Fe2O3Extract - Revision history

NebarnixWikiSysop: /* Isolation Procedure */

2018-07-06T13:14:54Z

Isolation Procedure

NebarnixWikiSysop: /* Isolation Procedure */

2018-07-06T13:12:57Z

Isolation Procedure

NebarnixWikiSysop: /* Isolation Procedure */

2018-06-23T15:33:18Z

Isolation Procedure

NebarnixWikiSysop: /* Isolation Procedure */

2018-06-23T15:32:09Z

Isolation Procedure

NebarnixWikiSysop: /* Isolation */

2018-06-22T15:04:20Z

Isolation

NebarnixWikiSysop at 14:10, 22 June 2018

2018-06-22T14:10:39Z

NebarnixWikiSysop: /* Isolation Procedure */

2018-06-22T13:54:12Z

Isolation Procedure

NebarnixWikiSysop at 13:50, 22 June 2018

2018-06-22T13:50:34Z

NebarnixWikiSysop: /* Isolation Procedure */

2018-06-20T15:11:56Z

Isolation Procedure

NebarnixWikiSysop at 15:07, 20 June 2018

2018-06-20T15:07:34Z

@@ Line 82: / Line 82: @@
 #* Clays should be light colored and no longer red.
 # Add 50g of oxalic acid dihydrate OR 410 mL of a 1M solution.
-#* No reaction should occur.
+#* No immediate reaction should occur.
 # Place resulting solution into the sunlight or expose to short wave UV light until it turns from brown orange to yellow green.
 #* Gasses will be generated (CO2). Allow gasses to vent, do NOT seal flask!
 #* If liquid turns black coffee colored the solution is likely saturated with CO2 gas which has stopped the photoreaction.
-#** Agitate or provide nucleation sites in the presence of sunlight.
+#** Agitate or provide nucleation sites in the presence of sunlight to allow CO2 to offgas.
 # Either dry in a fume hood or distill off liquid.
 #* Solution will have >50% excess of HCl due to Ph dependent solubility of Fe2O3.

@@ Line 101: / Line 101: @@
 #* Areas of the solid may turn brownish red until decomposition temperature is reached
 #* A runaway reaction will occur converting the iron(II) oxalate to pyrophoric iron
 #* Under adequate stirring the pyrophoric iron Will oxidize to form red Fe2O3.
 # Grind or mill to fine consistency.
 # Win!

@@ Line 86: / Line 86: @@
 #* Gasses will be generated (CO2). Allow gasses to vent, do NOT seal flask!
 #* If liquid turns black coffee colored the solution is likely saturated with CO2 gas which has stopped the photoreaction.
-#** Agitate or provide nucleation sides and allow to offgas in the presence of sunlight.
+#** Agitate or provide nucleation sites in the presence of sunlight.
 # Either dry in a fume hood or distill off liquid.
 #* Solution will have >50% excess of HCl due to Ph dependent solubility of Fe2O3.

@@ Line 78: / Line 78: @@
 # Boil for 30 minutes under reflux.
 #* Liquid will turn reddish brown.
-# Filter out clays and insoluble substances once cooled. Liquid will be tea colored.
+# Filter out clays and insoluble substances once cooled.
 #* Clays should be light colored and no longer red.
 # Add 50g of oxalic acid dihydrate OR 410 mL of a 1M solution.
 #* No reaction should occur.
 # Place resulting solution into the sunlight or expose to short wave UV light until it turns from brown orange to yellow green.
 # Either dry in a fume hood or distill off liquid.
 #* Solution will have >50% excess of HCl due to Ph dependent solubility of Fe2O3.

@@ Line 64: / Line 64: @@
 == Isolation ==
-In order to isolate the iron from the soil mixtures, we must digest then selectively precipitate out the iron. HCl will ingest metallic iron, iron(II), and iron(III) compounds. Much of the HCl can be recovered and used again in the next cycle.
+In order to isolate the iron from the soil mixtures, we must digest then selectively precipitate out the iron. HCl will ingest metallic iron, iron(II), and iron(III) compounds. UV light will reduce the iron(III) to iron(II). Iron (II) Oxalate is not soluble in water and will precipitate out. Much of the HCl can be recovered and used again in the next cycle.
 The process goes like this, in summary:

@@ Line 27: / Line 27: @@
 # (1 - ((Mtotal - Mfilter) / 2.000)) x100% = Percent Soluble Material
 * Note that this is an upper bound to the iron oxide percentage, but could also contain other acid soluble metals and compounds such as nickel, aluminum, copper oxides, etc.
 == Isolation ==

@@ Line 49: / Line 49: @@
 #* No reaction should occur.
 # Place resulting solution into the sunlight or expose to short wave UV light until it turns from brown orange to yellow green.
-# Dry in a fume hood.
+# Either dry in a fume hood or distill off liquid.
-#* Solution will have a 50% excess of HCl due to Ph solubility of Fe2O3.
+#* Solution will have >50% excess of HCl due to Ph dependent solubility of Fe2O3.
 #** Distill this excess off to recover and recycle or boil to NEARLY dry
 #** Take into account HCl vapors that will form!
-#* Do NOT allow to fully dry under heat or exothermic decomposition will occur!!
+#* '''Do NOT allow to fully dry under heat or exothermic decomposition will occur!!'''
 #* Yellow crust will form.
 # Add 200mL of H2O to yellow brown crust and bring to a boil then let cool.
 #* This is to dissolve water soluble impurities.
 # Filter off yellow solid and dry.
-# Add yellow solid iron(II) oxalate to crucible or pan. Break up clumps and "fluff" to allow adequate oxygen supply. Heat to 250 degrees C while stirring to ensure adequate oxygenation during decomposition. Areas of the solid may turn brownish red until decomposition temperature is reached, when a runaway reaction will occur converting the iron(II) oxalate to pyrophoric iron, which will oxidize under stirring to form red Fe2O3.
+# Add yellow solid iron(II) oxalate to crucible or pan.
 # Grind or mill to fine consistency.

@@ Line 32: / Line 32: @@
 # Add 150mL of H2O to 33g of Fe2O3 in a boiling flask
 # Add 200mL of 10M (32%) HCl
-* The acid is diluted to the azeotropic point (6M) to prevent nasty vapors from escaping the reflux column
+#* The acid is diluted to the azeotropic point (6M) to prevent nasty vapors from escaping the reflux column
-# Boil for 30 minutes under reflux. Liquid will turn reddish brown.
+# Boil for 30 minutes under reflux.
-# Filter out clays and insoluble substances once cooled. Liquid will be tea colored. Clays should be light colored and no longer red.
+#* Liquid will turn reddish brown.
-# Add 50g of oxalic acid dihydrate OR 410 mL of a 1M solution. No reaction should occur.
+# Filter out clays and insoluble substances once cooled. Liquid will be tea colored.
 # Place resulting solution into the sunlight or expose to short wave UV light until it turns from brown orange to yellow green.
-# Solution will have a 50% excess of HCl due to Ph solubility of Fe2O3. Distill this excess off to recover and recycle or boil to NEARLY dry in a fume hood. Yellow crust will form.
+# Dry in a fume hood.
-# Add 200mL of H2O to yellow brown crust and bring to a boil then let cool to dissolve water soluble impurities.
+#* Solution will have a 50% excess of HCl due to Ph solubility of Fe2O3.
-# Filter off yellow solid and dry.
+#** Distill this excess off to recover and recycle or boil to NEARLY dry
-# Add yellow solid iron(II) oxalate to crucible. Break up and clumps and allow adequate air supply. Heat to 250 degrees C while stirring to ensure adequate oxygenation during decomposition. Areas of the solid may turn brownish red until decomposition temperature is reached, when a runaway reaction will occur converting the iron(II) oxalate to pyroforic iron, which will oxidize under stirring to form red Fe2O3.
+#** Take into account HCl vapors that will form!
 # Grind or mill to fine consistency.

@@ Line 16: / Line 16: @@
 # Measure 2.000g of Sample
-# Add 25mL HCL (10M) to Sample in a 250mL flask
+# Add 25mL HCl (10M) to Sample in a 250mL flask
 # Boil for 20 minutes
 # (Optional) Dry filter paper at 105 degrees C
@@ Line 27: / Line 27: @@
 # (1 - ((Mtotal - Mfilter) / 2.000)) x100% = Percent Soluble Material
 * Note that this is an upper bound to the iron oxide percentage, but could also contain other acid soluble metals and compounds such as nickel, aluminum, copper oxides, etc.