8. (in German)
- Handbook of Preparative Inorganic Chemistry, 2nd ed.; Brauer, G., Ed.; Academic Press: New York; London, 1965; Vol. 2.
- R. A. Lidin, V. A. Molochko, and L. L. Andreeva, Reactivity of Inorganic Substances, 3rd ed.; Khimia: Moscow, 2000. (in Russian)
$endgroup$
2
$begingroup$
That's an awesome answer :)
$endgroup$
– Hans
Jul 28 at 22:52
add a comment |
$begingroup$

The paper linked below indicates that the proper temperature is north of 535°C. This decomposition should be carried out with great caution though as some of the products might enflame, or even initiate a thermite reaction if carried out in the presence of Aluminum (as in the experimental setup used for the paper hereafter).
Source: https://pubs.rsc.org/en/content/articlelanding/2006/jm/b514565a#!divAbstract
$endgroup$
2
$begingroup$
The CO would give one pause, unless this was being done with proper facilities and safety equipment.
$endgroup$
– Ed V
Jul 28 at 21:06
1
$begingroup$
Agreed! Maybe with a way to vacuum extract the gases from the container once the decomposition has proceeded
$endgroup$
– Veritas
Jul 28 at 21:11
add a comment |
Your Answer
StackExchange.ready(function()
var channelOptions =
tags: "".split(" "),
id: "431"
;
initTagRenderer("".split(" "), "".split(" "), channelOptions);
StackExchange.using("externalEditor", function()
// Have to fire editor after snippets, if snippets enabled
if (StackExchange.settings.snippets.snippetsEnabled)
StackExchange.using("snippets", function()
createEditor();
);
else
createEditor();
);
function createEditor()
StackExchange.prepareEditor(
heartbeatType: 'answer',
autoActivateHeartbeat: false,
convertImagesToLinks: false,
noModals: true,
showLowRepImageUploadWarning: true,
reputationToPostImages: null,
bindNavPrevention: true,
postfix: "",
imageUploader:
brandingHtml: "Powered by u003ca class="icon-imgur-white" href="https://imgur.com/"u003eu003c/au003e",
contentPolicyHtml: "User contributions licensed under u003ca href="https://creativecommons.org/licenses/by-sa/3.0/"u003ecc by-sa 3.0 with attribution requiredu003c/au003e u003ca href="https://stackoverflow.com/legal/content-policy"u003e(content policy)u003c/au003e",
allowUrls: true
,
onDemand: true,
discardSelector: ".discard-answer"
,immediatelyShowMarkdownHelp:true
);
);
Sign up or log in
StackExchange.ready(function ()
StackExchange.helpers.onClickDraftSave('#login-link');
);
Sign up using Google
Sign up using Facebook
Sign up using Email and Password
Post as a guest
Required, but never shown
StackExchange.ready(
function ()
StackExchange.openid.initPostLogin('.new-post-login', 'https%3a%2f%2fchemistry.stackexchange.com%2fquestions%2f118606%2fwhat-is-the-most-convenient-way-to-prepare-ferrous-oxide-feo-in-the-laboratory%23new-answer', 'question_page');
);
Post as a guest
Required, but never shown
2 Answers
2
active
oldest
votes
2 Answers
2
active
oldest
votes
active
oldest
votes
active
oldest
votes
$begingroup$
In appears that the synthetic procedure for preparation of iron(II) oxide from iron(II) oxalate has been first described by Günther et al. [1] and subsequently summarized in Brauer's Handbook of Preparative Inorganic Chemistry [2, p. 1497]:
Iron (II) Oxide
I.
$$ceunderset143.8FeC2O4 = underset71.8FeO + underset28.0CO + underset44.0CO2$$
Thermal decomposition of $ceFeC2O4$ yields pure $ceFeO$ only under specific conditions.
The decomposition is carried out in a quartz vessel (Fig. 332) whose lower section is kept at $pu850 °C$ by means of an electric furnace.
The joint is surrounded by a water-cooled lead coil or a rubber hose.
The nascent gases should be removed as quickly as possible; for this reason, the reactor is connected to two parallel mercury pumps and a good forepump; the gas is carried into two liquid-nitrogen-cooled traps containing activated charcoal.
Fig. 332. Preparation of iron (II) oxide.
The starting $ceFeC2O4$ $(pu0.5 - 0.8 g.)$ is placed in the small bulb above the quartz vessel, and the water of crystallization is completely vaporized by heating in vacuum for 12 hours at $pu200 °C.$
The bulb is turned in the joint, and the $ceFeC2O4$ drops into the heated lower section of the reactor where it is rapidly decomposed to $ceFeO,$ $ceCO$ and $ceCO2$ (the decomposition is complete in about 20 seconds). The product $ceFeO$ is retained by a quartz wool plug, which must be loose enough to prevent a buildup of pressure during the decomposition.
The furnace is now removed and the hot quartz tube is chilled as rapidly as possible in cold water, since $ceFeO$ is unstable in the range of $pu300-560 °C$ and decomposes according to:
$$ce4 FeO = Fe3O4 + Fe$$
(this decomposition proceeds most rapidly at about $pu480 °C,$ but
ceases below $pu300 °C).$
The above procedure yields a jet-black product, readily soluble in dilute acids; it is rapidly oxidized in air, but does not ignite.
Alternatively, iron(III) oxide can be reduced by iron to iron(II) oxide [2, p. 1498]:
II. The preparation from stoichiometric quantities of commercial $ceFe2O3$ and reduced iron can also be recommended.
The mixture and a few drops of water are sealed into a preevacuated quartz tube, heated for about three days at $pu900 °C,$ and quenched in cold water.
$$ceFe + Fe2O3 ->[pu900 °C] 3 FeO$$
Iron(II) oxide can also be produced from iron(III) oxide reduction by carbon monoxide at the temperature range between $pu500 °C$ and $pu600 °C$ (adapted from [3, p. 415]):
$$
beginalign
ce3 Fe2O3 + CO &->[pu400 °C] 2 Fe3O4 + CO2 \
ceFe2O3 + CO &->[pu500-600 °C] 2 FeO + CO2 \
ceFe2O3 + 3 CO &->[pu700 °C] 2 Fe + 3 CO2
endalign
$$
as well as by thermal decomposition of magnetite [3, p. 415]:
$$ce2 Fe3O4 ->[>pu1538 °C] 6 FeO + O2$$
References
- Günther, P. L.; Rehaag, H. Über Die Thermische Zersetzung von Oxalaten II. Mitteilung. Darstellung von Reinem Ferrooxyd. Z. Anorg. Allg. Chem. 1939, 243 (1), 60–68. https://doi.org/10/cqzgk8. (in German)
- Handbook of Preparative Inorganic Chemistry, 2nd ed.; Brauer, G., Ed.; Academic Press: New York; London, 1965; Vol. 2.
- R. A. Lidin, V. A. Molochko, and L. L. Andreeva, Reactivity of Inorganic Substances, 3rd ed.; Khimia: Moscow, 2000. (in Russian)
$endgroup$
2
$begingroup$
That's an awesome answer :)
$endgroup$
– Hans
Jul 28 at 22:52
add a comment |
$begingroup$
In appears that the synthetic procedure for preparation of iron(II) oxide from iron(II) oxalate has been first described by Günther et al. [1] and subsequently summarized in Brauer's Handbook of Preparative Inorganic Chemistry [2, p. 1497]:
Iron (II) Oxide
I.
$$ceunderset143.8FeC2O4 = underset71.8FeO + underset28.0CO + underset44.0CO2$$
Thermal decomposition of $ceFeC2O4$ yields pure $ceFeO$ only under specific conditions.
The decomposition is carried out in a quartz vessel (Fig. 332) whose lower section is kept at $pu850 °C$ by means of an electric furnace.
The joint is surrounded by a water-cooled lead coil or a rubber hose.
The nascent gases should be removed as quickly as possible; for this reason, the reactor is connected to two parallel mercury pumps and a good forepump; the gas is carried into two liquid-nitrogen-cooled traps containing activated charcoal.
Fig. 332. Preparation of iron (II) oxide.
The starting $ceFeC2O4$ $(pu0.5 - 0.8 g.)$ is placed in the small bulb above the quartz vessel, and the water of crystallization is completely vaporized by heating in vacuum for 12 hours at $pu200 °C.$
The bulb is turned in the joint, and the $ceFeC2O4$ drops into the heated lower section of the reactor where it is rapidly decomposed to $ceFeO,$ $ceCO$ and $ceCO2$ (the decomposition is complete in about 20 seconds). The product $ceFeO$ is retained by a quartz wool plug, which must be loose enough to prevent a buildup of pressure during the decomposition.
The furnace is now removed and the hot quartz tube is chilled as rapidly as possible in cold water, since $ceFeO$ is unstable in the range of $pu300-560 °C$ and decomposes according to:
$$ce4 FeO = Fe3O4 + Fe$$
(this decomposition proceeds most rapidly at about $pu480 °C,$ but
ceases below $pu300 °C).$
The above procedure yields a jet-black product, readily soluble in dilute acids; it is rapidly oxidized in air, but does not ignite.
Alternatively, iron(III) oxide can be reduced by iron to iron(II) oxide [2, p. 1498]:
II. The preparation from stoichiometric quantities of commercial $ceFe2O3$ and reduced iron can also be recommended.
The mixture and a few drops of water are sealed into a preevacuated quartz tube, heated for about three days at $pu900 °C,$ and quenched in cold water.
$$ceFe + Fe2O3 ->[pu900 °C] 3 FeO$$
Iron(II) oxide can also be produced from iron(III) oxide reduction by carbon monoxide at the temperature range between $pu500 °C$ and $pu600 °C$ (adapted from [3, p. 415]):
$$
beginalign
ce3 Fe2O3 + CO &->[pu400 °C] 2 Fe3O4 + CO2 \
ceFe2O3 + CO &->[pu500-600 °C] 2 FeO + CO2 \
ceFe2O3 + 3 CO &->[pu700 °C] 2 Fe + 3 CO2
endalign
$$
as well as by thermal decomposition of magnetite [3, p. 415]:
$$ce2 Fe3O4 ->[>pu1538 °C] 6 FeO + O2$$
References
- Günther, P. L.; Rehaag, H. Über Die Thermische Zersetzung von Oxalaten II. Mitteilung. Darstellung von Reinem Ferrooxyd. Z. Anorg. Allg. Chem. 1939, 243 (1), 60–68. https://doi.org/10/cqzgk8. (in German)
- Handbook of Preparative Inorganic Chemistry, 2nd ed.; Brauer, G., Ed.; Academic Press: New York; London, 1965; Vol. 2.
- R. A. Lidin, V. A. Molochko, and L. L. Andreeva, Reactivity of Inorganic Substances, 3rd ed.; Khimia: Moscow, 2000. (in Russian)
$endgroup$
2
$begingroup$
That's an awesome answer :)
$endgroup$
– Hans
Jul 28 at 22:52
add a comment |
$begingroup$
In appears that the synthetic procedure for preparation of iron(II) oxide from iron(II) oxalate has been first described by Günther et al. [1] and subsequently summarized in Brauer's Handbook of Preparative Inorganic Chemistry [2, p. 1497]:
Iron (II) Oxide
I.
$$ceunderset143.8FeC2O4 = underset71.8FeO + underset28.0CO + underset44.0CO2$$
Thermal decomposition of $ceFeC2O4$ yields pure $ceFeO$ only under specific conditions.
The decomposition is carried out in a quartz vessel (Fig. 332) whose lower section is kept at $pu850 °C$ by means of an electric furnace.
The joint is surrounded by a water-cooled lead coil or a rubber hose.
The nascent gases should be removed as quickly as possible; for this reason, the reactor is connected to two parallel mercury pumps and a good forepump; the gas is carried into two liquid-nitrogen-cooled traps containing activated charcoal.
Fig. 332. Preparation of iron (II) oxide.
The starting $ceFeC2O4$ $(pu0.5 - 0.8 g.)$ is placed in the small bulb above the quartz vessel, and the water of crystallization is completely vaporized by heating in vacuum for 12 hours at $pu200 °C.$
The bulb is turned in the joint, and the $ceFeC2O4$ drops into the heated lower section of the reactor where it is rapidly decomposed to $ceFeO,$ $ceCO$ and $ceCO2$ (the decomposition is complete in about 20 seconds). The product $ceFeO$ is retained by a quartz wool plug, which must be loose enough to prevent a buildup of pressure during the decomposition.
The furnace is now removed and the hot quartz tube is chilled as rapidly as possible in cold water, since $ceFeO$ is unstable in the range of $pu300-560 °C$ and decomposes according to:
$$ce4 FeO = Fe3O4 + Fe$$
(this decomposition proceeds most rapidly at about $pu480 °C,$ but
ceases below $pu300 °C).$
The above procedure yields a jet-black product, readily soluble in dilute acids; it is rapidly oxidized in air, but does not ignite.
Alternatively, iron(III) oxide can be reduced by iron to iron(II) oxide [2, p. 1498]:
II. The preparation from stoichiometric quantities of commercial $ceFe2O3$ and reduced iron can also be recommended.
The mixture and a few drops of water are sealed into a preevacuated quartz tube, heated for about three days at $pu900 °C,$ and quenched in cold water.
$$ceFe + Fe2O3 ->[pu900 °C] 3 FeO$$
Iron(II) oxide can also be produced from iron(III) oxide reduction by carbon monoxide at the temperature range between $pu500 °C$ and $pu600 °C$ (adapted from [3, p. 415]):
$$
beginalign
ce3 Fe2O3 + CO &->[pu400 °C] 2 Fe3O4 + CO2 \
ceFe2O3 + CO &->[pu500-600 °C] 2 FeO + CO2 \
ceFe2O3 + 3 CO &->[pu700 °C] 2 Fe + 3 CO2
endalign
$$
as well as by thermal decomposition of magnetite [3, p. 415]:
$$ce2 Fe3O4 ->[>pu1538 °C] 6 FeO + O2$$
References
- Günther, P. L.; Rehaag, H. Über Die Thermische Zersetzung von Oxalaten II. Mitteilung. Darstellung von Reinem Ferrooxyd. Z. Anorg. Allg. Chem. 1939, 243 (1), 60–68. https://doi.org/10/cqzgk8. (in German)
- Handbook of Preparative Inorganic Chemistry, 2nd ed.; Brauer, G., Ed.; Academic Press: New York; London, 1965; Vol. 2.
- R. A. Lidin, V. A. Molochko, and L. L. Andreeva, Reactivity of Inorganic Substances, 3rd ed.; Khimia: Moscow, 2000. (in Russian)
$endgroup$
In appears that the synthetic procedure for preparation of iron(II) oxide from iron(II) oxalate has been first described by Günther et al. [1] and subsequently summarized in Brauer's Handbook of Preparative Inorganic Chemistry [2, p. 1497]:
Iron (II) Oxide
I.
$$ceunderset143.8FeC2O4 = underset71.8FeO + underset28.0CO + underset44.0CO2$$
Thermal decomposition of $ceFeC2O4$ yields pure $ceFeO$ only under specific conditions.
The decomposition is carried out in a quartz vessel (Fig. 332) whose lower section is kept at $pu850 °C$ by means of an electric furnace.
The joint is surrounded by a water-cooled lead coil or a rubber hose.
The nascent gases should be removed as quickly as possible; for this reason, the reactor is connected to two parallel mercury pumps and a good forepump; the gas is carried into two liquid-nitrogen-cooled traps containing activated charcoal.
Fig. 332. Preparation of iron (II) oxide.
The starting $ceFeC2O4$ $(pu0.5 - 0.8 g.)$ is placed in the small bulb above the quartz vessel, and the water of crystallization is completely vaporized by heating in vacuum for 12 hours at $pu200 °C.$
The bulb is turned in the joint, and the $ceFeC2O4$ drops into the heated lower section of the reactor where it is rapidly decomposed to $ceFeO,$ $ceCO$ and $ceCO2$ (the decomposition is complete in about 20 seconds). The product $ceFeO$ is retained by a quartz wool plug, which must be loose enough to prevent a buildup of pressure during the decomposition.
The furnace is now removed and the hot quartz tube is chilled as rapidly as possible in cold water, since $ceFeO$ is unstable in the range of $pu300-560 °C$ and decomposes according to:
$$ce4 FeO = Fe3O4 + Fe$$
(this decomposition proceeds most rapidly at about $pu480 °C,$ but
ceases below $pu300 °C).$
The above procedure yields a jet-black product, readily soluble in dilute acids; it is rapidly oxidized in air, but does not ignite.
Alternatively, iron(III) oxide can be reduced by iron to iron(II) oxide [2, p. 1498]:
II. The preparation from stoichiometric quantities of commercial $ceFe2O3$ and reduced iron can also be recommended.
The mixture and a few drops of water are sealed into a preevacuated quartz tube, heated for about three days at $pu900 °C,$ and quenched in cold water.
$$ceFe + Fe2O3 ->[pu900 °C] 3 FeO$$
Iron(II) oxide can also be produced from iron(III) oxide reduction by carbon monoxide at the temperature range between $pu500 °C$ and $pu600 °C$ (adapted from [3, p. 415]):
$$
beginalign
ce3 Fe2O3 + CO &->[pu400 °C] 2 Fe3O4 + CO2 \
ceFe2O3 + CO &->[pu500-600 °C] 2 FeO + CO2 \
ceFe2O3 + 3 CO &->[pu700 °C] 2 Fe + 3 CO2
endalign
$$
as well as by thermal decomposition of magnetite [3, p. 415]:
$$ce2 Fe3O4 ->[>pu1538 °C] 6 FeO + O2$$
References
- Günther, P. L.; Rehaag, H. Über Die Thermische Zersetzung von Oxalaten II. Mitteilung. Darstellung von Reinem Ferrooxyd. Z. Anorg. Allg. Chem. 1939, 243 (1), 60–68. https://doi.org/10/cqzgk8. (in German)
- Handbook of Preparative Inorganic Chemistry, 2nd ed.; Brauer, G., Ed.; Academic Press: New York; London, 1965; Vol. 2.
- R. A. Lidin, V. A. Molochko, and L. L. Andreeva, Reactivity of Inorganic Substances, 3rd ed.; Khimia: Moscow, 2000. (in Russian)
edited Jul 29 at 20:50
Buttonwood
10.6k1 gold badge22 silver badges46 bronze badges
10.6k1 gold badge22 silver badges46 bronze badges
answered Jul 28 at 22:31
andselisk♦andselisk
21.9k8 gold badges77 silver badges147 bronze badges
21.9k8 gold badges77 silver badges147 bronze badges
2
$begingroup$
That's an awesome answer :)
$endgroup$
– Hans
Jul 28 at 22:52
add a comment |
2
$begingroup$
That's an awesome answer :)
$endgroup$
– Hans
Jul 28 at 22:52
2
2
$begingroup$
That's an awesome answer :)
$endgroup$
– Hans
Jul 28 at 22:52
$begingroup$
That's an awesome answer :)
$endgroup$
– Hans
Jul 28 at 22:52
add a comment |
$begingroup$

The paper linked below indicates that the proper temperature is north of 535°C. This decomposition should be carried out with great caution though as some of the products might enflame, or even initiate a thermite reaction if carried out in the presence of Aluminum (as in the experimental setup used for the paper hereafter).
Source: https://pubs.rsc.org/en/content/articlelanding/2006/jm/b514565a#!divAbstract
$endgroup$
2
$begingroup$
The CO would give one pause, unless this was being done with proper facilities and safety equipment.
$endgroup$
– Ed V
Jul 28 at 21:06
1
$begingroup$
Agreed! Maybe with a way to vacuum extract the gases from the container once the decomposition has proceeded
$endgroup$
– Veritas
Jul 28 at 21:11
add a comment |
$begingroup$

The paper linked below indicates that the proper temperature is north of 535°C. This decomposition should be carried out with great caution though as some of the products might enflame, or even initiate a thermite reaction if carried out in the presence of Aluminum (as in the experimental setup used for the paper hereafter).
Source: https://pubs.rsc.org/en/content/articlelanding/2006/jm/b514565a#!divAbstract
$endgroup$
2
$begingroup$
The CO would give one pause, unless this was being done with proper facilities and safety equipment.
$endgroup$
– Ed V
Jul 28 at 21:06
1
$begingroup$
Agreed! Maybe with a way to vacuum extract the gases from the container once the decomposition has proceeded
$endgroup$
– Veritas
Jul 28 at 21:11
add a comment |
$begingroup$

The paper linked below indicates that the proper temperature is north of 535°C. This decomposition should be carried out with great caution though as some of the products might enflame, or even initiate a thermite reaction if carried out in the presence of Aluminum (as in the experimental setup used for the paper hereafter).
Source: https://pubs.rsc.org/en/content/articlelanding/2006/jm/b514565a#!divAbstract
$endgroup$

The paper linked below indicates that the proper temperature is north of 535°C. This decomposition should be carried out with great caution though as some of the products might enflame, or even initiate a thermite reaction if carried out in the presence of Aluminum (as in the experimental setup used for the paper hereafter).
Source: https://pubs.rsc.org/en/content/articlelanding/2006/jm/b514565a#!divAbstract
answered Jul 28 at 20:45
VeritasVeritas
2821 silver badge15 bronze badges
2821 silver badge15 bronze badges
2
$begingroup$
The CO would give one pause, unless this was being done with proper facilities and safety equipment.
$endgroup$
– Ed V
Jul 28 at 21:06
1
$begingroup$
Agreed! Maybe with a way to vacuum extract the gases from the container once the decomposition has proceeded
$endgroup$
– Veritas
Jul 28 at 21:11
add a comment |
2
$begingroup$
The CO would give one pause, unless this was being done with proper facilities and safety equipment.
$endgroup$
– Ed V
Jul 28 at 21:06
1
$begingroup$
Agreed! Maybe with a way to vacuum extract the gases from the container once the decomposition has proceeded
$endgroup$
– Veritas
Jul 28 at 21:11
2
2
$begingroup$
The CO would give one pause, unless this was being done with proper facilities and safety equipment.
$endgroup$
– Ed V
Jul 28 at 21:06
$begingroup$
The CO would give one pause, unless this was being done with proper facilities and safety equipment.
$endgroup$
– Ed V
Jul 28 at 21:06
1
1
$begingroup$
Agreed! Maybe with a way to vacuum extract the gases from the container once the decomposition has proceeded
$endgroup$
– Veritas
Jul 28 at 21:11
$begingroup$
Agreed! Maybe with a way to vacuum extract the gases from the container once the decomposition has proceeded
$endgroup$
– Veritas
Jul 28 at 21:11
add a comment |
Thanks for contributing an answer to Chemistry Stack Exchange!
- Please be sure to answer the question. Provide details and share your research!
But avoid …
- Asking for help, clarification, or responding to other answers.
- Making statements based on opinion; back them up with references or personal experience.
Use MathJax to format equations. MathJax reference.
To learn more, see our tips on writing great answers.
Sign up or log in
StackExchange.ready(function ()
StackExchange.helpers.onClickDraftSave('#login-link');
);
Sign up using Google
Sign up using Facebook
Sign up using Email and Password
Post as a guest
Required, but never shown
StackExchange.ready(
function ()
StackExchange.openid.initPostLogin('.new-post-login', 'https%3a%2f%2fchemistry.stackexchange.com%2fquestions%2f118606%2fwhat-is-the-most-convenient-way-to-prepare-ferrous-oxide-feo-in-the-laboratory%23new-answer', 'question_page');
);
Post as a guest
Required, but never shown
Sign up or log in
StackExchange.ready(function ()
StackExchange.helpers.onClickDraftSave('#login-link');
);
Sign up using Google
Sign up using Facebook
Sign up using Email and Password
Post as a guest
Required, but never shown
Sign up or log in
StackExchange.ready(function ()
StackExchange.helpers.onClickDraftSave('#login-link');
);
Sign up using Google
Sign up using Facebook
Sign up using Email and Password
Post as a guest
Required, but never shown
Sign up or log in
StackExchange.ready(function ()
StackExchange.helpers.onClickDraftSave('#login-link');
);
Sign up using Google
Sign up using Facebook
Sign up using Email and Password
Sign up using Google
Sign up using Facebook
Sign up using Email and Password
Post as a guest
Required, but never shown
Required, but never shown
Required, but never shown
Required, but never shown
Required, but never shown
Required, but never shown
Required, but never shown
Required, but never shown
Required, but never shown

4
$begingroup$
If you were an undergrad student, this would qualify as "homework": literature research. Are you? ;-)
$endgroup$
– Karl
Jul 28 at 20:11