I figured since this is a random experiment threed then I may as well add random notes that I have been keeping here and there within reason of course. Alot of this may not make sence to anyone you but ill attempt to doctor it here and there to make it more readable. Understand much was written in a haste long ago and where written for my eyes and not anyone elses so any questions or corrections feel free to ask.
Cavone removal from Dill oil
28.7 * .15 = 4.305 apiol
28.7 * .552 = 15.8 carvone
28.7 * .166 = 4.7642 bylimonene
28.7 * .037 = .790
30gr h20
3+3+33311 bisulfite 114.2
30grm bs + DA + 50ml h2o
104.06 sBisulfite
15.9994 oxygen
1.00794 hydrogen
32.065 sulfur
81.07114 solfonic acid mol (=O)-SO2OH
H
/
R-C--OH
\
SO2Na
Addition of sodium bisulfite- a reaction formed from aldehydes and some ketones
saturated(40%)(aq) solution
Sodium nitrate from Ammonia nitrate and Sodium Bicarbonate
Na 23.00 g/mol
O 16.00 g/mol
C 12.01 g/mol
N 14.01 g/mol
H 1.00 g/mol
03 48.00 g/mol
NO3 62.01 g/mol
NH3 17.03 g/mol
Reagents and Materials Formula Molar Weight
-----------------------------------------------------------------------
28.8 grams sodium bicarbonate NaHCO3 84.007 g/mol
27.5 grams ammonia nitrate NH4NO3 80.043 g/mol
------
27.5 grams sodium nitrate. NaNO3 84.990 g/mol
2d attempt
-------------
79.3 grams ammonia nitrate
39.5 grams sodium hydroxide 39.997 g/mol
3d attempt
----------------
79.4 grams ammonia nitrate
83. grams of sodium bicarbonate
Results
-----------------
1: 27.5 grams sodium nitrate
2:
3: 74 grams sodium nitrate
discussion
----------------
1: product was a bright white when dried after some effort.27.5 grams it a little two high and makes me think that some bicarbonate contamination is in the mix because after a lose of NH3 and a
gain of Na there should be a net lose in the molar weight yet quantitive yeilds where observed.
2:lots of fizzing and very strong ammonia smell. It has come to my attention that the NaOH I was using was a mix of NaOH and KOH so the ratio will
be way to low for my liking so I will attempt another bicarbonate reaction.
After it had dried I added a very small portion of NaOH and the smell of ammonia became appearent so More conversion could be used because as it stands now it is a
mixture of sodium/potassium/ammonia nitrate.
After drying a small amount of NaOH solution was added and the smell of ammonia because quickly appearent so it it obvious that a total conversion did not take place.
Im going to slowly add more and dry and ad more and dry until i no longer smell NH3 from NaOH addition. Smells gone now but it has a hint of urinal smell
3: 2mm crystals precipitated and where dryed but there is some concern with H2O being traped within the crystal structure so i am going to grind it very fine and continue heating it.
Next phase:Sodium Nitrite
CaO 56.0774 g/mol
NaNO3 84.994669 g/mol
NaNO2 68.995267 g/mol
nitrite percent of nitrate = 81.175289%
nitrite = 18.824711% loss in weight
ammonia nitrate
------------------------
Molar mass 80.043 g/mol
Sodium bicarbonate
------------------------
Molar mass 84.007 g/mol
78.5
.980722%
82.38.
61.7 total bicarb
58.7 total NH3NO3
118.8 total weight of reactants
.734462
Urea/ammonia chloride seperation
NH4Cl 29.7 g/100 water at 0 °C
(NH2)2CO 108 g/100 water at (20 °C)
Mercuric Chloride
2.6gr Hg
52.1gr h2so4
---Heat--->20 minutes---->large SO2 production and irritating oder
White flat needles crystals on cooling.
Piperine to pipernol weight loss
piperine ----> pipernol = 52.6%
285.33766 150.13144
Mn(IV) Electrochemical Cell and other
------------------------------------------------------------------------------
H2SO4 = 98.08
MnO2 = 86.94
17.8
{======Neograviton quote=============================================================================================================================
Here is a easy way to do it with Mn(V)sulfate. A way I used many time!
1:First get some MnO2. You can buy it as "Manganese-Black" a pigment for cement and concrete. Thats about 70% MnO2.
2:Then put it in an equimolar amount of H2SO4 (100%) and heat it up. Make it really hot. (>200°C).
3:Let it be there for about half an hour. When I do this, I let The acid become so hot, that white steam comes out.
4:After that, let it cool down. You just have made Mn(V)SO4. It is soluble in 37% H2SO4 (battery acid) with a deep, chocolate like brown color.
5:After that put it 1:1 with the toluene in about 60% H2SO4 (enough H2SO4, so that nearly everything dissolves).
6:Heat (or cool) it to about 50-60°C and stirr it well. After 3-4 hours you will have mostly Benzaldehyd (in my cases about 70%)
7:Distill the Benzaldehyd/Toluene out by a simple steam distillation. (Just boil water out, until there is no oily layer any more)
When you start boiling that stuff, the color of the liquid becomes sand-like. Thats because the rest of the Mn(V)SO4 breaks down to Mn(II)SO4.
And now the best: just put the liquid in a electrolytic cell (in the anode-part) and put some electricity through it, while stirring.
The color will chance to chocolate brown once again, and you can use it again!!! About 6 times!
================================================================================================================================================}
100 grams 93% H2SO4 = 93 grams H2SO4 = .9482 mol per 100 grams.
100/.93% = 107.526 grams H2SO4
1.1281 grams 93% H2SO4 per 1 gram MnO2
95.313 grams MnO2
==============================================================================
------------------------------------------------------------------------------
20 grams MnO2 added to 22 grams H2SO4
Sodium acetate / bisulfate to acetic acid
120.6 sodium bisulfate 66.359%
82.03 sodium acetate. .2438
25.3700 grams sodium bisulfite
20 grams of sodium acetate = 14 grams acetic acid = 15.35817822 ml acetic acid from 20 grams of pure (anhy)sodium acetate
.2438
sodium acetate -- > acetic acid === 73.2039% weight kept from the conversion/
Ethyl Bromide synthesis
Materials
----------------------------------
NaBr
Molar mass 102.894 g/mol / 53 = .5150
H2SO4
Molar mass 98.08 g/mol * .5150= 50.5112 grams
C2H6O
Molar mass 46.07 g/mol * .5150 = 23.726
--------------------------------------------
HBr
Molar mass 80.91 g/mol
--------------------------------------------
==============================
Products
----------
C2H5Br
Molar mass 108.97 g/mol * .5150 = 56.1195
H2O
Molar mass 18.01528(33) g/mol * 2 = 36.03056 * .2526 = 9.10
NaHSO4
Molar mass 120.06 g/mol
==============================================
2NaBr + H2SO4 = Na2SO4 + 2HBr
2EtOH + 2HBr = 2EtBr + 2H2O
==============================================
Based on 52 gram pack of NaBr
-----------------------------------
52grams NaBr / 1mol NaBr = 50.53%
1mol H2SO4 * 50.53% = 49.55 grams H2SO4 / 2 = 24.775 grams H2SO4
1mol EtOH * 50.53% = 23.2791 grams EtOH
==============================================
Conclusion
------------------------
IN
---
NaBr = 52
H2SO4 = 49.559 grams
EtOH = 23.279 grams
Equals 100.0469 grams
========================
OUT
---
EtBr = 55.051 grams * 1.14(density) = 62.7ml
Na2SO4 = 35.886
H2O = 9.1031grams
Equals 100.0401
==============================================
EtBr boiling point = 102 degrees F
EtOH Bp = 173 degrees F
Dibromoethane
NaBr + H2SO4 = HBr + NaHSO4
HBr + C2H4(OH)2 = H2O + C2H4(Br)2
Materials / Total mass in 396.008
----------------------------------
H2SO4
Molar mass 98.08 g/mol * .5053 = 49.55 grams
NaBr
Molar mass 102.894 g/mol / 52 grams = 50.53%
--------------------------------------------
Na2SO4
Molar mass 142.04 g/mol (anhydrous)
HBr
Molar mass 80.91 g/mol * .5053 = 40.883 grams
C2H4(OH)2
Molar mass 62.068 g/mol * .5053 = 31.362 grams
49.55 grams of H2SO4 and 20 grams of H2O is added to 31.362 grams Ethylene Glycol. 52 grams of finely powdered Sodium Bromide is added and reaction is stirred until sodium bromide is consumed. Dibromoethane distills over at 131-132 °C.
EtOH placed into a cold water bath and 130 grams of 45% H2SO4 was added slowly via dropper seringe over a 10 minute period inorder to keep the heat down
KI tablets Iodine extraction
---------------
active
---------
120 pills*
84mg calcium 10.08 grams calcium : as dibasic phosphate#Solubility: Practically insoluble in water.
32.5 mg = 3900mg KI : Solubility in water 128 g/100 ml (6 °C)
Inactive
--------------
dibasic calcium phosphate
steric acid
mod cellouse gum
magnesium stearate.
35.8 grams 150ml Distilled H2o
Time 1:20
200 ml total after addition to wash remaining calcium phosphate.
evaperation reduced to dryness
2.7 grams yeild yellow powder sticky when damp.
Ammonia Methyl Sulfate
50.1 grams of Sulfamic acid
105 ml of MeOH.
Refluxed N? Hours
As you can see much is incomplete due to the fact that I find paper notes more rewarding but now and then I need to figure up a quick number or two and save it there.
Cavone removal from Dill oil
28.7 * .15 = 4.305 apiol
28.7 * .552 = 15.8 carvone
28.7 * .166 = 4.7642 bylimonene
28.7 * .037 = .790
30gr h20
3+3+33311 bisulfite 114.2
30grm bs + DA + 50ml h2o
104.06 sBisulfite
15.9994 oxygen
1.00794 hydrogen
32.065 sulfur
81.07114 solfonic acid mol (=O)-SO2OH
H
/
R-C--OH
\
SO2Na
Addition of sodium bisulfite- a reaction formed from aldehydes and some ketones
saturated(40%)(aq) solution
Sodium nitrate from Ammonia nitrate and Sodium Bicarbonate
Na 23.00 g/mol
O 16.00 g/mol
C 12.01 g/mol
N 14.01 g/mol
H 1.00 g/mol
03 48.00 g/mol
NO3 62.01 g/mol
NH3 17.03 g/mol
Reagents and Materials Formula Molar Weight
-----------------------------------------------------------------------
28.8 grams sodium bicarbonate NaHCO3 84.007 g/mol
27.5 grams ammonia nitrate NH4NO3 80.043 g/mol
------
27.5 grams sodium nitrate. NaNO3 84.990 g/mol
2d attempt
-------------
79.3 grams ammonia nitrate
39.5 grams sodium hydroxide 39.997 g/mol
3d attempt
----------------
79.4 grams ammonia nitrate
83. grams of sodium bicarbonate
Results
-----------------
1: 27.5 grams sodium nitrate
2:
3: 74 grams sodium nitrate
discussion
----------------
1: product was a bright white when dried after some effort.27.5 grams it a little two high and makes me think that some bicarbonate contamination is in the mix because after a lose of NH3 and a
gain of Na there should be a net lose in the molar weight yet quantitive yeilds where observed.
2:lots of fizzing and very strong ammonia smell. It has come to my attention that the NaOH I was using was a mix of NaOH and KOH so the ratio will
be way to low for my liking so I will attempt another bicarbonate reaction.
After it had dried I added a very small portion of NaOH and the smell of ammonia became appearent so More conversion could be used because as it stands now it is a
mixture of sodium/potassium/ammonia nitrate.
After drying a small amount of NaOH solution was added and the smell of ammonia because quickly appearent so it it obvious that a total conversion did not take place.
Im going to slowly add more and dry and ad more and dry until i no longer smell NH3 from NaOH addition. Smells gone now but it has a hint of urinal smell
3: 2mm crystals precipitated and where dryed but there is some concern with H2O being traped within the crystal structure so i am going to grind it very fine and continue heating it.
Next phase:Sodium Nitrite
CaO 56.0774 g/mol
NaNO3 84.994669 g/mol
NaNO2 68.995267 g/mol
nitrite percent of nitrate = 81.175289%
nitrite = 18.824711% loss in weight
ammonia nitrate
------------------------
Molar mass 80.043 g/mol
Sodium bicarbonate
------------------------
Molar mass 84.007 g/mol
78.5
.980722%
82.38.
61.7 total bicarb
58.7 total NH3NO3
118.8 total weight of reactants
.734462
Urea/ammonia chloride seperation
NH4Cl 29.7 g/100 water at 0 °C
(NH2)2CO 108 g/100 water at (20 °C)
Mercuric Chloride
2.6gr Hg
52.1gr h2so4
---Heat--->20 minutes---->large SO2 production and irritating oder
White flat needles crystals on cooling.
Piperine to pipernol weight loss
piperine ----> pipernol = 52.6%
285.33766 150.13144
Mn(IV) Electrochemical Cell and other
------------------------------------------------------------------------------
H2SO4 = 98.08
MnO2 = 86.94
17.8
{======Neograviton quote=============================================================================================================================
Here is a easy way to do it with Mn(V)sulfate. A way I used many time!
1:First get some MnO2. You can buy it as "Manganese-Black" a pigment for cement and concrete. Thats about 70% MnO2.
2:Then put it in an equimolar amount of H2SO4 (100%) and heat it up. Make it really hot. (>200°C).
3:Let it be there for about half an hour. When I do this, I let The acid become so hot, that white steam comes out.
4:After that, let it cool down. You just have made Mn(V)SO4. It is soluble in 37% H2SO4 (battery acid) with a deep, chocolate like brown color.
5:After that put it 1:1 with the toluene in about 60% H2SO4 (enough H2SO4, so that nearly everything dissolves).
6:Heat (or cool) it to about 50-60°C and stirr it well. After 3-4 hours you will have mostly Benzaldehyd (in my cases about 70%)
7:Distill the Benzaldehyd/Toluene out by a simple steam distillation. (Just boil water out, until there is no oily layer any more)
When you start boiling that stuff, the color of the liquid becomes sand-like. Thats because the rest of the Mn(V)SO4 breaks down to Mn(II)SO4.
And now the best: just put the liquid in a electrolytic cell (in the anode-part) and put some electricity through it, while stirring.
The color will chance to chocolate brown once again, and you can use it again!!! About 6 times!
================================================================================================================================================}
100 grams 93% H2SO4 = 93 grams H2SO4 = .9482 mol per 100 grams.
100/.93% = 107.526 grams H2SO4
1.1281 grams 93% H2SO4 per 1 gram MnO2
95.313 grams MnO2
==============================================================================
------------------------------------------------------------------------------
20 grams MnO2 added to 22 grams H2SO4
Sodium acetate / bisulfate to acetic acid
120.6 sodium bisulfate 66.359%
82.03 sodium acetate. .2438
25.3700 grams sodium bisulfite
20 grams of sodium acetate = 14 grams acetic acid = 15.35817822 ml acetic acid from 20 grams of pure (anhy)sodium acetate
.2438
sodium acetate -- > acetic acid === 73.2039% weight kept from the conversion/
Ethyl Bromide synthesis
Materials
----------------------------------
NaBr
Molar mass 102.894 g/mol / 53 = .5150
H2SO4
Molar mass 98.08 g/mol * .5150= 50.5112 grams
C2H6O
Molar mass 46.07 g/mol * .5150 = 23.726
--------------------------------------------
HBr
Molar mass 80.91 g/mol
--------------------------------------------
==============================
Products
----------
C2H5Br
Molar mass 108.97 g/mol * .5150 = 56.1195
H2O
Molar mass 18.01528(33) g/mol * 2 = 36.03056 * .2526 = 9.10
NaHSO4
Molar mass 120.06 g/mol
==============================================
2NaBr + H2SO4 = Na2SO4 + 2HBr
2EtOH + 2HBr = 2EtBr + 2H2O
==============================================
Based on 52 gram pack of NaBr
-----------------------------------
52grams NaBr / 1mol NaBr = 50.53%
1mol H2SO4 * 50.53% = 49.55 grams H2SO4 / 2 = 24.775 grams H2SO4
1mol EtOH * 50.53% = 23.2791 grams EtOH
==============================================
Conclusion
------------------------
IN
---
NaBr = 52
H2SO4 = 49.559 grams
EtOH = 23.279 grams
Equals 100.0469 grams
========================
OUT
---
EtBr = 55.051 grams * 1.14(density) = 62.7ml
Na2SO4 = 35.886
H2O = 9.1031grams
Equals 100.0401
==============================================
EtBr boiling point = 102 degrees F
EtOH Bp = 173 degrees F
Dibromoethane
NaBr + H2SO4 = HBr + NaHSO4
HBr + C2H4(OH)2 = H2O + C2H4(Br)2
Materials / Total mass in 396.008
----------------------------------
H2SO4
Molar mass 98.08 g/mol * .5053 = 49.55 grams
NaBr
Molar mass 102.894 g/mol / 52 grams = 50.53%
--------------------------------------------
Na2SO4
Molar mass 142.04 g/mol (anhydrous)
HBr
Molar mass 80.91 g/mol * .5053 = 40.883 grams
C2H4(OH)2
Molar mass 62.068 g/mol * .5053 = 31.362 grams
49.55 grams of H2SO4 and 20 grams of H2O is added to 31.362 grams Ethylene Glycol. 52 grams of finely powdered Sodium Bromide is added and reaction is stirred until sodium bromide is consumed. Dibromoethane distills over at 131-132 °C.
EtOH placed into a cold water bath and 130 grams of 45% H2SO4 was added slowly via dropper seringe over a 10 minute period inorder to keep the heat down
KI tablets Iodine extraction
---------------
active
---------
120 pills*
84mg calcium 10.08 grams calcium : as dibasic phosphate#Solubility: Practically insoluble in water.
32.5 mg = 3900mg KI : Solubility in water 128 g/100 ml (6 °C)
Inactive
--------------
dibasic calcium phosphate
steric acid
mod cellouse gum
magnesium stearate.
35.8 grams 150ml Distilled H2o
Time 1:20
200 ml total after addition to wash remaining calcium phosphate.
evaperation reduced to dryness
2.7 grams yeild yellow powder sticky when damp.
Ammonia Methyl Sulfate
50.1 grams of Sulfamic acid
105 ml of MeOH.
Refluxed N? Hours
As you can see much is incomplete due to the fact that I find paper notes more rewarding but now and then I need to figure up a quick number or two and save it there.