the extraction of the sulphur of iron via citrus fruit & citric acid

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The Extraction of the

Sulphur of Iron via Citrus

Fruit & Citric Acid

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Written by L.C. Kennedy

Copyright © VITRIOLUM Publishing. All Rights Reserved.

May not be copied, shared, or reproduced in any manner without

expressed written consent from the author, and VITROLUM

Publishing.

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The sulphur of iron is relatively easy to obtain using a variety of different processes,

menstruums, acids, etc. In this guide the author will attempt to explain the theory &

process of opening & extracting the sulphur from two forms of red iron oxide (synthetic

red iron oxide jeweler‟s rouge & natural red hematite pigment powder) via the juice of

lemons, and pure citric acid.

Please note: we are not only limited to iron in this process, but a number of

different metals/materials may be used.

Background Information & Theory:

The opening of a metal can be carried out with an organic acid (once the metal

has been opened we can obtain the metallic sulphur principle). Organic acids are called

carboxylic acids in the realm of organic chemistry (containing the COOH functional

group). Two forms of organic acids exist: liquid, and solid (e.g. unfixed and fixed). An

unfixed (liquid) organic acid is acetic acid. A fixed (solid) acid is citric acid. This process

focuses on the fixed solid organic citric acid.

Citric acid was “discovered” and used by the 8th

century Persian alchemist Geber

(Jabir Ibn Hayyan). It occurs throughout the vegetable & animal kingdoms. It is found

most abundantly in citrus fruits (lemons, limes, oranges, etc). Citric acid plays a vital role

in energy metabolism of all life (this is called the citric acid cycle). Chemically speaking,

citric acid forms citrate salts when added to bases/alkalis (e.g. sodium citrate, magnesium

citrate, calcium citrate, potassium citrate).

When choosing our starting materia we must choose a matter that does not readily

react with citric acid. We do not want to form a citrate salt via the normal chemical route!

The test to determine if a starting material is appropriate is quite simple. One way to test

for this type of reaction is by adding a concentrated solution of citric acid, or lemon juice

to your chosen starting material. A reaction should not occur upon addition; no color

change should be evident, and no air component evolution should occur (even upon

heating).

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If no reaction occurs the matter can be utilized for this process! A wide variety of

materials can be used. We choose red iron oxide for the ease of demonstrating this

process. This will even work with gold (use gilding leaf)!

The process itself is somewhat straightforward. A concentrated solution of

lemon/citrus juice, or pure citric acid is added to your chosen powdered starting material.

The solution is stirred, and brought to a boil. Boil it down gently until completely dry.

Care must be taken to not burn the coagulated red resin-like mass that is obtained at the

moment when dehydration is complete! Once complete, the flask is removed from the

heat source, and allowed to cool.

Once cooled, enough water is added to completely dissolve the hard resin-like

mass (hot water helps dissolution). To ease dissolution, the hard resin-like mass can be

ground to a powder in a glass mortar & pestle. A glass stirring rod may also be used to

break apart the mass.

After the solubilized portion has completely dissolved, the solution is shaken, and

allowed to settle. The red iron oxide particles will settle to the bottom of the flask. Once

settled, take note of the amount of tincture drawn from the material (note the color of the

liquid). Tip: we advise taking a picture at the end of each boil-down in order to compare

the actual color of the tincture with previous boil-downs.

The first boil-down will yield a relatively mild-colored tincture. The boil-down

process needs to be reiterated a number of times (seven or more – this is up to you) in

order for the matter to be fully opened, and the sulphur to be completely drawn from the

body. The matter is opened more and more with each boil-down.

When no more tincture is drawn from the matter, we can decant/filter the sulphur

tincture from the dead body. The empty shell can be saved, or discarded. We recommend

saving the body for future experimentation/use. Be sure to label it appropriately („empty

body/shell of iron‟).

Process in Practice:

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Below we attempt to give a moderately detailed explanation of the process. We

use 100% pure crystalline food-grade citric acid dissolved in water, and the juice of citrus

fruits (lemons & limes contain the highest concentration of citric acid).

Materials Needed: Food-grade citric acid, citrus fruits (lemons, limes, oranges,

grapefruits, etc), red iron oxide (natural from crushed hematite, and synthetic jeweler‟s

rouge), glass stirring rod, glass mortar & pestle, beakers, Erlenmeyer flasks, and a hot-

plate/heating element.

1. A) Make concentrated solution of citric acid. Add 36.5g citric acid to 50ml of

distilled water, and stir/shake until completely dissolved. Label as ’100% pure

citric acid concentrate solution,‟ and sit aside.

B) Obtain juice from citrus fruits. Take a quantity of fresh lemons (any citrus fruit

may be use), squeeze the juice from each, and filter. We need 40ml of undiluted

lemon juice. Use as many lemons as needed to obtain 50ml of juice. Label as

„Freshly squeezed lemon juice concentrate,‟ and sit aside.

2. Weigh two 4g quantities of your chosen red iron oxide containing material (a ratio

of 1g red iron oxide per 10ml of citric acid/lemon juice). We use natural hematite

powder pigment in our lemon juice experiment, and synthetic jewelers rouge in

~100% citric acid solution.

3. Pour 40ml of concentrated citric acid solution into one beaker, and freshly

squeezed lemon juice concentrate into another beaker. Label if needed.

4. Add both of the previously weighed 4g quantities of red iron oxide into two

separate Erlenmeyer flasks (100ml or 250ml). Label one flask as „Martian citric

acid tincture,‟ and the other as „Martian lemon juice tincture.‟

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5. Add 40ml of lemon juice concentrate previously measured in step 3 into one

flask, and 40ml citric acid concentrate solution into the other. Stir well using the

stirring rod to break up any clumps (shake if needed). Let settle.

6. After the red iron oxide particles have settled, take note of the color of the

solution. No tincture should be drawn from the starting matter at this point, and

no visible reaction should occur! We recommend taking pictures at this step in

order to document the color/amount of tincture drawn with each and every

iteration of the boil-down process.

7. Place each flask on a hot-plate/heating mantle, and slowly bring to a boil. The

water/moisture needs to be boiled off over the course of a couple of hours. Be

sure to watch the process carefully. When the boil-down process is nearing

completion a red thick gel-like mass will be obtained. Be sure to not burn this

mass! Swirl the flask around if needed in order to prevent burning. Once the water

has been completely boiled off, take it off the burner, and let cool. It will solidify

into a hard resin-like mass.

8. Break apart the red iron oxide resin mass using a glass stirring rod. Take it out of

the flask, and add to a glass mortar & pestle. Grind well until completely

pulverized. Be sure to note which resin material came from which flask (citric

acid versus lemon juice). Also, be sure to wash the mortar & pestle after you‟ve

finished powdering the material from one flask, and before powdering the other

(i.e. do not cross-contaminate products!).

9. Add the pulverized resin powders to the appropriate flask (reuse the labeled flasks

from above). Pour 40ml of water in each flask, and stir well using a glass stirring

rod until the soluble portion is completely dissolved. Let settle.

10. Take note of the amount of tincture drawn from the red iron oxide containing

material. Take a picture if needed. Reiterate the boil-down process as many times

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as needed to completely open & draw out the tincture from the matter (this means

go back to step 7, and carry out steps 7-10 as many times as needed until no more

tincture is drawn from the body).

11. After the final boil-down iteration, decant/filter the tincture from the dead Martian

body. Pour the lemon juice tincture into a bottle labeled „Martian-sulphur lemon

juice tincture,‟ and the citric acid tincture into a bottle labeled „Martian-sulphur

citric acid tincture.‟ The process is complete! Save the iron body for possible

future experimentation.

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Images of various steps in this process are included below.

Note: The first set of images is with a concentrated citric acid solution, and the

second set is with a lemon juice concentrate. A small description is included below each

image.

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Fig 1. – 4g red iron oxide jeweler‟s rouge in 250ml Erlenmeyer flask.

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Fig 2. – Approximately 100ml of 100% pure citric acid solution added to the red iron

oxide jeweler‟s rouge. Please use 40ml as called for in the process.

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Fig 3. – Final stage of boil-down dehydration. It possesses a thick gum/gel-like

consistency due to only a very small amount of water remaining.

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Fig 4. – First boil-down is complete! The mass is completely dry. Please note the rich

color indicating that the mass was not burned at all. The flask was swirled to prevent

hotspots/burning of the matter.

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Fig 5. – A quantity of water was added to the dried powdered matter. Any amount of

water can be added as indicated in this image (we added approximately 250ml distilled

water). Use 40ml distilled water as called for in the process.

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Fig 6. – After the soluble portion has dissolved it is allowed to sit. Iron oxide particles

will settle to the bottom.

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Fig 7. – Taken approximately one hour after the previous image. More iron oxide has

settled.

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Fig 8. – The iron oxide has completely settled (it was allowed to sit overnight). The liquid

should be clear & brilliantly transparent. This image is indicative of the amount of

tincture drawn after the first boil-down.

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Fig 9. – The tincture from the first boil-down is shown above after being

decanted/filtered. We see the brilliant orange Martian sulphur quite well in this image!

Please note that we only decanted/filtered in order to show the student what the tincture

looks like after the first boil-down. There‟s no need to decant/filter when reiterating the

boil-down process each time.

---- End of First Image Set ----

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Fig 10 & 11. – Natural iron oxide hematite pigment powder on the left, and various citrus

fruits on the right.

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Fig 12. – 4g natural iron oxide hematite pigment powder has been measured. Note: does

not include the weight of weighing dish (the digital scale was tared).

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Fig 13. – 40ml freshly squeezed lemon juice (filtered).

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Fig 14. – 4g natural red iron oxide hematite pigment powder in 250ml Erlenmeyer flask

on left, and 40ml freshly squeezed filtered lemon juice on right.

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Fig 15. – 40ml lemon juice was added to 4g of hematite in the flask. The contents were

stirred with a glass stirring rod to completely break apart all clumps. Please note that no

real reaction has occurred. The color is simply due to colloidal/finely divided powder

being suspended in the lemon juice concentrate.

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Fig 16. – End of the first boil-down iteration.

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Fig 17. – Another image of the mass at the end of the first boil-down iteration.

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Fig 18. – Approximately 80ml of distilled water was added to the powdered mass from

above. The soluble portion was completely dissolved, and the insoluble portion has

settled. Please use 40ml as noted in the original process to avoid confusion.

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Fig 19. – Another image.

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Fig 20. – The tincture of the hematite pigment powder was filtered, and poured into a

clean 250ml Erlenmeyer flask. Enough water was added to bring it to the 250ml mark.

This tincture is from the first boil-down iteration. Please note the deep coloration of the

tincture! The hematite ore is opened much better with lemon juice. We see that quite a bit

more tincture is drawn out of the matter when compared with the first boil-down of the

citric acid solution experiment.

the extraction of the sulphur of iron via citrus fruit & citric acid

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