Reproduction of the NaHCO3 method (ff ff method) with Celtic Sea Salt to obtain pure m-state material

Hello This is the Draft 1 for the Ff's Method.

I try to reproduce the method done by Panoramix. Instead of Dead Sea Salt (DSS) I used Celtic Sea Salt.

The one I used came from Germany: http://www.celticseasalt.com/product/fine-ground-celtic/


In the experiments we did several runs with 50, 100, 200, 250 grams of Salt dissolved in a saturated solution of NaHCO3 under different conditions.

I will try to explain the method I follow step by step. (We called it the Ff's Method)
But this Step by Step will also include lots of secondary experiments we did and their results.
This Secondary experiments are marked as (You dont need to do this step) but they will give some insight information for the researcher.
Some steps are missing also because the amount of secondary experiments was too much.
I will include those missing steps or I will Edit the Post to make it easier to follow depending on your feedback.


STEPS:


Step 0: Create a Saturated Solution of NaHCO3 (Sodium Bicarbonate) on a container of 2 to 5 Liters
You need Filtered Water or Distilled Water.
You need NaHCO3 (Sodium Bicarbonate)
For every liter of distilled water or filtered water you chose to use you are going to need around 96 grams of NaHCO3 at 20C.
So if you chose to make 5 Liters of the Saturated NaHCO3 you are going to need: 480 Grams of NaHCO3.
You can make this solutions with a balance to weight the NaHCO3 and a volumetric flask
OR
You can pick a container add some water and keep adding NaHCO3 until some of the NaHCO3 can not dissolve anymore.
When you reach the point of adding more NaHCO3 / Shake wait 5 minutes and there is still solid remaining you reached the point of a saturated solution. If your water can not dissolve anymore Sodium Bicarbonate (NaHCO3) you reached the point of SATURATION.
The solubility depends with the temperature:
http://mstate-research.nstars.org/t18-sodium-bicarbonate-nahco3


Step 1: I measure the ambient conditions because different parts of the world have different average temperatures and humidity.
This influence the solubility of NaHCO3 and the speed you can evaporate your solutions. The more humidity the longer it takes to evaporate your H2O2.

Humidity is relative high in my city around 80% or more and Temperature was around 25C.




Step 2: Weight 150 grams of Celtic Sea Salt. This was done with a balance of 0.01 mg accuracy but dont need to measure the amount with any accuracy at all. You can use any ammount you like.




Step 3: Put the amount of Celtic Sea Salt weighted on Step 2 on a glass container. We used an Erlenmeyer of 1000 ml but you can use a bigger Glass Beaker if you start with more Salt.




Step 4: Add the solution created on Step 0 (Saturated Sodium Bicarbonate Solution - NaHCO3) to the Beaker from Step 3.
You are going to need about 450 ml of the solution to dissolve 150 gr.
You are going to need about 600 ml of the solution to dissolve 200 gr.
Etc.




Step 5-6-7: Add Solution and Mix until you dissolve the salt or a little remains in the bottom part of the Beaker. If you need add more solution.








Step 8-9-10: The salt has some impurities so we need to filter the remaining solids.

Prepare the Funel and the Filter Paper (We used Technical White Filter Paper)


Filter


Difference in color/turbidity from the Original Solution and the Filtered One.


The Filtered Solution will start getting cloudy as the time goes by (fist steps of the creation of crystals)


Step 11: (You dont need to do this step) We measure the pH of the Saturated Solution of Sodium Bicarbonate (Step 0). pH 8.04




Step 12: (You dont need to do this step) We measure the pH of the Filtered Solution (Step 8 to 10). pH 7.29




Step 13: The Filtered solution starts to get Cloudy after a few minutes.




Step 14-20-21: We let the solution settle and slowly evaporate (open to the atmosphere). Slowly crystals began to form on the surface, on the walls of the Beaker and on the bottom. We did several experiments some in a dark room others exposed to the sun.
The ones exposed to the sun evaporated more quickly but the ones on the dark room created better shaped crystals.

Wall Crystals 14




Surface Crystals 14





Dark Room Crystals After 1 or 2 Weeks: 20




Dark Room Crystals After 4 or 5 Weeks: 21





Step 15: (You dont need to do this Step) We try to accelerate the formation of crystals using a Air Pump to inject Air during the night and see if the formation of Crystals speed up.

Air Pump


Glass Pan with the forming crystal on the Air Experiment



Step 16-17-18-19: (You dont need to do this Step). We Did a Parallel Experiment with Air Injection and Without Air Injection.

Two Beakers with the Same Salt and NaHCO3 Solution


One Beaker with the Air Injection (Left) and the one without the Air Injection (Right)


Top View Solutions Air Injected (Left) the other on the Right.


Side View Solutions Air Injected (Left) more crystals the other on the Right



Step 22: After 2 to 4 weeks more crystals grow on the surface and as they grow bigger some of them sunk in the bottom of the Beaker.








Step 23-24: Filter the Precipitate Formed (mstate crystals and impurities) we used a Buchner Filter

Buchner Filter


Crystals formed on the Bottom of the Beaker







Step 25: Filtered Crystals on the Bucher Filter



















Step 26: We put the Crystals from the previous step on a dry beaker and heat to 40C for several hours / days to dry the precipitate.






Step 27: Dry or Almost Dry crystals. Different Batchs.














Step 28: (You dont need to do this Step) We measure the weight of the dry mass of Crystals formed to have a yield on the process results.








Step 29: Grind or Powlder the Crystals obtained. Some crystals are like Paper or Cotton some are hard and crunchy.
The idea is to reduce the particle size because is easy to dissolve in the future step. We used a ceramic bowl and pestle.










Step 30: We put the grinded crystals in a flask 500ml.






Step 31-32: This step is DANGEROUS!!!. We added concentrated H2O2 75% (250 volumes) to the crystals on the flask of Step 30.
You need about 100 ml of H2O2 every 5 grams of crystals.
But this will change depending on the salt and how did you follow the previous steps.
H2O2 75% is dangerous because is one of the most powerful oxididants on Earth and also decompose to form H2O and O2 (oxigen).

Use Protective Glases, Nitrile Gloves and some protective cloths becouse it will bleach you cloths with a few drops.
BE EXTRA CAREFUL. READ THE MSDS SHEET Before working with concentrated H2O2.

According to Ff the H2O2 will make the mstate soluble and will let the carbonates and other impurites out of the solution.

Concentrated H2O2 75%. BE CAREFUL!. DON BE AFRAID. BE CAREFUL!.


Addition of H2O2 to the Crystals first minutes. No Bubbles or little bubbles.


Bubbles forming after a few minutes. Still Cold but temperature will rise quickly. Also I am wearing Nitrile Gloves to avoid the harmful efects of H2O2.









Step 33: Temperature Rise to quickly and the Decomposition of H2O2 is Catalized. You need to put the Beaker or Flask on a water Bath to reduce the speed of the reaction.

Reaction catalized by Temperature


Small Water Bath to reduce the speed of the reaction



Step 34:  After some time the reaction COULD or NOT slow down but normaly the water bath is needed for 48 hours.



Step 35: Some impurities may remain undisolved. You could add more H2O2 to see if they dissolve.
Sometimes they form strange paterns depending on the beaker/flask bottom, the ammount dissolved and the quantity of H2O2 added.






Step 36: Reaction Stoped after 3 days.




Step 37: Add some more H2O2 and filter the solution on White Techincal Filter Paper and a Funel.




Still some bubbles after filtration. The Decomposition of H2O2 is still catalized by something... maybe the mstate elements.
The Flask with H2O2 75% does not get bubbles only a few.






Step 42: After 3 days of the H2O2 reacting we start to evaporate the H2O2 on a Glass Beaker at 40C this process takes several days depending on the exposed Surface.






Step 43: Some precipitate formed. Surface and Bottom crystals.












Step 44: We evaporate a small portion on a glass pan forcing it with a Air Dryer and we obteined some surface crystals.
We add some distilled water and put it on another 500ml flask. The solid didnt dissolve after 3 days at 50C we keep adding water.




MORE EXPERIMENTS and Photos in the next week.

Added Some Videos:

Some Crystals were Like Paper some were more crunchy. Related to Step 26


Making the Powlder out of Crystals. Some of them Behave like Paper or Cotton: Related to Step 29


Decomposition of H2O2 with the mstate elements presents. Related to Step 31 to 34. H2O2 after 48 hs still bubbling.


Formation of Crystals in the Evaporation of H2O2. Related to Step 43.

Hay Mariano,

this is a great replication very well done,
very clear pictures, and videos as well

With love...
Panoramix