WET-METHOD PROCEDURE
Please read CAUTION!! and WARNING!! before proceeding.
First you need to prepare a dilute lye solution. Label an eyedropper bottle or squirt bottle "Lye-poison" so the bottle will not confused with something else. Work in a sink so that any spills will be contained. Lye gives off eye-stinging fumes when mixed with water. To avoid inhaling fumes, hold your breath and wear goggles while doing the following procedure.
Working over a sink, put 8 teaspoons of distilled water in a sturdy glass then stir in 1 teaspoon of lye. Stir until the lye is dissolved. Heat will be generated as the lye dissolves and the glass may get fairly hot. You may want to close your eyes to avoid eye-stinging fumes, taking a peek periodically.
Pour the lye solution into a labeled eyedropper bottle or squirt bottle.
If you are using pH paper, tear off several 1/4" pieces and put them on a piece of white paper on a plate.
For the best accuracy, recalibrate the pH paper throughout the day with changes in temperature and humidity, as well as day-to-day. Buffer solutions of pH 4, 7 and 10 will help with this. Sources of pH buffer solutions are listed near the end of this document under LAB SUPPLIES.
If you are using dried sea minerals, mix 1/2 cup of dry material with 2 cups of distilled water. This makes sea water. Now proceed as described below:
1. First, you might want to pour the sea water through a coffee filter to remove any scum.
2. If the starting material does not contain magnesium hydroxide (sea water does contain magnesium hydroxide), add some, or add a teaspoon of Epsom salts per gallon of water.
3. Pour the sea water into a stainless steel pot. Slowly, drop-by-drop, add the lye solution WHILE STIRRING. Every ten drops or so, test the pH. You might want to take at least 3 to 5 samples from different regions of the liquid. If you are using pH paper, the goal is to bring the pH up to 9.5, then stop to be on the safe side. If you are using a pH meter, stop just before you get to pH 10.78.
A white precipitate which includes m-state elements will form.
CAUTION: You must proceed slowly and patiently so that you do not exceed pH 10.78 with a meter or pH 9.5 with pH paper. If you go higher than pH 10.78, you might get a "Gilcrest precipitate" of toxic heavy metals. It is alleged that the Dead Sea salt water does not produce any Gilcrest precipitate. This has not been proven and should not be assumed.
4. Once you are at the correct pH, stop.
5. Pour the solution into a clean glass jar or test tube.
6. The white precipitate (slurry) slowly settles on the bottom of the jar. Let the slurry settle overnight. If metals or other toxins have been ruled out by prior testing of your starting material, the slurry is probably mostly calcium hydroxide, Mg(OH)2, lye, and a small amount of m-state.
You can speed this settling process with a centrifuge, which forces the precipitate to settle rapidly. Inexpensive second-hand centrifuges may be found at American Science and Surplus, http://www.sciplus.com.
7. Using a large syringe (or siphon), remove the liquid above the slurry.
8. Add distilled water to the precipitate (filling the jar), stir thoroughly, and let it settle again for at least 4 to 5 hours, preferably overnight.
9. Repeat steps 7 and 8 at least three times to thoroughly wash the precipitate. This should remove almost all of the lye. The remaining lye can be neutralized with HCl or distilled white vinegar as well. Washing three times is intended to reduce the dissolved "impurities" (like salt, for example) by 87.5%. Four washes would provide a 93.75% reduction, five washes a 96.875% reduction, and so on.
At this point, the precipitate is likely to contain some m-state, milk of magnesia Mg(OH)2, calcium, and perhaps some impurities.
Pour the precipitate and water into a stainless steel pot on a stove burner. A gas burner is preferred over electric because any magnetic fields from the electric burner may drive off some of the m-state material. Cover the pot with a lid to contain the m-state, and boil the solution for 5 minutes to sterilize it. Be careful not to spill the hot solution! Let it cool back to room temperature and recheck the pH to make sure it hasn't exceeded pH 9.
DISCUSSION: WHEN TO BOIL THE SOLUTION
In this document, we suggested that you not boil the solution until you have made the washed precipitate. However, boiling can be done earlier in the procedure with certain advantages. Here are four times that boiling could be done, with a discussion of the pros and cons of each:
1. Boil before adding lye solution.
PROS: Faster reaction, faster precipitation. CONS: You may spill the hot lye solution. You may inhale fumes.
2. Boil while adding lye solution.
PROS: Faster reaction, faster precipitation. CONS: You may spill the hot lye solution. You may inhale fumes. Danger of lye spurting out of pot. Not recommended.
3. Boil and cool after adding lye solution.
PROS: No danger of inhaling fumes. Little danger of spilling hot lye solution. CONS: Slower reaction, slower precipitation.
4. Boil the washed precipitate (recommended).
PROS: No danger of inhaling fumes. No danger of spilling hot lye solution. pH is unlikely to change after boiling because the reaction has already taken place. CONS: Slower reaction, slower precipitation. If safety is the main issue, this seems to be the best method.
Caution: If you boil the solution on an electric burner, the magnetic field in the burner may "blow off" some of the m-state materials, resulting in a small yield. This can be minimized by adding a source of sodium (such as sodium hydroxide or salt) to the solution before boiling.
Since sea water contains sodium in salt, none of the boiling methods will be a problem with sea water. However, if you are starting with low-sodium fresh water, add a sodium source (such as table salt or lye solution) before boiling.
Once the precipitate and water have been sterilized, the next step is required to concentrate the m-state.
HOW TO PURIFY YOUR PRECIPITATE
The precipitate made from sea water contains milk of magnesia (Mg(OH)2), which precipitates approximately around the same pH range that m-state does.
Here are four methods to separate Mg(OH)2 from m-state:
METHOD 1
1. Suppose you just made a precipitate by adding lye solution to sea water. The precipitate is m-state mixed with Mg(OH)2.
2. Use a syringe to remove the liquid over the precipitate, and discard the liquid. This leaves only the m-state/Mg(OH)2 precipitate.
3. To the wet precipitate, add hydrochloric acid (HCl) until you reduce the pH to 1.0 - 3.5. You can use muriatic acid (31% HCl) from a hardware store, but lab-grade HCl is less likely to be contaminated. A safe alternative to HCl is distilled white vinegar.
4. The white colloidal precipitate should dissolve, leaving a clear solution.
5. Add lye solution VERY SLOWLY drop-by-drop to bring the pH back up to 8.5 - 8.7. The precipitate that forms should be m-state mostly free of Mg(OH)2 (because m-state precipitates in this pH range, and Mg(OH)2 does not precipitate until pH 9.)
Note that your total yield may be diminished because you are not going past pH 8.7.
6. Remove the liquid above the precipitate, and wash the precipitate. It should be mostly m-state.
METHOD 2
This procedure removes the Mg(OH)2 by dissolving it below pH 9. First get some HCl (or muriatic acid) and coffee filters. A safer alternative to HCl is distilled white vinegar.
1. Dry the precipitate in a dark oven at about 275 degrees F for one or two hours. This forms a dry powder.
2. Take the dry powder and pulverize out any clumps.
3. In a glass container, cover the powder with some distilled water. For example, one liter of water for one cup of powder.
4. Add HCl or distilled white vinegar drop-by-drop to bring the pH to 5 or 6.
5. Shake the bottle and let it sit overnight. The dried m-state should not dissolve at that pH, but the Mg(OH)2 should dissolve.
6. The next day, after all the Mg(OH)2 has dissolved, pour everything into filter paper.
7. Wash the powder collected in the filter paper several times with distilled water to remove any residual traces of HCl or vinegar.
8. The washed powder may be oven-dried again at about 275 degrees F, and you should have m-state powder free of Mg(OH)2.
METHOD 3
1. Dry the original precipitate at about 200 degrees F.
2. Mix the resulting powder with distilled white vinegar or 30% HCl. Everything which does not dissolve in m-state. This will be quite a small amount if you start with sea water. (If you mix pure HCl with distilled water, remember: ADD ACID TO WATER, NEVER ADD WATER TO ACID).
3. Measure the amount of HCl/m-state solution (or vinegar/m-state solution).
4. Add distilled water to the HCl/m-state solution. Add an amount of water that is at least ten times the amount of HCl/m-state solution. (You may substitute distilled white vinegar for HCl).
5. Filter the solution through 5 layers of coffee filters.
6. Wash the powder at least three times in a large amount of distilled water.
METHOD 4
1. Starting with clean wet precipitate, add lye to bring the pH up to 12. The m-state precipitate will dissolve, but magnesium hydroxide and the Gilcrest precipitate will not.
2. Filter out the precipitate.
3. To the remaining liquid containing only m-state, add HCl or distilled white vinegar drop-by-drop until the pH reaches 8.5.
4. Add lye solution drop-by-drop to bring the pH back up to 10.78. The resulting precipitate should be only m-state.
5. Wash the precipitate as described earlier.
6. To be safe, check the pH of the precipitate slurry. It should be 9 or less before ingesting.