Artificial soil

Abstract

The invention provides a composition comprising a silicate-based compound (e.g. clay and / or basalt) and one or more humates and / or fulvates. The invention also provides an artificial soil comprising said composition, as well as methods of making said composition and said artificial soil.

Description

[0001] ARTIFICIAL SOIL

[0002] This invention relates to a composition, in particular a (stable, chemically bonded) composition of silicate-based (e.g. clay) particles and one or more humate(s) and / or fulvate(s). The invention also relates to an artificial soil comprising the composition, as well as methods of making said composition and said artificial soil.

[0003] Background of the Invention

[0004] In agriculture and other plant growing industries, it is desirable to use fertile, nutrient rich soils. However, often natural soils are barren and nutrient poor. Therefore, one aim of the present invention is to provide a soil which is fertile and nutrient rich and, specifically, to introduce organic matter into barren soil.

[0005] A number of artificial soils and fertilisers are known in the art and some contain humates or fulvates. Known methods of obtaining humates or fulvates typically involved starting with potassium extraction or sodium hydroxide and then using multiple modification steps to achieve the desired humate or fulvate. Potassium extraction is likely a popular method because potassium humate is water soluble. However, these methods are time consuming and involve a number of lengthy modification steps.

[0006] In contrast, the present invention involves a much simpler process. The methods of the present invention may not require modification or conversion of humates or fulvates into other humates or fulvates. Instead, humate I fulvate extraction may be done in a single step and once extracted the humates I fulvates can be dried for later use or bonded with the silicate-based compound (e.g. clay) and larger rock particles straight away. Therefore, the chemical route is much simpler.

[0007] Other known methods for obtaining humates and fulvates use calcium hydroxide. However, again, this cannot be converted to calcium humate I fulvate in a single step. Further, the majority of manufactured and artificial soils are produced by starting from natural soils, e.g. terra preta. Manufactured or artificial soils are typically made by mixing different natural soils (sieved or otherwise) and adding more organic matter and minerals I rocks etc. Conversely, the artificial soil of the present invention is manufactured entirely from scratch, without using natural soils.

[0008] By controlling the chemical composition of the input materials and controlling the particle size distributions based on the desired texture, the methods of the present invention can be used to replicate any soil type and nutrient profile, making them customisable based on the specific plant requirements.

[0009] The compositions and methods of the present invention are therefore useful in many forms of plant growing industries including, but not limited to, horticulture, agriculture, vermiculture, viticulture, gardening, commercial farming, floristry, microbiological and mycological research, soil remediation and terra-forming.

[0010] The Invention

[0011] The invention provides a composition comprising a silicate-based compound (e.g. clay and / or basalt) and one (or more) humate(s) and / or fulvate(s). Compositions of the invention may be referred to as clay humate (or clay humus) or clay fulvate complexes. The definition of the term clay humate I fulvate (complex), as used herein, is intended to extend to (complexes comprising) silicate-based compounds other than clay, e.g. basalt. The compositions or complexes are suitably chemically (e.g. ionically) bonded, for example using (e.g. divalent) metal ions. The compositions are preferably water stable, for example they do not dissolve or disperse (when submerged) in water and / or they are insoluble in water.

[0012] Preferably, the silicate-based compound is a of natural origin I naturally occurring I from a natural source. Suitably, it comprises a clay. The clay may comprise or consist of a mineral or mineral species. For example, the clay may comprise one or more of silicon, aluminium, magnesium, iron, potassium, sodium and / or calcium. Suitably, the clay comprises one or more of silica, aluminia and / or magnesia. Preferably, the clay comprises silicon. In addition to minerals, the clay may also comprise water. Alternatively, the silicate-based compound is a mineral obtained from rock, such as igneous rock, preferably basalt. Optionally, it is a combination of clay and basalt.

[0013] For example, the clay or other silicate-based compound may comprise phyllosilicate and / or aluminosilicate and / or tetrasilicate. Preferably, the clay comprises a phyllosilicate. The phyllosilicate may comprise one or more of bentonites, smectites, kaolinites, micas, vermiculites and / or chlorites, or any other clay form I type naturally found in phyllosilicates (or aluminosilicates, or tetrasilicates). Suitably phyllosilicate clays include, but are not limited to, those (Examples given) in Fig. 5. Examples of suitable structures of phyllosilicate clays of the invention are also shown in Fig. 6(a) and Fig. 6(b). Preferably, the phyllosilicate comprises bentonite. Bentonite containing clay is preferred because the humic substances are able to form chemical (e.g. ionic) bonds with the hydroxyl groups in the bentonite during the process of forming the clay humate I fulvate complex. In addition, other cations and / or water molecules may be incorporated into the inter-layer spaces in the bentonite during complex formation. This provides a stable complex whilst also ensuring increased nutrient and water capacity in the resulting soil. An example of a suitable structure of bentonite clay is shown in Fig. 7.

[0014] Alternatively, other phyllosilicate containing clays or mixtures of different clays may be used. For example, kaolinite clay can be used in addition to, or as an alternative to, bentonite. Kaolinite allows for a higher humic substance: clay ratio as it has far more available hydroxyl groups than bentonite, however the swelling capacity that bentonite can offer is not replicated in kaolinite. A comparison of the structure of kaolinite clay versus the structure of bentonite clay is shown in Fig. 8 (Fig. 8(a) shows a suitable structure of a kaolinite clay and Fig. 8(b) shows a suitable structure of a bentonite clay).

[0015] Mixtures of different types of clay are advantageous as they allow for further control of the end characteristics. The different clays may originate from a range of origins. Below is a table highlighting the theoretical origins of a number of phyllosilicate clays suitable for use in the invention. The theorised mode of action is weathering (physical, chemical and biological).

[0016] Humic substances, also known as humus, are organic matter resulting from the decomposition of plant material and animal residues. Humic acids (HA) and fulvic acids (FA) are compounds found in humic substances or humus. Humin is a separate compound found in humic substances or humus, similar in structure to humic and fulvic acids but insoluble in water. Humic acids and fulvic acids are both organic molecules that play essential roles in improving soil properties, plant growth and agronomic parameters. Humic acids are larger molecules and are insoluble in water at pH lower than 2. Fulvic acids are smaller molecules and are fully soluble in water. Humic and fulvic acids also differ in other ways, including their carbon and oxygen content, acidity, degree of polymerisation, molecular weight and colour. For example, fulvic acid has a higher oxygen content, which is in part the reason for the difference in solubilities. Fig. 9(a) and Fig. 9(b) shown examples of humic and fulvic acids (and humin). Suitable sources of humic and fulvic acids include but are not limited to leonardite, peat, lignite, coal, soil, compost and other organic materials. Humates and fulvates are formed when humic acids and fulvic acids, respectively, bind to minerals.

[0017] The composition comprising clay and one or more humates and / or fulvates (i.e. the clay humate complex, also referred to as the clay humus complex, and / or the clay fulvate complex) refers to aggregate formation of organic fragments (e.g. humic substances such as humic acid and fulvic acid) and inorganic particles (e.g. clay or mineral species). Aggregation may be accomplished either by hydrogen bonding or the incorporation of metallic cations. An example of a suitable structure of a clay humate / clay fulvate complex of the invention is shown in Fig. 10 and a detailed explanation of one way in which the clay humate I clay fulvate complex may be formed is given in Example 23.

[0018] The ratio of clay to humate or fulvate in the composition (i.e. in the clay humate or clay fulvate complex) may be between 0.5:1 and 1 :3, suitably between 1 :1 and 1 :2.5, preferably between 1 :1 and 1 :2. For example, the ratio may be 0.5:1 , or 1 :1 , or 1 :1.5, or 1 :2, or 1 :2.5, or 1 :3. In an example described below, the ratio is 1 :2.5.

[0019] The composition may also comprise one or more alkaline earth metal ions, suitably beryllium, magnesium, calcium, strontium, barium and / or radium. Suitably, the one or more alkaline earth metal ions comprises magnesium, calcium and / or strontium. Preferably, the one or more alkaline earth metal ions are selected from magnesium and calcium. More preferably, the one or more alkaline earth metal ions comprise or consist of calcium ions.

[0020] The one or more alkaline earth metals may be bonded to the one or more humates and / or fulvates, for example the one or more humates and / or fulvates may be present as alkaline earth metal humates and / or fulvates. Suitably, the composition comprises magnesium humate and / or magnesium fulvate. Preferably, the composition comprises calcium humate and / or calcium fulvate. More preferably, the composition comprises calcium humate. Suitably, the composition may comprise a combination of magnesium humate / fulvate and calcium humate / fulvate.

[0021] Alternatively, or in addition to alkaline earth metal ions, the composition may comprise one or more other elements which are able to form cations, preferably 2+ cations or divalent metal ions. The one or more other elements may be selected from scandium, lanthanum, zinc, iron, silicon, aluminium, zirconium, titanium, yttrium, barium, lithium, copper, sodium, potassium and rubidium. Suitably, the one or more other elements are selected from scandium, lanthanum, zinc, silicon, aluminium, zirconium, titanium, yttrium and barium. Preferably, they are selected from scandium, lanthanum, zinc and aluminium, or more preferably scandium, lanthanum and zinc.

[0022] Suitably, the composition also comprises water. Suitably, the water or moisture content can be altered, e.g. by varying the amount of manipulation, to obtain the desired texture. Suitably, the composition also comprises rock. Compositions of the invention comprising rock may be referred to as a soil mineral matrix. The soil mineral matrix is preferable water stable, e.g. it does not disperse in water. The rock may comprise or consist of one or more minerals such as in the form of solids. The rock may comprise any naturally occurring rock (for example igneous, sedimentary and / or sedimentary rock forms). The solid minerals may be in the form of grains or crystals. Suitably, the rock is present in the form of rock particles. The rock particles may be less than 2mm in diameter, or less than 1mm in diameter, or less than 0.5mm in diameter, or less than 0.2mm in diameter, or less than 0.1 mm in diameter. Preferably, the rock particles are less than 0.05mm in diameter, or more preferably less than 0.01 mm in diameter, or even more preferably less than 0.002mm in diameter.

[0023] The size of the rock particles may be varied depending on the desired texture of the composition, or soil mineral matrix, or artificial soil. For example, if the desired texture is coarse, the rock particles may be greater than 0.05mm in diameter. If the desired texture is medium (i.e. somewhere between coarse and fine) the rock particles may be between 0.05mm to 0.002mm in diameter. If the desired texture is fine, the rock particles may be less than 0.002mm in diameter. Finally, if the desired texture is very fine, the rock particles may be less than 0.001mm in diameter, for example less than 0.0005mm in diameter. When the desired texture is fine or very fine, the rock may be present in the form of rock dust or rock powder. Rock dust or rock powder is formed when rock is ground or crushed into fine powder. The composition may comprise a mixture of different rock sizes, for example it may comprise some rock having a diameter of greater than 0.05mm, some having a diameter of between 0.002mm and 0.5mm, and some having a diameter of less than 0.002mm.

[0024] The one or more minerals present in the rock may be referred to as rock forming minerals. These may be selected from feldspar (preferably potassium rich feldspar, such as orthoclase), quartz, amphibole, mica, olivine, garnet, calcite, pyroxene, augite, hornblende, biotite, plagioclase (preferably calcium rich plagioclase, such as anorthite, or sodium-rich plagioclase, such as albite), muscovite and calcium carbonate containing species (such as dolomite, limestone, calcite and sandstone). Suitably, the rock comprises a mixture of minerals, for example a mixture of quartz, feldspar and plagioclase (i.e. granite) or feldspar (e.g. plagioclase feldspar, such as labradorite), pyroxene, olivine, biotite, hornblende and optionally quartz (i.e. basalt, e.g. if not already present as the silicate-based compound). Different mineral or rock species exhibit different micro crystal structures. Below are two examples of chemically equivalent mineral (rock) species which are mainly differentiated through their micro crystal size. This difference in micro crystal size is typically caused by the depth or lack thereof during the solidification stage.

[0025] It is preferred that the types of rock or minerals used in compositions of the invention have phyllosilicates within its structure. As mentioned above, the minerals may originate from igneous, metamorphic or sedimentary rock species. Minerals originating from igneous and metamorphic rock species are preferred, although phyllosilicate containing minerals originating from sedimentary rock species can also be used in the invention.

[0026] Preferably, the rock comprises basalt (e.g. if not already present as the silicate- based compound) and / or granite. For example, the rock may comprise basalt. Alternatively, the rock may comprise granite. Suitably, the rock comprises basalt and granite. This combination is preferred because of the natural abundance and worldwide availability of these common species, making these species a less expensive option. Alternatively, the methods of the invention work successfully any other rock types containing phyllosilicates. Suitably, the rock comprises basalt and granite in a ratio (w / w) from between 0.1 :1 and 1 :0.1. Alternatively, the rock comprises basalt and granite in a ratio (w / w) from between 2:1 and 1 :5, or 1.5:1 and 1 :1.5, or 1.2:1 and 1 :1.2 respectively. For example, the rock may comprise basalt and granite in the ratio 1 :1.

[0027] The ratio of clay to rock or mineral species may be between (w / w) 1 :9 and 9:1 , or between 1 :5 and 5:1 , or between 1 :3 and 3:1. For example it may be 1 :9, or 1 :5, or 1 :3, or 1 : 1 , or 3: 1 , or 5: 1 or 9: 1 . Preferably, the ratio of clay to rock or mineral species is between 1 :9 and 1 :3 for use as soil. For a 1 : 1 clay, the structure consists of 1 silica tetrahedral sheet and 1 alumina octahedral sheet. For a 2:1 clay, the structure consists of 2 silica tetrahedral sheets and 1 alumina octahedral sheet.

[0028] The composition may also comprise one or more of organic matter, fauna (e.g. microfauna) and microorganisms. For example, the composition may comprise organic matter. Alternatively, or additionally, the composition may comprise fauna or microfauna. Alternatively, or additionally, the composition may comprise microorganisms. When the compositions comprise one or more of organic matter, fauna (e.g. microfauna) and microorganisms, they may be referred to as an artificial soil, specifically a stable and / or fertile artificial soil. The artificial soil is preferably bioactive and suitable for plant growth. The organic matter may comprise between 0% and 50%, for example it may be up to 50%, or up to 40%, or up to 30%, or up to 20%, or up to 10%.

[0029] The invention also provides methods of making the compositions, soil mineral matrices and artificial soils described above. The methods of the invention involve extracting one or more humates and / or fulvates from a natural source and combining the one or more humates and / or fulvates with a silicate-based compound (such as clay and / or basalt). Preferably, the combination of the one or more humates and / or fulvates involves chemically (e.g. ionically) bonding these components. For example, using (e.g. divalent) metal ions. For example, to form a stable complex, suitably which is insoluble in water. Ideally, the process of combining of the one or more humates and / or fulvates with the silicate-based compound (e.g. clay I basalt) is a (e.g. single-step) chemical process or reaction.

[0030] Suitably, the one or more humates and / or fulvates are extracted by an exothermic reaction, such as an acid-base reaction. Typically, the extraction is an alkali extraction. The acid-base reaction may take place in the presence of water, for example it may take place in aqueous solution. The acid-base reaction may take place between one or more humic acids and / or fulvic acids present in the natural source and one or more alkaline earth metal compounds and / or divalent metal ions. In other words, the one or more humates and / or fulvates may be extracted from the natural source resulting in the humic and / or fulvic acid bonding to one or more alkaline earth metal compounds and / or divalent metal ions. The divalent metal ions may comprise scandium, lanthanum, zinc, iron, silicon, aluminium, zirconium, titanium, yttrium, barium, lithium, copper, sodium, potassium and / or rubidium The one or more alkaline earth metal compounds may be selected from alkaline earth metal hydroxides, carbonates, oxides, peroxides, silicates and phosphates. Where oxides and / or peroxides are present they may form hydroxides as an intermediate, for example they may react with water to form hydroxides.

[0031] Where silicates are present in alkaline conditions, they may undergo hydrolysis, depolymerisation and / or recondensation to form new silicates and / or carbonates in the presence of cations. Suitably, the one or more alkaline earth metal compounds are selected from hydroxides, carbonates, oxides, peroxides and silicates. Preferably, they are selected from hydroxides and carbonates. Suitably, the one or more alkaline earth metal compounds are or include calcium hydroxide and / or calcium carbonate, or magnesium hydroxide and / or magnesium carbonate, or a combination or magnesium and calcium hydroxides and / or carbonates. Preferably, the one or more alkaline earth metal compounds are or include calcium hydroxide and / or calcium carbonate, more preferably calcium hydroxide.

[0032] The one or more alkaline earth metal compounds suitably have a pH greater than 7. The one or more alkaline earth metal compounds may have a pH less than 12.5, e.g. less than 12 or less than 10. For example, the one or more alkaline earth metal compounds suitably have a pH between 7 and 12.5, e.g. between 7 and 12 or between 7 and 10. Where the alkaline earth metal compound(s) is or comprises calcium hydroxide, the pH is suitably less than 12.5, for example between 7 and 12.5.

[0033] The high pH environment provided by the alkaline earth metal compounds may cause deprotonation of the humic I fulvic acid ligand structure and / or the clay chemical structure, typically at the hydroxyl groups (including but not limited to silanol and aluminol). This may facilitate bonding between the humic I fulvic acid with alkaline earth metal ions (such as Ca2+ ions) in the solution. The bonding to alkaline earth metal ions may promote the combination of the clay and humate I fulvate to form aggregate particles (i.e to form the clay humus complex). These aggregate particles (or clay humus complex) suitably provide the ‘glue’ for the larger mineral particles and the overall soil structure. Group II alkaline earth metals are preferred to ensure there is sufficient charge to bond to both the humic I fulvic acid and the silicate-based compound (e.g. clay and / or basalt). Calcium is particularly preferred because it is commonly available in nature and therefore easy to obtain. Calcium can be obtained, for example, from water with dissolved ions such as a river or earthworms excreting calcium ions during digestion (from the calciferous gland). Earthworms have a calciferous gland that excretes calcium ions into the intestinal tract, typically though calcium carbonate and calcite crystals. Some research suggests that this plays a role in neutralising acidic intake such as humus or it could be a way to reduce the bloods pH by excreting the excess cations. Although the exact reason is still to be determined, this is evidence that there are instances whereby excessive calcium ions, humus and phyllosilicate clays are in the same environment. Magnesium is also a preferred alkaline earth metal.

[0034] The natural source may be, for example, leonardite, peat, lignite, coal, marine algae, rock shales, sapropels, treated sewage, soil, manure, treated sewage or compost. Suitably, the natural source is either leonardite or compost. Preferably, the natural source is leonardite. The leonardite may comprise plant substance, preferably humified plant substance. It may also comprise organic matter and is preferably rich in organic matter. The leonardite is suitably an intermediate between peat and lignite. It may originate from the breakdown of plant materials underground over millions of years and may be found in the upper layers of mines of lignite or coal. Alternatively, the natural source may be compost. The compost may be formed from a mixture of decomposed organic matter, such as plant matter, food waste and manure.

[0035] The methods of the invention may further comprise one or more subsequent steps, including but not limited to, adding rock, reducing the pH, adding organic matter, adding fauna (e.g. microfauna) and adding microorganisms.

[0036] Following reaction of the humic and / or fulvic acid with one or more alkaline earth metals to extract the humates and / or fulvates, the pH of the composition may be high, for example greater than 7. The desired pH of the soil can vary depending on the intended use of the soil. In some cases, is advantageous for soil pH to be around 6 to 8, for example around 6 to 7.5 or 6.5 to 7.5. In other cases, it is preferred that the pH is less than 7, for example from 5 to 7 or 6 to 7. Therefore, following the acidbase reaction, the pH of the composition may need to be reduced. The pH reducing step preferably takes place after the step of combining the one or more humates and / or fulvates with clay. The pH reducing step suitably involves reacting the composition with acid. Suitable acids include but are not limited to phosphoric acid, carbonic acid, acetic acid, citric acid, sulphuric, nitric and formic acid. Preferably, the acid used is phosphoric or sulphuric acid. The pH may be reduced to between 5 and 8. For example, the pH may be reduced to between 6 to 7.5 or 6.5 to 7.5. Preferably, the pH is reduced to less than 7, for example from 5 to 7 or from 6 to 7. In a specific embodiment of the invention, the pH was reduced (from 12.5) to 6.3.

[0037] Unreacted (or free) calcium and / or metal ions may react with the atmosphere. Optionally, by selecting different acids, it may be possible to control the reactions taking place with any excess calcium ions and metal ions. For example, when using phosphoric acid, the excess ions may react with the acid to form apatite. Alternatively, when using sulphuric acid, the excess ions may form gypsum, for example, or when using nitric acid, the excess ions may form nitrides, such as calcium nitride. Where the free ions are able to interact with the atmosphere, they may interact with CO2 (and H2O) to form a metal-carbonate compound.

[0038] Following the step of combining the one or more humates and / or fulvates with the silicate-based compound (e.g. clay and / or basalt), and optionally the step of reducing the pH when present, the method may comprise the addition of rock. The step of adding rock may be carried out before or after the step of reducing the pH (when present). When the clay comprises phyllosilicate, it is preferred that the step of adding rock is carried out before the step of reducing the pH to allow bonding to take place between the composition (i.e. the clay humate and / or clay fulvate complex) and the rock. This bonding occurs when the pH of the composition is kept high because the phyllosilicate comprises hydroxyl functional groups, therefore an acid-base reaction takes place. The free oxygen bonding sites then bond with the cationic metal species. The bonding results in a more stable resulting composition or soil mineral matrix. The amount and particle size of the rock added can be varied depending on the desired texture of the soil.

[0039] As a final step or steps the method may comprise adding organic matter and / or fauna (e.g. microfauna) and / or microorganisms. Preferably, the method involves at least adding organic matter. The organic matter suitably comprises living organisms, the fresh dead residue, well-decomposed (or burned) material or a combination. Suitable components of the organic matter include but are not limited to worm humus, vegetable compost, bovine / horse manure, seaweed, insect frass, Gammarus, treated sewage and bat / seabird guano. Suitably, the method may involve adding organic matter and fauna (e.g. microfauna) and microorganisms. Suitable microorganisms include but are not limited to fungi, springtails, soil mites, nematodes and various types of microbes and mycorrhizae spores (suitably, one or more microbes and mycorrhizae spores, optionally selected from but not limited to the list given in Example 3(a)). The number of microorganisms added can vary depending on the required biomass of the soil. Increasing the number of microorganisms added will increase the biomass of the soil. Allowing the composition to rest after adding the microorganisms will also increase the biomass. Optionally, the addition of a simple sugar and / or complex carbohydrate solution may also boost the microbe I fungi content and, hence, increase the biomass. A suitable example of a sugar solution is unsulphured blackstrap molasses.

[0040] In natural soils nitrogen-fixing bacteria can supply up to 80% of a plant’s nitrogen, although this is more typically within the range of 30-60%. Therefore, there is generally a need for the nitrogen level to be supplemented for optimum growth. In the artificial soils of the present invention, the rest of the required nitrogen may be supplied by the organic matter and / or microorganisms, such as symbiotic mycorrhizal fungi. Other types of microorganism which may optionally be present in the soils of the invention include but are not limited to phosphate solubilizing bacteria and / or potassium solubilizing bacteria. The combination of symbiotic mycorrhizal fungi and solubilizing bacteria is preferable to ensure the plants are provided with all their required nutrients.

[0041] The amount of organic matter (and optionally fauna and / or microorganisms) added can be varied according to the desired nutrient profile of the soil. It will be appreciated that the desired nutrient profile of the soil changes depending on the intended use of the soil, for example which plants are intended to be grown in the soil and how many nutrients they require for optimal growth.

[0042] During the step of adding the organic matter (and optionally fauna and / or microorganisms), volcanic rock or stone may also be added to improve aeration. The volcanic rock or stone is suitably added after the organic matter (and optionally fauna and / or microorganisms) and before mixing. The volcanic rock or stone may be added and then the mixture may be mixed thoroughly to promote the intake of air whilst mixing the organic matter (and optionally fauna and / or microorganisms) into the composition. Preferably, the volcanic rock or stone is porous and may have a sponge-like structure. The volcanic rock or stone suitably comprises lapilli and / or pumice, preferably a mixture of both lapilli and pumice.

[0043] The invention also provides calcium humate and / or calcium fulvate and / or (humate I fulvate) salt forms of other metal ions, such as zinc, zirconium, iron, scandium, yttrium and lanthanum. Suitably, the invention provides calcium humate. Suitably, the invention provides calcium fulvate.

[0044] Advantages and Uses of the Invention

[0045] The methods of the invention allow the chemical composition of the input materials and the particle size distributions of the resultant artificial soil to be carefully controlled. This means that it is possible to accurately obtain the desired texture and nutrient profile and, hence, the methods can be used to replicate any soil type, making the resultant artificial soils customisable based on the specific intended use and plant requirements.

[0046] One aim of the present invention is to introduce organic matter into barren soil. This is facilitated by the chemically (specifically, ionically) bonded clay humate complex which allows organic matter to instantly bind to barren soil, reducing the recovery time of the soil. This technology could also be used to turn another planet’s surrounding rock into a fertile soil with the just one component from earth, the one component being a source of humate. For example, the present invention may make it possible to produce large quantities of fertile soil on planets such as Mars, where there is naturally occurring calcium carbonate which can be heated to form calcium hydroxide, with only leonardite and, preferably, also some organic matter.

[0047] Another aim of the present invention is to retain as many minerals and microbes in the soil as possible. The clay humate and clay fulvate complexes of the present invention can therefore be used to form fertile soil from nutrient poor soils, such as desert or sandy soils. The clay humate and clay fulvate complexes of the present invention are also useful for land reclamation and / or rejuvenation. The clay humate and clay fulvate complexes are not only able to instantly re-fertilise barren sandy soil, but they also do not disperse when submerged in water and therefore they are able to resist being washed away. Hence, the stable complexes can also be used for desert reclamation or as microbial I fungal carrier to further speed up recovery as well as mineralising compost / old substrate. When mixed with minerals (to form a clay mineral matrix) the stable, chemically bonded complexes can be used as a highly nutrient rich, long-lasting, instant fertilisers for sandy, silt-based soil. For example, the clay mineral matrix or complex of the invention can be used to form fertile soils from clay or silt-heavy land. This can also be used as an additive for compost I substrate.

[0048] The artificial soil of the invention can be used as a replacement for other classical substrates, as an additive fertiliser and for rebalancing clay soils. Due to the ability to control the exact composition, particularly sensitive plants or one’s requiring exact parameters can also be accommodated by the compositions of the invention.

[0049] As per Ell and other world body reports there is increasing risk of land degradation, nutrient run-off caused by industrial practices and soil loss which could all be addressed using the artificial soil of the present invention. As clay is naturally retentive of nutrient ions and remains in place unless under pressure or overwatered (as natural soil would), the clay complex is particularly advantageous for addressing nutrient run-off. The artificial soil of the present invention can also be used as a top layer to help prevent erosion.

[0050] Known artificial soils are effectively just modified soil blends or water-soluble fertilisers. For example, known methods start with natural soils and make minor modifications to them, e.g. by adding calcium oxide for pH adjustment. In known methods, the calcium (or other metal ion) is not used to chemically or ionically bond humates or fulvates to the clay or phyllosilicates, as it is in the methods of the present invention. In known methods, clay (e.g. bentonite) is used merely as a carrier and, in use, the product (e.g. leonardite) is quickly released from said carrier. Hence, known artificial soils are not chemically or ionically bonded and, thus, they are unstable (since no stable complex is formed). Conversely, the stable complexes of the present invention are chemically (specifically, ionically) bonded using divalent metal ions and, thus, the clay is present as a reactant, which forms part of the final product and not just a carrier which is quickly released.

[0051] Specifically, methods of calcium humate production are known. However, known methods include multiple steps and use far lower concentrations, limited by solubility in water. Methods of using calcium hydroxide are known. However, these methods start with humic acid (e.g. potassium / sodium humate) and, thus, require substitution of potassium with calcium. In contrast, the methods of the present invention achieve extraction and product formation in a single step, using reactants above their solubility limit, with water functioning more as a catalyst. Moreover, the application of the methods disclosed herein is for asphalt additives, not soil fertility.

[0052] Older methods (e.g. dating back to the 1950s) describe ‘lime-clay humus complexes, but these involve embedding extracted humate salts in excess calcium oxide dried to resemble clay. They all use multiple steps (bubbling, heating, separate extraction and product formation) and, although some methods mention that clay or similar additives can be added to achieve desired chemical profile, this is in the context of a mechanical blend, not a chemically bonded product.

[0053] In summary, all known methods rely on clay as a binder or carrier rather than achieving true chemical bonding. The direct bonding of humates with rock aggregate or the formation of stable clay-humus complexes is not known. The methods disclosed herein involve the creation of new reactive sites though chemical reaction and are not limited, e.g. to bentonite, but apply to other silicates.

[0054] Preferred features and / or characteristics of one aspect of the invention are applicable to another mutatis mutandis. The invention is now described by way of example with reference to the drawings which are not to be construed as limiting.

[0055] Brief Description of the Drawings

[0056] Fig. 1 (a) and 1(b) show a flow chart outlining an example of a full method of making an artificial soil of the invention starting from the raw materials (i.e. clay and humate and / or fulvate).

[0057] Fig. 2 shows a flow chart outlining a method of making a first composition (i.e. a clay humate / fulvate complex) of the invention starting from raw materials.

[0058] Fig. 3 shows a flow chart outlining an example of a method of making a second composition (i.e. a soil mineral matrix) of the invention starting from the first composition made by the method outlined in Fig. 2.

[0059] Fig. 4 shows a flow chart outlining an example of a method of making a third composition (i.e. an artificial soil) of the invention starting from the second composition made by the method outlined in Fig. 3. Fig. 5 shows a number of non-limiting examples of phyllosilicate clays suitable for use according to the invention.

[0060] Fig. 6(a) and Fig. 6(b) show two examples of suitable structures of phyllosilicate clays suitable for use according to the invention.

[0061] Fig. 7(a) shows an example of the structure of a bentonite clay suitable for use according to the invention (with a 2:1 swelling ratio) and Fig. 7(b) shows the molecular structure of bentonite.

[0062] Fig. 8 shows a comparison between the structures of kaolinite and bentonite clays. Fig. 8(a) shows an example of kaolinite clay, having many hydroxyl groups on the octahedral layer, and Fig. 8(b) shows an example of bentonite clay, still featuring hydroxyl groups on the octahedral layer but showing that the hydroxyl groups are less available due to bonding with the additional tetrahedral layer.

[0063] Fig. 9(a) shows a comparison between fulvic acid, humic acid and humin and Fig. 9(b) shows an example of a humic acid molecule versus a fulvic acid molecule.

[0064] Fig. 10 shows an example of a structure of a clay humate I clay fulvate complex.

[0065] Fig. 11 (a) shows a hypothetical molecular structure of a leonardite humic acid and Fig. 11 (b) also shows a hypothetical molecular structure of humic acid with important functional groups labelled.

[0066] Fig. 12(a) shows examples of the structures of two 2:1 sheet silicate clays, illite and montmorillonite, showing strong chemical bonds form the alumina octahedral and silica tetrahedral sheets and cations held between the sheets by relatively weak electrostatic attraction. Fig. 12(b) shows an example of the structure of a kaolinite clay Layer, showing strong chemical bonds making the kaolinite clay chemically stable. The strong chemical bonds also produce highly refractory clay crystals with consistent physical properties. Fig. 12(c) shows a table detailing the properties of four key types of silicate clay. Kaolinite and halloysite are simple and have the same chemical composition, but different crystal structure (plate versus tube). The illite and montmorillonite formulae shown in the table are the scientifically agreed upon theoretical formulae, but much variability exists in nature in the percentage of alkali and alkaline earth elements found in a given deposit and even within a deposit. It is well understood that for a given weight of illite and montmorillonite there is much less alumina than in kaolinite and halloysite. The amount of water in montmorillonite is not fixed. Given time it absorbs as much water as is available to it.

[0067] Fig. 13(a) shows a schematic structure of a 1 :1 phyllosilicate layer and Fig. 13(b) shows a schematic structure of a phyllosilicate clay mineral with stabilised ion / water clathrates. The left-hand side of Fig. 13(b) shows that the metal ion-doped silicate structure exhibits platonic geometry and the right-hand side of Fig. 13(b) shows that the surface structure of the clay mineral offers binding sites.

[0068] EXAMPLES

[0069] Example 1 - Production of a Composition Comprising Humate and Clay (i.e. Production of a Stable Clay Humus Complex)

[0070] Leonardite was added to water and blended to form an aqueous solution. A basic compound, containing alkaline earth metals in its structure, of pH greater than or equal to 8, was added to the aqueous solution. In this example calcium hydroxide was used, however other suitable compounds include but are not limited to calcium carbonate and other hydroxides I carbonates. The quantity of alkaline earth metal compound added can be varied and is determined by the intended organic matter content. The ratio used in this example was 1.2:1 (calcium hydroxide to leonardite %w / w), however other suitably ratios include but are not limited to 1 :1 , 1.1 :1 , 1.3:1 and 1.4:1. 1.2:1 is the optimum ratio for the leonardite source used in this example. These ratios are based on experimentation and given as a guide and the actual ratios used in the invention may vary depending on the leonardite source. This is because leonardite from different sources may comprise or contain different types or quantities of functional groups. In practice, the ratio of calcium hydroxide to leonardite may be between 0.5:1 and 1 :2, for example between 1 :1 and 1 :1.5.

[0071] The solution was then mixed, using agitation or sonication, until the liquid became a uniform mixture. This step is an exothermic reaction, so considerable heat was produced. The mixing was continued until no further heat was produced.

[0072] A raw phyllosilicate clay was then added to the aqueous solution and mixed thoroughly until combined. In this example bentonite was used, however other suitably examples include but are not limited to smectites, kaolinites, micas, chlorites. In this example, a ratio of 1 :2.5 (bentonite to calcium humate %w / v) was used. Other suitable ratios for bentonite to calcium humate (%w / v) include 0.5:1 , 1 :1 , 1 :1.5 and 1 :2. Results show an increasing amount of unbounded calcium humate when using a ratio above 1 :2.5, therefore a ratio of 1 :2.5 or lower is preferred. A ratio of between 0.5:1 and 1 :2.5 is particularly preferred.

[0073] The pH of the mixture was then reduced to between 6 and 7 using an acid. The acid used in this example was phosphoric acid, however other suitable acids include but are not limited to acetic acid, carbonic acid, citric acid, nitric, sulphuric and formic acid. This step involved an acid-base reaction. A considerable amount of heat was produced during the acid-base reaction and additional water was needed to ensure consistent combination. The resultant mix formed silt sized aggregates. The water content was then reduced to the desired level. The desired water content may vary depending on the intended use and properties of the soil.

[0074] Example 1 (a) - Production of a Composition Comprising Humate and Clay (i.e. Production of a Stable Clay Humus Complex) in More Detail

[0075] 1000mL of reverse osmosis (RO) water was placed in a 1.5L blender and 300g of leonardite was added. The leonardite was then blended to reduce the particle size (this step may not be required if the leonardite particles are small). 231g of calcium hydroxide was then added to the blender and mixed at high speed for 5 minutes. The mixture was allowed to rest for 5 minutes before blending again. This exothermic process was repeated 3 times to maximise extraction.

[0076] 4000g of calcium bentonite clay was then placed in a bucket and the calcium leonardite mixture was added to the bentonite clay. The resulting mixture was mixed with a paddle mixer. This process was also exothermic and additional water was required to ensure smooth mixing (approximately 0.5-1 L of water was added).

[0077] The pH was then reduced to between 6 and 7 using phosphoric acid. Approximately 300-600mL of phosphoric acid was used. This reaction was also exothermic. Finally, the water content was reduced to the desired level.

[0078] Example 2 - Production of a Composition Comprising Rock (i.e. Production of a Soil Mineral Matrix)

[0079] The steps detailed in Example 1 were performed but the pH was not reduced. Instead, the pH reduction step was carried out after combining with crushed primary rock containing phyllosilicate minerals. Suitably primary rock species include any naturally occurring rock crushed to the correct particle size (for example igneous, sedimentary & metamorphic rock forms are all suitable).

[0080] Various primary crushed rock forms were mixed until evenly dispersed. The particle size and type of rock used can be varied based on nutrient requirements and of the desired particle size distribution of the soil. In this example, a mixture of basalt and granite was used. The particle size of the crush rock was less than 2mm in diameter. The crushed rock included a mixture of particles of different diameters in the following ratios: 25%-55% of particle size greater than 0.05mm, 25-80% of particle size between 0.002mm and 0.05mm, and 5-40% of particle size less than 0.002mm.

[0081] The primary rock mix was then combined with the high pH clay humus complex of Example 1 using physical mixing methods until evenly combined. In this example, the primary rock species used contained phyllosilicate minerals (although this is not essential) which meant that bonding between the primary rock species and the clay humus complex could occur, thereby improving the soil structure. The optimal ratio, and the ratio used in this example, was 40% w / w clay humus complex to crushed primary rock species.

[0082] Following combination of the clay humus complex with the primary rock species, the pH of the mixture was reduced to between 6 and 7 using an acid, whilst continuing to agitate / mix the mixture. The pH reducing step was carried out after combining the clay humus complex with the rock because the primary rock species contained phyllosilicate minerals, therefore maintaining the clay humus complex at high pH during combination with the crushed primary rock species allowed for further alkaline metal bonding with the clay humus complex (i.e. the alkaline metals present in the primary rock species were able to bond with the clay humus complex, further increasing the stability of the composition). The step of reducing the pH was carried out primarily to ensure optimum conditions for plant growth, but it also induced weathering I breakdown of the primary rock species producing further clay particles and thereby promoting better adhesion of the rock species to the clay humus complex.

[0083] Example 2(a) - Production of a Composition Comprising Rock (i.e. Production of a Soil Mineral Matrix) in More Detail

[0084] The steps outlined in Example 1(a) were performed, with the exception of the pH reduction step. 20kg of granite (of particle size less than 2mm), 10kg of basalt (of particle size less than 5mm), 2.5kg of gypsum, 500g of dolomite, 500g of vermiculite and 370g of rock phosphate were added to a cement mixer. Any rock which was not already of the desired particle size was crushed (for example using a hammer, ball, or vertical or planetary mills) prior to mixing.

[0085] The various rock types were then mixed until evenly distributed, for approximately 5-10 minutes. The rock mixture was then combined with the high pH composition produced in Example 1(a) (i.e. the clay humus complex) and the mixture was mixed thoroughly until evenly distributed.

[0086] The pH of the resulting mixture was then reduced to between 6 and 7 using phosphoric Acid (59%). Approximately 800-1 OOOmL of acid was added whilst continuing to agitate / mix the mixture. Finally, the water content was reduced through the process of evaporation.

[0087] Example 3 - Production of a Composition Comprising Organic Matter (i.e. Production of an Artificial Soil)

[0088] Organic matter, in the desired guantity, was added to the composition produced in Example 2 (i.e. the soil mineral matrix) and mixed thoroughly. In this example, the organic matter used was compost comprising dead leaves, plant matter, dead insect matter and manure. The addition of organic matter can be varied depending on the desired nutrient profile of the soil, however the typical range is between 1 and 40%w / w. The amount of organic matter can be increased to obtain a more nutrient rich soil or decreased to obtain a less nutrient rich soil.

[0089] In this example pumice and lapilli were added before mixing thoroughly for improved aeration, although this step is optional. After mixing, the pH was altered to obtain the desired pH range using a pH buffer. Depending on the type and amount of organic matter added, this step may involve increasing or decreasing the pH, typically using an appropriate pH buffer.

[0090] Further microorganisms, including fungi and nematodes, and other desired fauna were then introduced until the reguired biomass ratios were reached. In this example, the addition of a simple sugar and complex carbohydrate solution was also implemented to help boost the microbe I fungi content and increase the biomass of the soil. The water content was adjusted to the desired level. Depending on the required properties and intended use of the soil, this step may involve adding or reducing the water content. The product was further manipulated by a physical mixing method and careful control of the moisture level. Finally, macrofauna, including springtails and isopods, were introduced to promote better nutrient cycling.

[0091] The resultant mixture was a stable and bio-active artificial soil with non-dispersive properties when submerged in water. The soil mix was seen to improve over time as plant roots and soil fauna further modified and improved the structure.

[0092] Example 3(a) - Production of a Composition Comprising Organic Matter (i.e. Production of an Artificial Soil) in More Detail

[0093] 5L of reverse osmosis (RO) water was added to a bucket, followed by 500mL of unsulphured blackstrap molasses mixing thoroughly. Bubbles were injected into the mixture for 30 minutes using an air pump with a suitable air filter to reduce contamination. 1 kg of biochar was added to the resultant mixture, as well as key microbes and mycorrhizae spores including:

[0094] Arthrobacter globiformis Azobacter chroococcum Azospirilum Lipoferum Azotobacter Vinelandii B. Circulans B. Subtilis

[0095] Bacillus amyloliquefaciens Bacillus azotoformans

[0096] Bacillus coagulans Bacillus licheniformis Bacillus megaterium Bacillus mucilaginous Bacillus pumilis Bacillus subtilis

[0097] Gigaspora margarita Glomus aggregatrum Glomus clarum Glomus deserticola

[0098] Glomus etunicatum Glomus intraradices Glomus monosporum Glomus mosseae Micrococus Roseurs Paenibacillus durum Paenibacillus polymyxa Paraglomus brasilianum Pisolithus tinctorius Pseudamonas Putida Pseudomonas aureofaciens Pseudomonas chlororaphis Pseudomonas fluorescens Pseudomonas Fluorescens Rhizopagan amylopogon Rhizopagan fulvigleba Rhizopagan luteolus Rhizopagan villosullus Saccharomyces cerevisiae Scleroderma cepa

[0099] Scleroderma citrinum Trichoderma harzianum

[0100] Trichoderma harzianum Trichoderma koningii

[0101] Trichoderma viride.

[0102] The mixture was agitated and injected with bubbles for 12-24 hours. To a bucket was added a mixture of organic matter including 2kg of worm humus, 1.5kg of vegetable compost, 500g of bovine / horse manure, 500g of seaweed, 325g of insect frass, 100g of gammarus and 150g of bat / seabird guano. The contents of the buckets were combined.

[0103] The biochar was removed from the unsulphured blackstrap molasses mixture and added to the organic matter bucket. The contents of the bucket were combined thoroughly and then left to mature to increase biomass prior to adding to the composition produced in Example 2(a) (i.e. the soil mineral matrix).

[0104] Once matured, the organic matter was added to the soil mineral matrix of Example 2(a) and the resulting mixture was combined thoroughly. 2.5kg of pumice and 2.5kg of lapilli were added and the mixture was combined thoroughly again.

[0105] The pH was then adjusted to the desired range (this step can involve reducing or increasing the pH depending on the desired properties and intended use of the soil) using an appropriate pH buffer.

[0106] The water content was also adjusted to the desired level (again, this step can involve increased or decreasing the water content depending on the desired properties and intended use of the soil). The final product was then further manipulated by a physical mixing method and careful control of the moisture level.

[0107] Example 4 - Breakdown of Ingredients Used to Replicate a Natural Soil

[0108] Example 5 - Breakdown of Ingredients Used to Produce a High Nutrient Soil Suitable for Use as a Soil Booster

[0109] Example 6 - Breakdown of Ingredients Used to Produce a Simple Soil Mix

[0110] Example 7 - Determination of the optimum ratio of Clay to Humate / Fulvate in the Clay Humate / Fulvate Complex

[0111] An experiment was carried out to determine the optimum ratio of clay to calcium humate when forming the clay humate complex and to determine the amount of energy released when combining calcium humate with clay.

[0112] Ingredients I Equipment: Ro water, Calcium hydroxide, Leonardite, Calcium bentonite (2:1 Calcium : sodium), pH Meter- Milwaukee, Glass thermometer, 7.5mL measuring spoon, Measuring cylinder, Pipette, Calcium test - Seifert. Method:1000mL of RO water was added to a blender. 250g of leonardite was added to water and blended for 30 seconds. 250g of calcium hydroxide was added and blended for 3 x 2 minutes. 50g of calcium bentonite was weighed out into a cup. A specified volume of calcium humate mixture was added to a measuring cylinder (T1). A specified volume of calcium humate mixture was added to the clay and combined thoroughly (T2). 7.5mL of clay mixture was taken and added to 50mL of RO water, allowed to settle and the supernatant was taken for a calcium test (CA1). The pH was reduced to below pH7, the mixture was agitated thoroughly and allowed to settle before the supernatant was taken again and retested for calcium (CA2). Results:

[0113] Discussion: The calcium hydroxide only sample was found to have a calcium concentration of 910ppm. The calcium humate sample was found to have calcium concentration 1375ppm. Clay humate samples were found to have calcium concentrations between 680 -900ppm.

[0114] This suggests that combining the leonardite with the calcium hydroxide allows for more of the calcium hydroxide to dissociate than without its presence. The calcium ions are then consumed again when the phyllosilicate clay is introduced to the calcium-humate mixture. This suggests that the calcium ions are heavily involved with the formation of the clay-humus complex.

[0115] Suggested range of ratios for the clay-humus complex: 1 :1 - 1 :2.5 (%w / v) clay : calcium humate (1 :1 w / w calcium hydroxide : leonardite solution at approx. 36% concentration). Suggested range of ratios for calcium humate: 1 :0.8 - 1 :4 calcium hydroxide : leonardite.

[0116] Example 8 - Determination of the Role of pH in the Formation of the Clay Humate / Fulvate Complex

[0117] An experiment was carried out, using the clay humate complex samples prepared in Example 7, to identify the role of pH in the formation of the clay humate complex. The samples were analysed using light microscopy.

[0118] Method: Sample Prep 1 (wash samples) - Approximately 7.5mL of sample was added to approximately 50mL of water and mixed. The pH was reduced to below pH7. A sample of the top layer of clay (approx. 2mL) was taken. The 2mL sample was dropped into a 50m L measuring cylinder re-filled with RO water. The unreacted leonardite was allowed to fall and then a sample of the suspended clay particles was taken. This sample was used for the analysis. Sample Prep 2 (no pH change) - An approximately 7.5mL sample was added to approximately 50mL of RO water and mixed thoroughly. The sample was allowed to settle, and the uppermost layer was taken using a pipette. This layer was used for the analysis. Sample Prep 3 (post pH change) - A sample of the suspended clay particles was taken from Sample Prep 1 and this was used for the analysis.

[0119] Results: between 1 :1 and 1 :2 (Clay : Calcium humate). pH is not the determining factor regarding clay humus complex formation and may even reduce successful bonding or have little effect. The effect noticed by the change in pH may be due to the phosphoric acid interactions with the calcium ions thereby changing the available cations or, alternatively, it may be electrostatic forces that are changed by the presence of the phosphoric acid side reactions.

[0120] It was also noticed that, when phosphoric acid was added drop-wise during sample prep 1 , a white substance formed and floated above the layer of clay. The reaction was considerably stronger in sample 8 vs sample 1 suggesting that the available calcium ions affect this reaction.

[0121] The primary factor affecting successful complex formation appears to be the ratio between clay : calcium ions : humates rather than the pH.

[0122] Example 9 - Determination of the Role of Temperature and the Concentration of Calcium Ions in the Formation of Calcium Humate and the Clay Humate / Clay Fulvate Complex

[0123] The process of creating the clay-humus complex and soil mineral matrix was performed with a higher concentration of calcium hydroxide to see if this would improve the extraction of humic acid from the leonardite and increase the quantity of calcium-humate obtained. Temperature in degrees Celsius and calcium ions (Ca2+) in ppm were analysed after each step to monitor chemical interactions and energy release. Individual particles were extracted and analysed.

[0124] Equipment and ingredients: Leonardite - 250g, Calcium hydroxide - 300g, Calcium bentonite - 100g, Phosphoric acid 81 %, RO Water, Basalt (3mm>), Dolomite (5mm>), Granite (3mm>), Limestone (Powder), Measuring Cylinder, Blender - 1.5L, Weighing scales - 0.01g readability, Thermometer- Liquid, Vacuum distillation apparatus, Suction bulb, Transfer pipettes, Microscope, Seifert calcium test.

[0125] Method: 1000mL of RO water was added to the blender. The starting temperature was measured and the result recorded. Next 300g of calcium hydroxide was added and the mixture was blended for 5 minutes. The temperature was measured and the result was recorded again. The calcium hydroxide was allowed to settle, and a 2 mL aliquot of the supernatant was taken to perform the calcium test. The PPM was recorded (the test was repeated a further three times to ensure an accurate reading). Water was placed to ensure the volume was maintained at lOOOmL. Next 250g of leonardite was added to the mixture. This was blended for 5 minutes and then the temperature was recorded. The solution was allowed to cool. A 2mL aliquot was taken from the supernatant and the calcium test was performed. The temperature was measured and the result was recorded. The mixture was blended for a further 5 minutes, the temperature was measured again and the result was recorded. This was repeated until no further heat was generated.

[0126] Once the reaction was complete, a sample of the resultant product was taken and wash steps were performed to isolate individual particles. This was done by dropping approximately 1mL of sample into a large glass of RO water (approx. 500mL) and mixing. The mixture was left to settle, the majority of the water was removed until less than 10mL remained. The vacuum distillation apparatus was set up with a paper filter. The 10mL of water was added and created the vacuum until all water was removed. The particles remaining on the filter were analysed both wet and dried using light microscopy (Top-lit).

[0127] Next 100g of calcium bentonite was weighed out and 100mL of the calcium-humate was also measured out. The temperature of both ingredients was measured and recorded. The ingredients were then combined until evenly dispersed and the resultant temperature was recorded. The wash step and vacuum distillation were performed to isolate particles on a paper filter. The particles were analysed wet and dried using light microscopy (Top-lit)

[0128] Due to the dryness of the sample, for the analysis of calcium ions, approx. 10mL of compressed clay-humus complex was taken and thoroughly mixed into 20mL of RO water. Vacuum distillation was then performed and the extracted liquid was taken for analysis using Seifert calcium test.

[0129] A sub-sample of the clay-humus complex was taken and the pH was neutralised using phosphoric acid. The particle isolation and microscopy steps were repeated.

[0130] 25mL basalt, 25mL Granite, 10mL dolomite, 10mL Limestone were combined together until evenly mixed. Approximately 14mL of high pH Clay-humus complex was added and mixed thoroughly. The pH was reduced using phosphoric acid and the analysis was carried out.

[0131] A large stone was isolated from the resultant mineral matrix and washed under running water whilst rubbing with fingers to try and remove any loose debris. Results:

[0132] Discussion: The calcium content of the calcium hydroxide water was the same as previous tests using lower quantities of calcium hydroxide, suggesting maximum dissolution of calcium hydroxide has been achieved, and no further reaction will take place without a change in conditions. The water increased by +1°C. When the leonardite was added to the mixture, significant heat was produced. The maximum temperature reading on the liquid thermometer (+50°C) was reached. It should be noted that although the mixture isn’t viscous per say, it is thick enough to suspend the solids quite effectively. The reaction seems to stop immediately once movement stops. As the temperature doesn’t appear to have hotspots and the top of the solution rises as quickly as the bottom, this suggests that the reaction is due to collision theory with minimum energy requirements and not just caused by the blades of the blender. Through this investigation, it has become evident that temperature change should be used as an indication of end point.

[0133] It is interesting to note that the calcium content significantly increased with the initial addition of leonardite (1405ppm vs 912.5ppm). This suggests that hydroxide ions are being neutralised by the deprotonation of the humates and allowing further calcium hydroxide to dissolve. The last calcium test performed on the calcium humate mixture after approximately 35 minutes of blending time showed a significant decrease in calcium ions (1405ppm vs 675ppm). This suggests that the calcium ions are indeed bonding with the humates from the leonardite. Water vapor and a gas that is unreactive to a flame was being released whenever mixing was occurring. This is likely CO2 due to the carbon from the leonardite.

[0134] When the calcium humate was combined with bentonite clay (100mL:100g), a temperature increase of +2.5°C was measured and a small reduction in calcium ions detected (675ppm vs 642.5ppm). The large release of energy in comparison to a relatively small reduction in calcium ions suggests the calcium humate is precharged with the necessary calcium ions to bond with the bentonite clay.

[0135] Based on particle isolation and microscopy analysis, post-reaction pH reduction does not seem to affect the ability of the clay humus complex to form particles but it does reduce the availability of the calcium ions.

[0136] Combining the clay-humus complex with the primary rock species mix at pH 12 and reducing the pH resulted in a much finer product and an even distribution of the clayhumus complex amongst the mineral complex. Washing a large particle under running water and rubbing with fingers was unable to remove clay-humus complex from the large particle. This suggests that clay-humus complex is able to bond with the phyllosilicate minerals within the overall rock mineral structure and cannot be washed off with water alone.

[0137] Example 10 - Determination of the Key Chemical Pathways

[0138] Calcium Hydroxide is an ionic salt comprising a single Ca2+cation and 2 OH' (hydroxide) anion that partially ionises in water due to water being highly polar. Primary action is ionisation, acid-base reactions, nucleophilic substitution and salt formation. 1 Mole Ca(OH)2 dissociates into 1 mole of Ca2+and 2 moles of OH'. Calcium Carbonate is an ionic salt comprising of a single Ca2+cation and a single CO32' (carbonate) anion. Due to both ions being of equal opposite charge, the salt is nearly insoluble in water but does slightly ionise. Primary action is acid-base reaction and salt formation reactions. Hydrolysis can also result in some nucleophilic substitution. 1 mole of CaCo3 dissociates into 1 mole of Ca2+and 1 mole of CO32'. Water easily ionises into a H+(proton) cation and a OH' anion. Primary action is acidbase reactions and nucleophilic attack.

[0139] Leonardite comprises of humic acid, fulvic acid and other humates as well as mixed organic compounds. The organic compound fraction comprises of cellulose, lignin, tannin, cutin, carbohydrates, proteins and lipids. All of these structures contain similar functional groups with the primary ones including hydroxyl, carboxyl, phenol, alcohol and thiol. Secondary functional groups include ester, aldehyde, ketone, carbonyl and peptide. Primary action is deprotonation, acid-base reactions, salt formation and saponification. As mentioned above, the ratios of leonardite (e.g. the ratio of calcium hydroxide to leonardite) disclosed herein are given as a guide and the actual ratios used in the invention may vary depending on the leonardite source. This is because leonardite from different sources may comprise or contain different types or quantities of functional groups. Phyllosilicate minerals comprise of silicon tetrahedral and aluminium octahedral sheets with the main functional groups comprising of hydroxyl groups.

[0140] Carboxyl, acid, alcohol and thiol functional groups readily ionise in polar solvents, e.g. water due to strong hydrogen bonding, thus reducing the energy requirements to break the covalent bonds. The released hydrogen ions can then neutralise the hydroxide anions or carbonate anion. The calcium cation is then free to bond with the negative oxygen species through ionic bonding, a much stronger bond than the original O-H bond. If carbonate is used, CO2 will also be a by-product.

[0141] Esters undergo nucleophilic substitution by hydroxide ions, leading to carboxylate salts and alcohol which is ionised into a salt. This requires long reaction times or heat (saponification). Aldehyde, ketone and carbonyl also undergo nucleophilic substitution resulting in a carboxylate salt but due to unfavored resonance, moves back to respective functional group without heat or long reaction times.

[0142] Peptide in high concentration of hydroxide anions leads to peptide hydrolysis consisting of nucleophilic substitution resulting in two carboxylate salt chains. This requires heat and time. Quinone and amine groups are unaffected by alkaline conditions and therefore do not need to be considered. Aldol reactions could also occur if mixture is heated. By controlling the reaction time and temperature, you can control the amount of chemical breakdown and recombination. There may be some chelation occurring with the Ca2+cation as well as dipole interactions. The addition of acid can stop the reaction or reverse the reactions, if in high enough concentration and with the input of heat. The bonding of the humic compounds to phyllosilicate minerals is ionic in nature and as per the below:

[0143] [R-O-][Ca2+][-Q-R] [R-O-][Mg2+][-O-R]

[0144] Due to leonardite being of natural origin with varied purity and quality, the exact quantity of functional groups is unknown without testing. 1 - 14 moles of carboxylic and phenolic hydroxyl functional groups per kg of leonardite. Additional functional groups increase this number, giving a theoretical number exceeding 14 moles.

[0145] Example 11 - Determination of the Preferred Elements for Ionic Bonding with the Humic Substances and Clay Minerals

[0146] Primary cation candidate elements (suitable charge, creates stable ions and nontoxic to plants): Magnesium, Calcium, Strontium, Zinc, Scandium, Lanthanum.

[0147] Secondary cation candidate elements (Toxic at elevated levels or more likely to form covalent bonds): Barium, Aluminium, Silicon, Titanium, Yttrium, Zirconium.

[0148] Beryllium and Boron do not readily form cationic species due to the close proximity of the 2S orbital to the nucleus. Radium is radioactive and therefore not a preferred choice of element. Group 1 elements do not generally have sufficient effective charge with the exception of Sodium (Octahedral) in combination with Aluminium (Tetrahedral) tessellation. As Potassium is larger and forms cubic crystals, it cannot typically tessellate with Aluminium to form strong bonds. Aluminium is suitable but can be plant toxic in elevated levels and should therefore be limited or used with caution. Copper is potentially suitable in combination with Aluminium but can be plant toxic in elevated levels and is also able to form an alloy or ligand complex. Copper should therefore be limited. Zinc, Scandium and Lanthanum are suitable. Titanium and Zirconium are suitable but can be plant toxic in elevated levels and should therefore be limited. They are also more likely to form covalent bonds which would weaken the bond between the phyllosilicate mineral and humic substance. Yttrium is suitable but can be plant toxic in elevated levels and should therefore be limited.

[0149] Less suitable elements: Period 1 elements, Transition, Lanthanides, Actinides, Posttransition, Metalloids and non-reactive metalloids.

[0150] Coulombs law: F = K (q1q2 / R2)

[0151] F = electric force, K = 8.99* 109N- m 2 / C 2, q1 , q2 = charges, R = distance of separation.

[0152] Water has a molecular size of 2.75*10'1°m and a permanent dipole moment of 6.1x1 O'30Coulombs.

[0153] When elements are bonded with oxygen, they form bonds of various lengths and differing strength. Sodium produces an average bond length of 2.44*10'1°m with an effective charge of -3.87x1 O'28Coulombs (Factor vs Dipole = 63). Potassium produces an average bond length of 2.92*10'1°m with an effective charge of - 2.6987x1 O'28Coulombs (Factor vs Dipole = 44). Magnesium produces an average bond length of 2.09*10'1°m with an effective charge of -1.71*10-27Coulombs (Factor vs Dipole = 173). Calcium produces an average bond length of 2.498*10'1°m with an effective charge of -7.3787x1 O'28Coulombs (Factor vs Dipole = 121). Aluminium produces an average bond length of 1.374*10'1°m with an effective charge of - 3.66x1 O'27Coulombs (Factor vs Dipole = 370).

[0154] As shown above, Potassium forms a bond with oxygen that is larger than a water molecule, allowing water molecules to penetrate the bond interface and interact with the cation / anion increasing the chance of breaking the bond. The factor stated in brackets is the relevant strength factor vs water dipole strength showing that alkali metals may be affected by the dipole moment whereas the alkaline earth metals are unlikely to be affected.

[0155] Due to alkali metals only having a +1 charge and large atomic radii, they have significantly lower effective charge than alkaline earth metals. This results in an effective charge between 2-4 times as strong in alkaline earth metals, compared to alkali metals, when ionically bonding with oxygen. Alkaline Metal Effective Charge {Coulombs)

[0156] X = The table below shows effective charge Alkali Metal Effective Charge Coulombs) of alkaline earth metals (Mg and Ca) vs effective charge of alkali metals (Na and K) using the following formula:

[0157] According to Pauling’s second law, the strength of an ionic bond to each atom is equal to the effective charge of an ion divided by its coordination number. Thus, in order of strongest possible ionic bonds with oxygen, the elements are as follows:

[0158] Conclusion: The preferred elements for ionic bonding of humic substances and phyllosilicate minerals to produce a fertile complex are scandium, magnesium, calcium, lanthanum, zinc and strontium.

[0159] Example 12 -Production of a Composition Comprising Humate and Clay (i.e. Production of a Stable Clay Humus Complex) Using Rock Mixture Instead of Clay

[0160] The desired amount of rock mixture was weighed out (based on desired chemical profile). The equivalent of 10% of the weight of the rock mixture was weighed out in calcium hydroxide (other divalent metal hydroxide salts could be used) and leonardite (1 :1 w / w ratio calcium hydroxide to leonardite). The method also works with the equivalent of 1% or 0.1 % of the weight of the rock mixture, but 10% is preferable. Water was measured out water in equal volume to the rock mixture.

[0161] The calcium hydroxide and leonardite were added to the water and stirred until uniform (for about 15 mins). The rock was added, and the mixture was stirred.

[0162] The hydroxide ions attacked the rock and it was broken down into clay particles which bonded with the humate salt to form clay-humus complex. The longer the mixture is left, the finer the product - immediate neutralisation forms a course product, but if the reaction time is increased prior to neutralisation, then the rock is broken down into clay-humus complex particles.

[0163] The pH was reduced to less than 7 and the mixture was left for 12 hours for the pH to equilibrate. The pH was then reduced again to less than 7. The product was dried using a dehumidifier and broken up into particles of the desired size. The product was then placed in a container and re-wetted, ready for planting. Further improvements could be made by adding organic matter and / or micro-organisms.

[0164] This method is advantageous as it removes the need for clay by using rock mixture as the starting material and reducing the rock into clay. The method is also highly water retentive and liberates ions from rock forming plant available nutrients, this reduces or possibly even eliminates the need for synthetic fertiliser. In summary, this is a simpler, very quick process and reduces the number of ingredients I reactants. One example of where this method can be used is in space travel as only leonardite (and optionally organic matter) is required to produce large quantities of fertile soil using just local rock. For example, calcium carbonate can be found on Mars and can be heated and subsequently hydrated to form calcium hydroxide for this method.

[0165] Whilst this method does work using carbonates (e.g. calcium carbonate), it works slower and through different pathways. The most likely pathway being the breakdown of carbonate into CO2 and Water, through acid-base attack, whilst the free calcium ion displaces the hydrogen in the hydroxyl groups directly or forms hydroxide ions by reacting with water resulting in a much weaker solution. The method works better with higher concentrations of hydroxide ions, which are difficult to obtain in sufficient concentration using, for example, just limewater which only possesses low concentrations of hydroxide ions. Reaction with humates is preferable because as the calcium ion is removed from solution, more hydroxide ions are liberated from the calcium hydroxide. This elevated level of hydroxide ions causes rapid breakdown of the rock mixture.

[0166] Example 13 - Comparison of the Crystal Structure of Unreacted Calcium Hydroxide, Calcium Humates / Fulvates (Primary and Secondary Extraction), Dry Mixed Calcium Hydroxide and Leonardite and Comparison of Surface Morphology

[0167] Equipment: 3L Plastic Jug, RO water, Leonardite, Calcium Hydroxide, Basalt crushed 0-3mm, 81% Phosphoric acid, 200w overhead mixer, 2L Duran bottle, 800mL Mayonnaise jar.

[0168] Methods: Calcium Hydroxide Slurry Preparation - Calcium hydroxide was stirred into RO water and analysed using top lit microscopy. A dry sample was prepared by tapping un-processed calcium hydroxide over a microscope slide.

[0169] Multiple Extraction Samples - 1400mL RO water was placed into the plastic jug. 90mL of Leonardite and 60mL of Calcium hydroxide were added. These were then mixed for 3 hours at 240 rpm. The overhead mixer was reduced to the slowest RPM possible and left for 20 minutes to allow the heavier particles to settle but keep the fine particles in suspension. The top layer of the solution was transferred to a Mayonnaise jar and neutralise using 5mL of phosphoric acid to reach pH6.2. This was set aside for later analysis (First Extraction).

[0170] The remaining thick solution with large dark particles was diluted to around 2.5L and approximately 100mL of calcium hydroxide was added. The sample was mixed at 160RPM for 1.5 hours and checked. Large dark particles were still visible, so the mixture was mixed for a further 2 hours. After settling the heavier particles using slow rotation, the upper layer was placed into a 2L Glass Duran Bottle and neutralised to pH6.8 (Second Extraction)

[0171] The remaining solution was diluted to 2L with RO water, 200m L of calcium hydroxide was added and left to mix for two hours. The upper layer was removed, placed into a mayonnaise jar and neutralised to pH 6.5 (Third Extraction).

[0172] The remaining solution was acidified repeatedly until a black syrup-like substance formed. I added some Calcium hydroxide, re-neutralised to pH6.8 and left to settle (Final Remains). Dry mixed Calcium hydroxide and leonardite preparation - A 1 :1 (%v / v) mixture of Calcium hydroxide and leonardite were placed into a mayonnaise jar. The sample was then aggressively shaken manually, ensuring audible impact of the lid and bottom, for approximately 5 minutes. The sample was then left to rest for 24 hours before being shaken again. This was repeated for two weeks. The sample was then analysed dry and post-wetting.

[0173] Observations: The leonardite becomes finer however the particles can be easily discerned under bright light using the naked eye.

[0174] Methods: Processed and Unprocessed basalt preparation - (10% Mix) 4500mL of RO water was added to a 20L bucket. 1025g Calcium Hydroxide and 1025g Leonardite was added to the bucket and stirred using the overhead mixer at approximately 30% Speed for 1 hr 15mins. The larger particles were then crushed and mixed in manually. 10250g of basalt was then slowly added to the solution over approximately 5 minutes to ensure sufficient coating. The pH was reduced using 500mL 81 % phosphoric acid and 200mL Biobizz Biodown (Based on lemon juice). Due to the high heat, an accurate pH could not be taken. The sample was left overnight to cool.

[0175] An additional 300mL of 85% phosphoric acid was added. Initially the pH reached pH5.1 but increased to pH6.1 after approximately 10 minutes of further mixing. The sample was left overnight to equilibrate.

[0176] The sample had risen to pH 7.5 so additional acid was used to reduce the pH to pH6.1. The sample was then placed under direct airflow of a dehumidifier for around 1 week to reduce the water content.

[0177] After the 10% Mix was dry, some particles that were clearly basalt were removed for analysis. The dry sample was brushed and analysed. The wet sample was aggressively washed in water and then rubbed aggressively dry using a clean cloth. For comparison, unprocessed basalt was also cleaned and prepared in the same way as above.

[0178] Dust analysis of Processed and Unprocessed basalt - After the processed basalt had dried, two larger rocks were separated and brushed clean. These were then struck together over the top of a microscope slide to capture dry particles for analysis. The same process was repeated with unprocessed basalt for comparison and the particles analysed.

[0179] Wet Analysis of Processed and Unprocessed Basalt - After pH reduction, a small quantity of the sample was placed into a 50mL centrifuge tube and aggressively shaken before being held stationary. As the particles began to settle, samples for analysis were taken from the top, mid and bottom section of the water column to analyse the particles based on their size and weight. The same preparation was done to unprocessed basalt for comparison.

[0180] Observations: The 10% Mix was extremely thin during the mixing stage and no noticeable accumulation of basalt was found at the bottom of the bucket - This was very unexpected. The particle size appeared reduced, and the consistency was like watery pea-soup. During the pH reduction step, the solution became thickest at around pH 10 and became continually thinner as the pH was reduced further below pH10.

[0181] Methods: Slide Preparation - A small aliquot of each sample was diluted in RO water and a drop placed onto a microscope slide for analysis. The samples were dried on a heat plate to see crystal patterns and analysed using top-lit microscopy.

[0182] Observations: Calcium hydroxide appears as an opaque, white colour.

[0183] The first extraction produced an intermix of different colour and size particles interlocked inside a clear crystalline substance. Upon drying, large plate-like crystals formed maintaining the interspersed coloured particles. It would appear that the range of humates and fulvates have formed different compounds with the calcium ions hence the differences. The clear crystalline structure could be a hydrated hydroxide crystal or a calcium-based crystal. Further analysis using superior equipment is required.

[0184] The Second extraction produced Hazy Blue-white crystals with clear definition and large quantities of dark-particles inside the structure. The dried samples have similar structure to the wet-dried calcium hydroxide samples. This is to be expected due to the large increase of calcium hydroxide in the sample.

[0185] The third extraction produced near-transparent crystals with the occasional dark particle visible. Upon closer inspection at higher magnification tiny dark particles could be found inter-dispersed however the concentration was greatly reduced, suggesting lower rates of reaction occurred after the second extraction.

[0186] The ‘final remains’ sample shows large dark particles however closer inspection of the particles clearly show chemical alteration compared to leonardite. There was evidence of some particles that looked like un-reacted leonardite. However, there was crystal growth on the outside suggesting either encapsulation preventing further extraction or chemical alteration that is difficult to discern with light microscopy. Higher magnification of the seemingly clear crystals were interspersed with dark particles and had a distinctive yellow-ish colour.

[0187] The dry-mixed calcium hydroxide and leonardite did show some evidence of reaction occurring, however the majority were clearly separate particles. For the most part, the sample when dry appears to reduce the particle size but does not react at a sufficient rate to be noticeable past this observation even after two weeks of interaction and impact mixing. The sample, when wet, has large, clearly unreacted leonardite embedded in an interlocking calcium hydroxide lattice. There is clear evidence of calcium hydroxide coating the leonardite but not reacting to form a humate / fulvate salt.

[0188] The Basalt post-process samples show a clear change when compared to unreacted basalt. After processing, the surface is coated in a crystalline substance. Dust analysis shows that a humate / fulvate complex has been formed.

[0189] Post-process water column samples show clear evidence of the formation of a new complex crystal. All crystals have dark patches showing that the larger crystals are made up from multiple small crystals, i.e it is not leonardite particles embedded in a crystal structure. The crystals themselves are various forms a calcium humate / fulvate compounds being bound together.

[0190] The unprocessed basalt mainly shows clear crystals or small fragments of basalt. There are some particles that look very similar to those being made during this process. Considering the basalt is a natural product and likely contaminated with soil, I would suggest that this is proof that this process is using the same principles as the natural processes.

[0191] The unprocessed and processed basalt surfaces are clearly different. The unprocessed basalt surface has translucent yellow crystals protruding from the surface amongst a black background. In other areas, the black crystalline structure has some clear-white crystal growth.

[0192] The processed basalt has a coating of smooth tan I white crystals interspersed with darker patches. There are areas that do not appear to have crystal growth on it which could be the quartz. The visual difference between the two samples is very clear. The processed basalt has smooth, tan-white crystal with dark particles interdispersed. The unreacted basalt has a jagged surface covered in clear-yellow crystals. These jagged crystals remained even after aggressive cleaning.

[0193] Conclusion: The different extractions produced very different crystal structures proving that the fulvic and humic acids are being extracted from the leonardite and reacting to form a humate / fulvate salt.

[0194] Dry-mixing Calcium hydroxide and leonardite has limited interaction largely producing finer particles of leonardite interspersed in a calcium hydroxide lattice forming a blend. Post-wetting with little to no mixing seems unable to produce Humate / Fulvate salts at a sufficient rate to be evident.

[0195] Particle formation is increased when the pH is reduced, and the resulting particles are larger however it is not the defining factor in the process as the particle have already been forming at the high pH stage.

[0196] There is a clear and identifiable difference in the surface profile of processed and unprocessed basalt proving interaction between the basalt and the solution.

[0197] 14 - Dissolution Test to Determine if Combination of Leonardite and

[0198] Calcium can ‘Dissolve’ Basalt, and Bind to to Form a '-Humate-Basalt Particle and '-humus

[0199] Equipment: 500mL glass jar x 4, Calcium hydroxide, Leonardite, Basalt Rock, Sieve, RO Water, 1000g scale with 0.1 readability, 200w overhead Stirrer.

[0200] Method: Pre-wash basalt in a fine kitchen sieve under aggressive water and movement until no further particles pass the sieve. Dry basalt in low heat with regular shaking to avoid hot spots. Ensure only solid, dry particles are transferred for testing. No particles below 1 mm in diameter. Prepare sample by measuring out calcium hydroxide and leonardite at a 1 :1 ratio and place into the glass jar. Add 60mL of RO water and mix at slow speed for 20 minutes (Approx 120RPM). After 20 minutes, add the basalt, weigh from the washed bulk, to the glass jar and mix for 20 minutes at 160RPM. Leave for 24 hours to soak with a lid to limit carbonate formation. Mix for 20 minutes at 160RPM and leave to soak for 24 hours. Mix for 20 minutes at 160RPM and take a sample. Reduce pH to less than 7 using an acid. Take a sample once target pH achieved. Leave sample to cool overnight. Retest pH. The sample taken is then diluted inside a pipette. Approx 0.2mL sample into 5mL. This is then placed onto a microscope slide and analysed using top illumination. Magnification 80x and 200x where higher magnification used. The basalt particles from each sample preparation were taken post-pH reduction, cleaned aggressively to remove any lose material, dried and analysed.

[0201] Discussion: 0% Sample - Prior to pH reduction, there is a snowflake like crystal formation with an opaque whiteness. After pH reduction the crystallisation becomes rounder and slightly clearer. There is no evidence of any clay particles or addition from the basalt. It seems that the calcium carbonate turns into Calcium phosphate or a similar compound.

[0202] 1 % Sample - Clear Change in crystal structure and an increase in different colouration. Most of the crystals are more see-through compared to the 0% sample with what looks like a coating of some sort creating a yellow I brown colour. The crystals are clearly grouping together both before and after pH Reduction. It is interesting to note that the dark, almost black particles are larger in the post pH reduction samples. There are some particles that look like the calcium-phosphate however they are clearly identifiable against the other, more numerous particles. Little to no evidence of clay in the liquid samples.

[0203] 10% sample - Same comments to above but the biggest difference is the large number of clay-humus particles that have been formed. These were not seen in the 0% or 1 % liquid samples. The dark, leonardite-looking particles have a different shape and colouration when compared against the majority of leonardite particles.

[0204] 10% no basalt - Prior to the pH reduction, there was clear evidence of calcium hydroxide still being present. There was no evidence of a clay-humus complex particle, however there was some unreacted leonardite and some hybrid crystals with a bluish-white outgrowth. After pH reduction, there is a dramatic and clear difference. The crystal size is almost incomparable however it is interesting that the majority of the crystals seem to be a bluish I white colour, some have remained very dark and then there is the occasional creme-coloured particle. There is no evidence of the clay humus particles as seen in the 10% including basalt sample.

[0205] Leonardite - The leonardite sample shows clear contamination of clay-humus particles in the background. Expected considering it is a natural, mined product. The large particles are a rich, deep black colour. Their texture is different to the dark particles being produced in the reaction.

[0206] Dry Basalt Post pH adjustment: Calcium Hydroxide only - The surface has clearwhite crystal bound to the surface of the rock. The basalt is generally smooth.

[0207] 1 % - Clear indications of calcium humate / fulvate deposition onto the surface of the basalt, however very sporadic and inconsistent. Surface is generally smooth with clearly unreacted features.

[0208] 10% - The calcium humate / fulvate deposition is more uniform across the surface. The general appearance is darker than that of the 1% sample. The surface is generally smooth with little crystal out-growth.

[0209] Unprocessed basalt - Patches of smooth and rough areas. The crystal formations generally protrude from the surface of the rock. The colouration of the white patches is clearer than in previous samples. The crystal outgrowth areas have clear protrusion and a tan colour.

[0210] Previous Tests - Referring to the calcium hydroxide and calcium humate I fulvate experiments (Example 12), this experiment looked at the effect on the surface of the basalt pre and post processing. The results show that the 10% sample is able to deposit and bond new material to the surface. This was also observed in the 1% sample but at a much lesser extend. This suggests that the reaction both requires time but also sufficient movement to remove the formed particles and allow further reaction to take place. pH - The amount of acid required to neutralise the sample suggest that the inclusion of both leonardite AND basalt changed the required amount of acid to neutralise the sample. Whilst at this time I have been unable to repeat the test and the error margin in the equipment used could explain the difference, other experiments suggested the same result. If this could be proved with more accurate data, this would further confirm the proposed reaction pathways.

[0211] Conclusion: The leonardite and calcium hydroxide solution are able to partially dissolve select parts of the basalt to form clay-humus complex particles. The 1% showed signs of reaction occurring, however this was seen as a deposition on the basalt surface rather than in the water column samples. This is likely due, however, to the concentration of hydroxide ions being insufficient for the reaction to occur at a more noticeable rate. These calcium-humus / fulvate complex particles both bond to the basalt rock itself and form particles that are released into the water column during the mixing phase. The particles formed are visibly different in all samples proving that reactions are occurring, depending on the reactants and is not a simple blend.

[0212] Summary of Examples 12 to 14: Production of Stable Complexes Using Basalt

[0213] Dry Leonardite and calcium hydroxide do not react sufficiently to form large quantities of Humate / fulvate salts - the particles stay mostly separate with some calcium hydroxide encrusting on the surface. Even post wetting, the particles do not mix and can be seen as separate entities. It needs time and physical movement to react properly.

[0214] Calcium hydroxide creates a slurry in water but does not dissolve. Post pH reduction, there is a clear difference in the formed crystals. Likely calcium phosphate or some variant.

[0215] The methods of the present invention form calcium humate and fulvate salts of various forms even prior to pH reduction. The larger particles are clearly made from smaller fulvate / humate salt crystals and higher magnification continues to show finer and finer 'speckles'. Reducing the pH increases particle size but the particle formation is clearly evident even at the high pH stage.

[0216] Calcium hydroxide and basalt in water can deposit calcium-based crystals but does not dissolve the basalt further than the surface crystals. Calcium humates and fulvates are able to dissolve basalt and form clay-humus particles. 1 % mainly just deposited on the surface. 10% has a clear clay formation on the surface and in the water column.

[0217] Contamination from the leonardite is not in sufficient quantities to explain the formation of the clay-humus particles alone as it was not seen in the preparation without basalt present at the same concentration.

[0218] The remaining dark particles, upon inspection, are clearly not leonardite and are some complex of heavy humic substances and crystals throughout the structure.

[0219] Based on these experiments, it is clear that the methods of the invention involve a chemical reaction, forming a unique and bonded particle. The resultant product is a complex structure (e.g. a clay-humus complex), chemically bonded into large crystals with defined cyst separation. The above results clearly show that the 10% sample can dissolve washed basalt to form clay-humus complexes, indicating that a chemically bonded complex is forming upon reaction with basalt, as well as natural clay. In combination with the previously highlighted increase in temperature, the above observations provide further evidence that the methods of the invention are chemical pathways creating chemically bonded products, not blend or mixtures. This is further supported by the observation that the resultant product is visually different to the dry-mix sample prepared.

[0220] Examples 12 to 14 (and Examples 15 onwards below) provide evidence that the methods of the invention work using basalt as an alternative starting material to clay. The methods are observed to alter the properties of basalt and form a clay-like substrate comparable to the bentonite preparations analyzed in the earlier examples (Examples 1 to 11), which suggests a similar reaction pathway. The basalt preparations have also shown promising potential for plant growth, removing the need for clay as an input. This supports the finding that both clay I bentonite preparations and mineral mixes, e.g. using basalt, result from a chemical reaction.

[0221] The use of basalt, or other rock species as previously described, as a replacement starting material to clay, has the potential to create an even more meaningful global impact. The simplified steps offer a significantly more field-ready approach compared to previously known processes, and notably, the implementation of the process is far more cost-effective thereby reducing the barriers for implementation. This makes the process much more scalable and practical — particularly for converting degraded or otherwise unusable land into fertile, productive ground.

[0222] Example 15 - 20%, 30% and 40% Test and Crush Test

[0223] Aim: To see if the increased concentration of leonardite and calcium hydroxide can break down Basalt faster and bind to the Silicate compounds to form Clay-Humate- Basalt particles and Clay-Humus complexes.

[0224] Equipment: 500mL Beakerx2, 800mL glass mayonnaise jarx 1 , Calcium Hydroxide, Leonardite, Basalt Rock, Sieve, RO Water, 1000g scale with 0.1 readability, 200w overhead Stirrer. Method: Basalt aggregate was dry sieved and washed to remove any particles 1mm or less. The samples were then dried in the oven at approximately 100 degrees for 2 hours before being left to cool.

[0225] For all samples, Calcium Hydroxide and Leonardite were placed into a 500mL beaker (20% Sample - 20g of Calcium Hydroxide and 20g of Leonardite, 30% Sample - 30g of Calcium Hydroxide and 30g of Leonardite, 40% sample - 40g of Calcium Hydroxide and 40g of Leonardite). 60mL of RO water was then added and the overhead was used to mix the reactants at a slow fixed speed, to reduce the ingress of air interacting with the cations in solution. This was left to mix for 2 hours (6 hours for 40% sample) prior to the addition of 100g of Basalt. The sample was then mixed for 30 minutes at 160RPM before being sealed and left to soak for 24 hours. The sample was then mixed for another 30 minutes at 160RPM before being sealed and left to soak for 24 hours. The sample was mixed for a final 30 minutes at 160RPM before being neutralised using 81% Phosphoric acid to <pH7. The sample was then left to equilibrate overnight prior to a second neutralisation.

[0226] Samples were taken from high-pH and Low-pH states for comparison. A small portion of Basalt was removed from each sample after 24 hours to investigate the compression strength of the Basalt prior to pH reduction. Another sample was tested post pH reduction. The samples were left exposed to the air without active airflow being applied to see how long it would take for the sample to dry out.

[0227] Results:

[0228] Observations: After mixing with the Calcium-Humate, the solution became progressively darker with noticeable large black particles interlocked between a pinky-coloured solution. After adding the Basalt, the solution became almost black in colour. 40% and 30% had to have additional water added during the pH reduction as the sample dried out too quickly (Approximately 20mL). Further study is needed to determine whether the water simply evaporated or became bound as part of a crystalline structure. The samples seem to have formed a large clay-like matrix with high water-retention.

[0229] 20% - Remained a relatively thin liquid after 6 hours of settling. Post Basalt addition texture was similar to semolina with most of the large Basalt particles dropping to the bottom of the beaker.

[0230] 30% - Remained a thick liquid after 6 hours of settling. Post Basalt addition texture was similar to ice-cream. It appeared to have lumps.

[0231] 40% - Initially appeared the thinnest I most watery of the samples and quickly started to become a uniform solution even with simple hand mixing. Once mixed, the sample quickly became a lumpy paste. The sample was left to mix at 160RPM for 6 hours prior to the addition of Basalt. As a timer had been used, the sample had been able to rest for a short while before being neutralised. The sample became very thick and took very high RPM to get the whole sample back into a liquid state. Once the sample was liquid, the rotation speed was reduced back to160RPM and the sample would mix uniformly. After the addition of Basalt, the sample quickly became a thick paste, similar to a high-quality humus. An additional 15mL of RO water was added to the sample prior to the third mixing as the sample was too thick and the overhead mixer head just carved a hole.

[0232] All samples appeared to thicken over time when at rest and would become more liquid with increasing rotation. The increasing concentration of Leonardite made the samples a lot smoother and, from observations made during the mixing stage, seemed to have significantly reduced the particle size of the Basalt even prior to pH reduction. After 7 weeks, the samples were tested and still found to be wet. After 8 weeks the samples were dry.

[0233] Crush Test Method: Particles of Basalt were placed between two stainless steel samplers and pressure was applied by hand using fingers as the base and two thumbs applying increasing pressure. Another small sample was placed onto a plastic plant tray and crushed by applying downward pressure in a rotating pathway. Samples were analysed using top-lit microscopy.

[0234] Results / Observations:

[0235] Example 16 - Basalt Comparisons Through the Process

[0236] Samples were prepared by sieving Basalt aggregate through a 1-1.5mm sieve, washing the rocks using RO water and drying them in an oven at 80 degrees centigrade. The samples were then mixed using the 30% recipe (30g of Calcium Hydroxide and 30g of Leonardite to 100g of Basalt) and sampled throughout the process. The samples were dried using a de-humidifer, washed using RO water, dried in the oven and then investigated.

[0237] Plain Comparison - Washed only: Dark Rocks are typically dark, almost black in appearance with dark glassy structures and small protruding crystals. When cleaned the protruding crystals were removed. There were orange-red patches indicative of iron-based compounds. Some clear phenocrysts and white phenocrysts are also present. Some very small amounts of dark inclusions are evident in some phenocrysts but not all.

[0238] Light coloured rocks are typically white and cream coloured with some dark patches, black spots and occasional orange patches.

[0239] Basalt dust is characterised by clear I white crystals outgrowing from darker core crystals. White, cream and yellow crystals with some inclusions are also seen.

[0240] High pH Samples - Post wash: Dark Rocks are characterised by dark out-crops and golden-brown crystal deposition intermixed with dark inclusions. White I Clear sections appear larger and with a higher concentration of dark inclusions. Noticeably the inclusions are both on the surface and inside the crystal structure. Light coloured rocks are characterised by an increase in the concentration of inclusions found in and on the crystal structure. Larger crystals have largely been replaced by smaller composite crystals.

[0241] Basalt dust is characterised by a nearly uniform golden-brown colouration. Crystals I rocks have largely been replaced by composite crystals of the same colouration. Some larger coloured crystals have noticeable inclusion within their crystal structure not seen in plain Basalt. Some white crystals have grown clearly a carbonate structure. During the analysis, the carbonate could be seen forming as the sample reacts with CO2 from the air.

[0242] Low pH - Post wash: Dark coloured rocks have large amounts of golden-brown crystal deposition with interspersed black inclusions. Whilst there are some noticeable Leonardite remains, many of the smaller inclusions are orange, pink, red, purple etc.

[0243] Light-coloured rocks have a darkened colouration and there is a wider variety of colours being displayed. Many crystals appear to be a hybrid of multiple smaller crystals. New large glass-like structures with inclusions and pieces of Leonardite can also be found on occasion.

[0244] Basalt dust remains are much more uniform with a darker golden brown interspersed with dark coloured inclusion. The inclusions do not appear uniform in their colouration. Whilst there are some noticeable Leonardite remains, many of the smaller inclusions are orange, pink, red, purple etc. The general colour has become noticeably darker.

[0245] Example 17 - Basalt Weight and Surface Effects

[0246] Aim: To investigate the effect of the various steps within the process on the Basalt to determine the overall effect.

[0247] Equipment: 500mL glass jar x 11 , Calcium Hydroxide, Leonardite, Basalt Rock, Sieve, RO Water, 1000g scale with 0.1 readability, 200w overhead Stirrer.

[0248] Method: The Basalt was pre-washed in a sieve with an average hole diameter of 1- 1.5mm. The sample was rinsed with RO water and then dried in the oven at approximately 85 degrees centigrade. This ensures all particles 1 mm and smaller were eliminated prior to the investigation. For all samples, 100g of Basalt was weighed out and put aside. The overhead mixer was fixed to the same depth. Samples 1-5 were mixed for 2 hours every 24 hours for 1 week comprising a total active mixing time of 14 hours. Samples 6-9 were mixed for 14 hours continuously. This was achieved using a mechanical plug timer.

[0249] For samples 1 -5 the mixer paddle was approximately 1 depth in the water. The RPM was set by turning the overhead mixer to the slowest rotation before it stopped and then adding a small buffer increase in speed to reduce the chance of stoppage. Samples 6-9 had variable RPM with the paddle placed just above the very bottom on the beaker for maximum contact with the sample. The RPM was calculated manually by counting the full rotations performed in 1 minute. 3 measurements were taken over 5 minutes for verification. Samples 10 and 11 were lightly swirled after being bathed in undiluted 81% phosphoric acid for 1 minute and 2 hours respectively.

[0250] Further investigation was carried out to determine the slowest possible rotation speed for each of the preparations. A representative sample for 30% and Basalt only were prepared using the same method. The overhead mixer blade was placed in the lowest position, just above the bottom of the beaker, and the overhead mixer was set to the slowest possible speed and measured 3 times. If the slowest speed stopped within 10 minutes, the result was discarded, and the test was re-started.

[0251] All samples were prepared in a 500mL beaker by combining the leonardite and calcium hydroxide in 120mL RO water followed by the addition of 100g basalt. The samples were mixed with the overhead mixer, washed using a shower head until they ran clear, rinsed in RO water and dried in the oven for 2 hours at 80 degrees before being re-weighed. The samples were as follows:

[0252] Sample 1 (Basalt and Water) - Basalt Only, Half-depth, 14 hours continuous at 75RPM

[0253] Sample 2 (30% - 5-hour High pH) - 30g Calcium Hydroxide, 30g Leonardite, Half Depth, 5 hours continuous at 75RPM

[0254] Sample 3 (30% - 14-hour High pH) -. 30g Calcium Hydroxide, 30g Leonardite, Half Depth, 14 hours continuous at 75RPM

[0255] Sample 4 (30% - 8-hour Low pH) - 30g Calcium Hydroxide, 30g Leonardite, Half Depth, 8 hours continuous at 75RPM Sample 5 (30% - 14-hour Low pH) - 30g Calcium Hydroxide, 30g Leonardite, Half Depth, 14 hours continuous at 75RPM

[0256] Sample 6 (30% - 14-hour pH3.3 for 1 minute No dry) -30g Calcium Hydroxide, 30g Leonardite, Half Depth, 14 hours continuous at 75RPM. Note - Unfortunately, too much acid was added erroneously causing the solution to reduce to pH3.3. The sample was immediately diluted using standard tap water until pH6< was achieved and placed back into the sieve and washed with RO water until running clear. The sample was then further washed using higher pressure from a shower head and repeatedly shaken until the water ran clear with no further signs of material being removed. The sample was then rinsed with RO water, placed onto a metal baking tray and dried in the oven for 2 hours at 80 degrees centigrade before being left to cool and weighed.

[0257] Sample 7 (Basalt and Water only 90RPM) - Basalt only, Bottom Depth, 14 hours continuous at 90RPM

[0258] Sample 8 (Basalt and Water only 120RPM) - Basalt only, Bottom Depth, 14 hours continuous at 120RPM

[0259] Sample 9 (Basalt and Water only 200RPM) - Basalt only, Bottom Depth, 14 hours continuous at 200RPM

[0260] Sample 10 (Acid was 1 minute) - 100g of Basalt was placed in a 500mL beaker and Phosphoric acid was added until the whole sample was submerged by approximately 1cm. The sample was swirled by hand for 5 seconds then left to rest for 60 seconds. The Sample was hand swirled for another 5 seconds and then immediately placed back into the sieve and washed with RO water until it ran clear. The sample was then further washed using higher pressure from a shower head and repeatedly shaken until the water ran clear with no further signs of material being removed. The sample was then rinsed with RO water, placed onto a metal baking tray and dried in the oven for 2 hours at 80 degrees centigrade before being left to cool and weighed.

[0261] Sample 11 (Acid Wash 2 hours) - 100g of Basalt was placed in a 500mL beaker and phosphoric acid was added until the whole sample was submerged by approximately 1cm. The sample was swirled by hand for 5 seconds then left to rest for 120 minutes. The Sample was hand swirled for another 5 seconds and then immediately placed back into the sieve and washed with RO water until it ran clear. The sample was then further washed using higher pressure from a shower head and repeatedly shaken until the water ran clear with no further signs of material being removed. The sample was then rinsed with RO water, placed onto a metal baking tray and dried in the oven for 2 hours at 80 degrees centigrade before being left to cool and weighed.

[0262] Sample Weight Reduction Investigation Results:

[0263] Slowest RPM Investigation Results: Hand Swirl and Magnetic Stirrer Results (see sample preparation in Example 18 below):

[0264] Discussion: During the washing stages, it was noted that when the residues were being washed using normal tap water, the change in pH was causing rapid flocculation into larger particles. It was also noticed that when instruments were being cleaned, extremely fine particles came together even during the active cleaning and settled as noticeably large crystals approximately 1 mm in size. This suggests a high charge imbalance in the crystals of the product. It was interesting to note that although the initial samples suggested that there was a direct correlation between the various major steps and the amount of reduction in weight of the retained Basalt particles, later samples do not seem to support the initial observation and actually suggest the opposite. The Calcium Humate seems to be acting as a lubricant and reducing the amount of energy required by the overhead mixer. It is also interesting to note that sample 7 appeared successful due to the overall weight reduction. However, in later tests, the same RPM was not achievable without the overhead stirrer becoming stuck. This may be due to natural variation within the aggregate sample resulting in larger particles being present in later samples or that the stirrer indeed became stuck. The limited weight reduction seen in sample 1 is likely due to the half-depth placement of the mixer blade which reduced direct contact between the Basalt and the blade-head.

[0265] The acid tests suggest that up to 3.2% of the weight loss could be attributed to acidic attack. This is largely negated, however, due to the high pH of the sample prior to acid addition. The protons will likely be neutralised instantly upon contact with the solution leaving the conjugate base to react elsewhere. The 1 -minute sample appeared to have little effect on the overall particle size however the Basalt was noticeably light in colour once dried when compared to just washed and dried aggregate. The 120-minute sample resulted in significantly reduced Basalt size and a much lighter colour giving the Basalt a silvery appearance.

[0266] Samples that included Calcium-Humate I Fulvates were noticeably darker than the washed and dried Basalt. It should also be noted that the longer reaction times resulted in darker Basalt in the end however the pH did not have as much of difference on the final colour. This suggests that the effect is not simply caused by the product materials depositing themselves onto the remaining Basalt as a shell or there would be a difference in colour between High and Low pH which is not seen as much as between 5-hour and 14-hour samples.

[0267] When analysed using top-lit microscopy, there is clear evidence of deposition on the surface of the Basalt with higher concentrations in the low-pH samples even post aggressive washing. It was also interesting to note that many of the medium sized particles were not Basalt but appeared to be calcite-like with heavy inclusion of dark material. This suggests that the coagulation of the product is forming crystals larger than 1mm and likely forming thick coatings on the remaining Basalt. Sample 5 has a remaining weight between the Basalt only samples mixed at 90RPM and 120RPM. Considering the sample was mixed at 75RPM, and the mixer was not placed at the bottom, this suggests that the process may be affecting the structural integrity of the Basalt, reducing the amount of energy required to reduce the particle size.

[0268] Both the Hand-Swirl and Magnetic Stirrer samples showed an increase in weight, both at high and low pHs, suggesting deposition on the Basalt surface irrespective of pH. When the samples are compared side-by-side there are clear visual differences between the two samples with the magnetic stirrer sample having noticeably darker basalt remains. As both samples were prepared at the same time and under the same conditions, this suggests that movement of the reactants is required for the reactants to interact with the Basalt in a measurable way.

[0269] Due to the limited number of samples prepared, it is difficult to make further analysis, however the general trends are consistent with observations made during earlier preparations.

[0270] Example 18 - Basalt Particle Size Distribution

[0271] Aim: To determine the effect of various processes on the final particle size distribution when compared to the initial particle size distribution.

[0272] Equipment: 500m L glass beaker, Calcium hydroxide, Leonardite, Basalt Rock, Sieve, RO Water, 1000g scale with 0.1 readability, 200w overhead Stirrer, Magnetic stirrer.

[0273] Method: Basalt rock was washed through a sieve with a hole diameter of 1-1.5mm diameter. The Basalt was then dried for 5-6 hours in the oven at 80 degrees centigrade with intermittent mixing to dry uniformly. Once finished, a small sample of the dried Basalt was measured to determine the particle distribution of the individual Basalt rocks. The batches were then separated into 100g samples. Initial samples were compared against the raw particle distribution from 1mm< Later samples were further separated to remove any particles below 4mm.

[0274] Sample ‘washed only’ was taken from the bulk sample and the particle distribution was determined by measuring the longest length possible of each rock I particle. Later samples had their individual particle distribution determined both pre and post processing. The following samples were taken from the same bulk batch of washed Basalt and therefore compared against ‘washed only’: 1 - 30%, 7 Days, 14 hours, Low pH, 75RPM; 2 - 30%, 3 days, 8 hours, Low pH, 75RPM; 3 - Basalt Only, 14 hours, 200RPM.

[0275] The following samples were tested before and after the process: 1 - Basalt Only, 14 hours, 120RPM; 2- 30%, 14 hours, Low pH, 75RPM; 3 - 30%, 14 hours, Low pH, 120 RPM; 4 - 30% 14 hours, High pH, 120RPM; 5 - Hand-Swirled, 30%, 1 Week; 6 - Magnetic Stirrer, 30%, 1 week.

[0276] Sample preparation I Method:

[0277] Samples were prepared by adding 100g of basalt to a solution comprising of 30g of Leonardite, 30g of Calcium Hydroxide and 120mL of RO Water pre-mixed for approximately 30 minutes. The samples were mixed at the specified RPM for equal hours over the number of days specified, with rest periods having the samples covered to stop interaction with the atmosphere. Where there is no indication of days, the sample was mixed continuously. After the final mix, the low pH samples were reduced to less than pH 7 using 81% phosphoric acid. The sample was then washed, dried and measurements taken. The samples were as follows:

[0278] Washed only - 100g of the bulk washed and dried Basalt sample was weighed out. A small portion was then measured using a ruler to determine the longest possible length and this was recorded.

[0279] 30%, 7 Days, 14 hours, Low pH, 75RPM

[0280] 30%, 3 days, 8 hours, Low pH, 75RPM

[0281] Basalt Only, 14 hours, 200RPM

[0282] Basalt Only, 14 hours, 120RPM

[0283] 30%, 14 hours, Low pH, 75RPM

[0284] 30% 14 hours, Low pH, 120RPM

[0285] 30%, 14 hours, High pH, 120 RPM Hand Swirled sample - 30g of Calcium hydroxide, 30g of Leonardite and 120mL RO water were added to a 2L Duran bottle and mixed by hand swirling periodically over approximately 8 hours prior to the addition of 100g washed and dried Basalt. The sample was then slowly swirled by hand one to two times per 24 hours for 1 week. The liquid layer was separated into a sealed jar for use later. The remaining Basalt was washed through the sieve under RO water before being dried in the oven at around 80 degrees centigrade for 2 hours before being weighed and the particle distribution measured. The sample was then re-added to the solution and left to sit for 2 hours before being neutralised using 81% Phosphoric acid. The sample was then dried in the oven at 80 degrees centigrade. It was then dry sieved to retain the dust layer. The Basalt was washed using RO water and a showerhead, rinsed with RO water before being dried in the oven at 80 degrees centigrade for 2 hours, weighed and the particle distribution measured. (27.2g of sample was measured).

[0286] Magnetic stirrer sample was prepared by adding the 30g of Calcium Hydroxide and 30g of Leonardite to a 500mL beaker and being lightly hand mixed. The dry mix was then pushed to the edges of the beaker, 200m L RO water added and a 25mm magnetic flea was dropped in center. The stirrer was turned to half speed. The beaker was then covered using a nitrile glove and the stirrer turned to maximum speed until the solution became uniform. The magnetic stirrer was then reduced to half power. The sample was left for 24 hours to mix thoroughly. A small amount of Basalt was measured to determine the size distribution and only those that were measured were added to the sample after the first 24 hours mixing. The Basalt rocks were added to the edges, careful not to be hit by the magnetic flea. The sample was then left for 1 week to react. Once per 24 hours the glove was removed, and the Basalt was lightly moved around with wooden chopsticks for 30 seconds before being re-covered. This was done to expose new sides to the flow of reactants. The liquid layer was separated into a sealed jar for use later. The remaining Basalt was washed through the sieve under RO water before being dried in the oven at around 80 degrees centigrade for 2 hours before being weighed and the particle distribution measured. The sample was then re-added to the solution and left to sit for 2 hours before being neutralised using 81% Phosphoric acid. The sample was dried in the oven at 80 degrees centigrade. The sample was then dry sieved to retain the dust layer. The Basalt was washed using RO water and a showerhead, rinsed in RO water before being dried in the oven at 80 degrees centigrade for 2 hours, weighed and the particle distribution measured. Results:

[0287] Increasing overhead RPM increased particle size reduction. The reduction appears consistent across all particle sizes suggesting a grinding I abrasive reduction.

[0288] There is a significant increase in particle size reduction when comparing total time rather than mixing time suggesting the ‘rest’ periods were still causing a reaction.

[0289] Basalt processed in Calcium Hydroxide and Leonardite solutions show a significant increase in smaller sized particles between 1-4mm when compared against plain RO water samples suggesting a different mechanism behind particle reduction.

[0290] Movement of the solution has an impact on the reactants’ ability to interact. Whilst there is some particle size reduction from the hand swirl sample, the magnetic stirrer sample showed significantly higher rates of particle size reduction.

[0291] Below is the difference in percentage of the Basalt particle size when compared to the distribution prior to processing.

[0292] Discussion: The results suggest that the process is changing the overall Basalt particle distribution, with each subsequent step producing a higher distribution of smaller particles. Variable factors were minimised by using the same amounts of each ingredient / reactant, same vessel types and mixing depth. When comparing the results obtained from different RPM samples of plain Basalt, it is evident that a higher RPM increases the rate of size reduction. There is also a significant increase in the rate of size reduction when the mixer paddle is in the lowest position.

[0293] When comparing the samples with the same RPM, the data suggests that the neutralisation step has a significant impact on the production of smaller sized particles in the range of 2-4mm. When comparing the data from the 30% 75RPM samples, it suggests that both the amount of time in solution, and the number of hours of active mixing, influences the final particle distribution.

[0294] The hand swirled sample was swirled for a minute before being left for 24 hours. This was repeated for a week, so the sample was largely stationary. The results showed a slight increase in particle size, at high pH, consistent with observations of the Calcium Humate / Fulvate complex deposition. The weight recorded was also 102 grams showing at least a 2% increase in weight both Pre and Post pH reduction. Whilst a slight change can be seen in the hand swirl sample, there is no significant overall change.

[0295] The magnetic stirrer sample shows a reduction in particle size at the high pH sample and then appears to show a slight increase in size post pH reduction. This is consistent with other experiments suggesting that the Basalt is becoming a reactant, conditional on consistent movement of the solution, and that the neutralisation step is causing the flocculation of small particles into larger aggregate crystals. As the magnetic flea used is just 25mm, it is not sufficient to lift the Basalt particles eliminating the effect of grinding or high energy impacts. As only measured particles were added, this eliminates the natural variation. The main variable is the judgement of the analyst on the particle size.

[0296] There was a noticeable difference in the final appearance of the Basalt between the hand swirl and magnetic stirrer samples.

[0297] Example 19 - Bentonite vs Basalt Dust Comparison

[0298] Aim: To understand the effect of different starting mineral composition I forms.

[0299] Equipment: 800mL glass jar with lid x 3, Calcium Hydroxide, Leonardite, Basalt Rock, Bentonite, Sieve, RO Water, 1000g scale with 0.1 readability, 200w overhead Stirrer. Method: 30g of Calcium Hydroxide and 30g of Leonardite was added to the jar alongside 120mL of RO water. The overhead mixer was placed just above the bottom of the jar and set to approximately 160RPM. The reactants were mixed for 15 minutes before adding the mineral component. The samples were then mixed for 2 hours before being sealed and left to rest for 24 hours. This was repeated for 1 week before being neutralised to less than pH7. The sample was dried in the oven for approx. 6 hours at 80 degrees centigrade before finishing under a stream of dehumidified air overnight. Samples were analysed using top-lit microscopy.

[0300] Sample 1 - 100g of 1 :2 Na:Ca Bentonite (RPM of 200-240 for uniform mixing).

[0301] Sample 2 - 100g of Basalt dust (Passed through Sieve).

[0302] Sample 3 - 100g of Sieved and washed Basalt (Retained by sieve).

[0303] Results: Macro observations show three distinct colours visible in the final product. The Bentonite sample had a paler colour, the Basalt dust had a light brown colour and the Basalt preparation had a very dark colour and a noticeably lumpier consistency. The Bentonite and Basalt dust preparations appear to have formed a similar macro-structure both in texture and in reaction to the drying process. This type of cracking is typically seen in dried soil with high-clay content. The Basalt preparation was noticeably darker than the other preparations and had a lumpy texture with clear Basalt particles remaining. The Basalt rock sample seemed to aggregate into larger particles than the Bentonite or Basalt dust suggesting an improved structure. When compared, using microscopy, the samples seem to be forming similar structures in physical characteristics although the difference in colour suggests that they are forming different products chemically.

[0304] Discussion: The Bentonite sample, when compared to plain Bentonite has a noticeably more golden-yellow colouration and clear integration of Calcium Humate I Fulvate crystals within the macro structure. Plain Basalt is mostly white with some pale-yellow colouration in some of the particles. At higher magnification, the plain Bentonite has a more noticeable yellow hue. There was clear evidence of the same crystal morphology with dark inclusions being present in much finer crystals. Typically, they have a more reddish colour than the larger dark crystals observed. When analysing the Low pH samples, distinct crystals were also found with significant quantities of dark inclusions suggesting formation during the chemical reaction. The Bentonite sample post-pH reduction takes on a more golden-yellow colour with a different sheen compared to the plain, raw Basalt suggesting a different chemical composition.

[0305] The Basalt dust preparation, when compared to plain Basalt dust, has a noticeably darker colour and the inclusion of Calcium-Humate / Fulvate crystals. When compared to the Bentonite sample, the colour has a more golden-brown colour.

[0306] The Basalt preparation is very similar in appearance to the Basalt dust preparation when viewed under a microscope. All preparations have white particles with dark inclusions suggesting the formation of carbonate compounds.

[0307] All preparations formed a noticeably lighter layer where it had been exposed to the atmosphere. When compared, they have a much higher concentration of carbonate compounds, suggesting there are still free cations present after neutralisation, which interact with carbon dioxide to form carbonate compounds.

[0308] Without chemical analysis, it is impossible to determine exactly what the products are, however it is clear that the atmosphere has a large effect on the final product. Higher yields of the target products could potentially be achieved by conducting the reaction and drying under pure nitrogen.

[0309] Example 20 - Following the Chemical Route (Comparison of raw material to the products produced at various points throughout the process)

[0310] Aim: To see if it is possible to identify the different products being produced in the reaction and try to identify their likely composition.

[0311] Eguipment: AmScope T490 Series Trinocular Biological Compound Microscope 40X-2000X with a C-mounted 5MP MA500 camera (1 / 2.8" CMOS), Magnification optics used were the 4x, 10x and 40x, Microscope LED ring with white light and stepless dimmer control (Unspecified but estimated to approximately 5000-6000K).

[0312] Method: Samples were taken from various experiments and raw material. Method of preparation included (1) dry dusting on microscope slide, (2) small piles of dry material on a microscope, (3) dropping a single drop of liguid sample to the microscope and diluting using RO water then spreading the sample and (4) following method step 3, allowing the sample to airdry / heat dry using open flame. The light was held at approximately 45 degrees at approximately 12 cm from sample. Photos were taken using the MA500camera and TCapture software. Most images were captured with a single shot however large 3D objects were also focus stacked using the free trial period of Zerene Stacker (64bit) Software. The images were prepared in order of the process for easy fellowship.

[0313] Results: Clear differences could be seen through the various stages of the process. The products formed were unique in appearance at each step.

[0314] Discussion: Calcium Hydroxide is a translucent I opaque white substance without any noticeable inclusions or dark patches. Even at high magnification, the samples’ overall appearance does not change.

[0315] Leonardite is a shiny, uniformly black material. The dust shows clear signs of other material being included. Due to this product being of natural origin, it is suspected to be Soil I Sand as residual contamination from the extraction process.

[0316] Calcium Humate (High pH) is a solution largely made up of white I clear crystals intermixed with very small dark inclusion, chunks of unreacted Leonardite and distinct white crystals with dark inclusions. There are also very occasional instances of golden crystal complexes incorporating dark particles present (<1 %). It should be noted that the smaller dark patches that are always inclusive in larger particles do not appear black when seen through the eyepiece. They appear purple and sometimes with a red-orange hue. It is interesting to note that if the Calcium-Humate has mixed for longer, the majority of the clear crystals take on a slightly pale-yellow hue. Crystal formation is also noticeable with larger particles looking like Calcite and Carbonate compound rocks. It is suspected that the white crystals are forming due to interaction with Co2 from the atmosphere with the clear crystals being the Hydroxide.

[0317] Calcium Humate (Low pH) produces a uniform product comprising of a pale creamyellow crystal interlocked with dark (not black) inclusion of various diameters. These crystal complexes are forming prior to dehydration suggesting a favoured state. Post-drying produced a slightly whiter product, which is likely due to additional formation of Carbonate compounds increasing the reflectance. It is suspected that this crystal is a Calcium-phosphate based crystal with Calcium-Humate I Fulvate inclusions. Calcium Humate with Basalt (High pH) is a dirty-brown-yellow colour. There is a noticeable increase in the amount of coloured crystals, including purple / maroon, red, orange, yellow and green. Larger crystals have formed in the high pH environment which are noticeably different to Calcium-Humate only samples.

[0318] Calcium Humate with Basalt (Low pH) is largely uniform. The colour changes to a golden brown intermixed with darker crystals and the occasional white crystal. It should be noted that even upon higher magnification, clear darker inclusions of various sizes are always found. Inclusions were seen within the particle. Most of the particles produced had a noticeable sheen, almost but not quite metallic.

[0319] Bentonite with Calcium Humate (Low pH) is a yellow hue when compared to plain Bentonite and has a significant increase in dark and coloured inclusions. Isolated particles show the same characteristics as the Basalt low pH samples.

[0320] All samples showed clear inclusion of unreacted Leonardite chunks. It is unknown currently whether this is due to incorrect reaction conditions or whether these are the carbon remains from the Leonardite (Leonardite is directly related to lignite, a soft, brown coal). Further investigation is required.

[0321] Due to various minerals looking similar and that changing hue can be imparted through crystal structure and impurities, it is not possible to identify the exact chemical make-up of the products without suitable analytical equipment and a reference library. It is, however, clear that there are physical differences between all samples analysed.

[0322] At High pH when rested, including post Basalt addition, a layer of yellow liquid was visible above the particles which had settled into a distinct layer. The extracted yellow liquid is likely Fulvic acid in solution.

[0323] Post-neutralisation step, the particles settled into a distinct layer with a clear liquid layer above suggesting the Fulvic acid has been incorporated into the final product.

[0324] Example 21 - Artificial vs Natural Soil Comparison

[0325] Aim: To compare artificial vs soil samples collected from various locations in Malta.

[0326] Background: Malta’s native soils are primarily calcareous characterised by high levels of Carbonates and bicarbonates. This typically forms the Limestone, Dolomite, Globerigina and Green-Clay layers. In the northern part of the island, the soil changes to a red soil which constitute the more fertile soils within Malta. These are characterised by a higher level of Iron-Silicate minerals and lower levels of Carbonate compounds.

[0327] Equipment; 100mL Glass measuring cylinder, Microscope slides, Spatula, Plastic Pasteur Pipette, AmScope Trinocular Microscope with 5MP camera. 4x and 10x optics (Note - According to information available on the AmScope website, the camera provides an effective magnification of 30-40x. This results in a total effective magnification of between 160x - 400x). The light source is a microscope LED ring with a cold white colour (unspecified by the manufacturer).

[0328] Method: Small samples of natural soil from various locations around Malta were analysed using top-lit microscopy. The samples were prepared by (1) lightly knocked above microscope slide to see dry clay layer, (2) wet and dried into a flat layer, (3) gravity separated using a water column with the bottom, middle and top layers analysed for analysis of different sized particles.

[0329] If it was not possible to obtain an image where the entire field of view was in focus, a program called Zerene Stacker was used to create a single stacked image to provide an in-focus image across the entire field of view. The Images were processed using DMap and PMax techniques and poorly resolved areas were overlayed with sections from the in-focus image using Adobe Photoshop. Samples were then compared side by side to compare overall structure and determine whether the process is creating a similar compound.

[0330] Results: Natural soil has a complex composition, texture and colour typically comprising of multiple discrete crystals bonded together to form a larger complex. The quantity of dark inclusions varies depending on their location of origin. Undisturbed soil typically exhibits higher concentrations of dark inclusions than those taken from farmland. Most of the samples analysed have a very noticeable red colour suggesting higher concentrations of Iron-based Silicate compounds.

[0331] The artificial soils are similar in structure although lack the red colour of the natural samples. The artificial soil typically comprises of golden-brown crystals with dark inclusions, however there are also crystals with a completely different colour but still displaying dark inclusions. Discussion: The natural samples have a much more complex composition suggesting a composite particle comprising of many different discrete crystals. Some samples appear to lack dark inclusions, suggesting low levels of organic matter being present. Other natural samples show high levels of dark inclusions more comparable to the artificial soils being produced. The red hue in the natural samples suggests iron-based silicate compounds and the white particles are likely Carbonate based. When excluding the colour, the artificial sample has the same general composition as the natural samples. A consistent theme across all samples is that they are comprised of translucent crystals with dark inclusions. This suggests that the method used to form the artificial soil is producing similar products to that of the natural processes. The higher complexity of the natural samples could be due both to the higher variance of material available for a reaction and the effects of agriculture I microbial I fungal attack.

[0332] Artificial soil produced using Bentonite, particularly with additional organic matter, is more comparable to the natural soils tested than the basalt preparations. Artificial soil produced with Basalt has a more uniform morphology, likely due to the limited reactants available, but still follows the trend of a crystal complex being formed from a mix of translucent crystals and dark inclusions.

[0333] When comparing the soils samples (Both natural and artificial) to the raw Basalt dust, there is a clear change in structure and composition. The Basalt dust, which was obtained from dry sieving and from a water column drop, is largely made up of transparent, glassy like particles with little to no dark inclusions. This suggests that the crystals are being formed due to the chemical process and did not come from the starter material. Further testing would need to be conducted to determine what effect different starting material would have on the final product.

[0334] Example 22 - 0.1 %-10% Growth Testing

[0335] Aim: To determine the minimum percentage of Leonardite relative to Basalt weight required for healthy plant growth.

[0336] Equipment: Mr Fothergill’s Sungold F1 tomato, 20L Bucket, Calcium Hydroxide, Leonardite, Basalt Rock, RO Water, 1000g scale with 0.1 readability, 200w overhead Stirrer Method: 10% Preparation (seeded 1 January 2025) - 1025g of Calcium Hydroxide and 1025g of Leonardite was added to the 20L bucket. Next, 4500mL of RO water was added and mixed using the overhead mixer for 1.5 hours. 10250g of Basalt was slowly poured into the solution and mixed for 1 hour before reducing the pH using 81% Phosphoric acid.

[0337] Approximately 500mL of 81% Phosphoric acid was used and the sample was left overnight. The next day, the pH was tested as pH7.5 so a further 300mL of 85% Phosphoric acid was added causing the sample to test as pH6.1 before leaving overnight to equilibrate. The sample, again, raised to pH7.5 so a further addition of Phosphoric acid, approximately 200mL, was used to reduce the sample further and placed under a dehumidifier to dry the sample. 600g of old supersoil was added to 6000g of sample to create 10% + 10% OM samples.

[0338] Observations: Once the sample settled, a translucent-white, shiny layer was formed on the surface of the excess water suggesting the formation of carbonate compounds. The 10% sample had a consistency similar to pea soup whilst wet.

[0339] Once the first ‘dry’ cycle was finished, A lighter layer formed approximately 1 / 3 of the way down. Once broken up and further dried, no increase in the white section occurred. Once dried, large particles were not found and the small particles of Basalt found were easily crushed into fine dust. Further investigation needed to determine whether the process is causing Basalt to dissolve or simply break apart.

[0340] Discussion: The reduction in particle size, change in colour and microscopy analysis suggests the formation of a new crystal complex formed from a mix of gold, white and black crystals.

[0341] Method: 1 % Sample (seeded 1 February 2025) - 50g of Calcium Hydroxide and 50g of Leonardite was added to a 10L bucket. 2000mL of RO water was then added and mixed using the overhead mixer for 15 minutes. Next, 5000g of Basalt was slowly poured into the solution and mixed for 15 minutes using a large stick. The pH was reduced using 81% Phosphoric acid until pH6.3 was achieved. Approximately 24mL of 81% Phosphoric acid was used before the sample was placed under a dehumidifier to dry the sample. Once dried, 25g of old super soil was added to 2500g of sample to form 1% + 1 % OM samples. Method: 0.1 % Sample (seeded 6 February 2025) - 4.3g of Calcium Hydroxide and 4.3g of Leonardite was added to a 10L bucket before being hand mixed. Next, 4276.5g of Basalt was added to the bucket and the ingredients were dry mixed by hand to disperse the Leonardite and Calcium Hydroxide mixture equally prior to wetting. The sample was wet with RO water using a hand pump until the sample was uniformly wet. Finally, the sample pH was then reduced to pH6.6 using a mixture of Lemon juice and Bio-down by BioBizz. The sample was left to equilibrate for 30 minutes before further use. 1672g of the 0.1 % sample was mixed with 1.7g of old Supersoil to make 0.1% + 0.1% OM samples. The 0.1% sample was added to three plastic 800mL cups.

[0342] Each soil preparation was used twice with the second preparation including microbes. 2 controls samples were prepared using old super soil.

[0343] 3 seeds were placed into each one and the strongest was kept with the others removed during the first transplant to minimise root damage as per below.

[0344] No fertiliser of any kind was used, and all plants were strictly watered using RO water only to ensure all nutrients were coming from the substrate and / or microbes.

[0345] Samples:

[0346] Started 1 January 2025 - 27 April 2025...

[0347] 1. Control 1

[0348] 2. Control 2

[0349] 3. 10% Plain

[0350] 4. 10% with microbes

[0351] 5. 10% + 10% plain

[0352] 6. 10% + 10% with microbes

[0353] Started 1 February 2025- 27 April 2025...

[0354] 1) Control 1

[0355] 2) Control 2

[0356] 3) 1 % Plain

[0357] 4) 1 % with microbes

[0358] 5) 1 % + 1% plain

[0359] 6) 1 % + 1% with microbes

[0360] Started 6 February 2025 (1 Seed per Cup) - Ongoing... I. 0.1 % Plain

[0361] II. 0.1 % with microbes

[0362] III. 0.1 % + 0.1 % plain

[0363] IV. 0.1 % + 0.1 % with microbes - Did not germinate

[0364] Results: Control samples grew well throughout the growth test. At Wk 10 / 11 , the 10%+10%OM with bacteria had the best growth characteristics. At the end of the experiment, Wk 16 / 17, the control SuperSoil samples performed the best. Substrate comprising of Leonardite and Calcium Hydroxide reacted with Basalt was not sufficient for long term healthy growth in the pot sizes used. Samples with additional organic matter showed significant improvements. Microbes and fungi provide significant improvements across all metrics. Insufficient light significantly impacted plant health.

[0365] Discussion: For the first 3 months, the artificial soil preparations with organic matter were clearly providing a healthier plant with faster growth. After the second month, the growing tent became overcrowded with significant issues with light penetration, and this started to impact the results. After reducing the plant density to just those involved in this experiment, the plants that were previously being shaded started to show signs of recovery. By month 4, the control samples in the Supersoil were clearly producing better plants. Based on the physical changes shown by the plants, it suggests that the nitrogen content was not sufficient for long-term growth of heavy consuming plants. It should be noted that no azo species were used, which may have yielded significantly better results. The Bacteria and mycorrhizal samples typically showed between 20-50% improvement vs the non-impregnated samples. However, by month 5 the non-impregnated samples produced larger plants as can be seen in the results. This may suggest a lack of sufficient sugars and carbohydrates in the soil to maintain the feed and / or direct competition with the plant due to insufficient available food.

[0366] It is interesting to note that the 1%-only samples performed better than the 10% only samples (Plain), investigation would be required to identify the underlying reason. Note - Watering issues were noted throughout, both excessive dry and excessive wet period for all plants. The samples with additional organic matter, in the form of old super soil, performed significantly better than the plain samples. The 0.1% sample have successfully grown however they have significantly stunted growth when compared to the 1 % and 10% samples. The fourth sample did not germinate due to an obvious layer of extremely fine substrate layering the top of the preparation (Due to the end of the substrate preparation being dumped on it) This layer created a highly impermeable barrier and the water did not penetrate the surface without physical mixing and creating a funnel through the layer. The seed was either impacted by the physical mixing or due to waterlogging.

[0367] This experiment was designed to test the lower limits for successful growth of a high consumption plant, in this case the tomato plant. Whilst the 0.1 % sample has grown successfully, the clearly stunted growth and signs of nutrient deficiency, especially phosphorous, suggest this would not be the ideal application rate for raw crushed rock and that 1 % application would be sufficient to reach flowering stage. However, the 10% + 10% with Bacteria and mycorrhizal achieved the best results.

[0368] It should be noted that the species of tomato plant used was ‘Mr Fothergill’s Sungold F1 tomato’ plants which are an indeterminate species. As per online recommendations, these should be grown in a minimum of 30cm diameter pot (Approx 22L), preferably 60cm diameter pot (100L). The maximum size pot of the 10% was in 4L, the 1 % was in a 2L pot.

[0369] The results could be improved by using a wider variety of input materials such as Rock Phosphate, Dolomite and Granite to give a different chemical balance. Whilst the data was clearly affected by the overcrowding issue, the overall results are promising showing that even a 0.1 % application could theoretically be enough to grow plants if supplemented with additional fertiliser.

[0370] Six excess plants from the 10% preparation were placed in a small 600mL food container with the remainder of the 10% substrate preparation. The sample showed significant root growth, and all plants grew relatively well but showed significant stretching and lack of nitrogen.

[0371] Further tests should be performed to determine the optimum percentage and additional input required for long-term healthy growth.

[0372] Summary of Examples 15 to 22

[0373] Summary: The experiments shown below suggest that both Basalt and Bentonite are reacting with the Calcium Hydroxide and Leonardite to form new, unique products that are comparable to each other and natural soil. Whilst the neutralisation step improves flocculation and changes the resultant product, the main reaction with Basalt appears to be during the high pH phase. Movement is necessary for the reaction to occur and the drying phase forms stable complexes. Carbon Dioxide in the atmosphere reacts with free cations within the solution to form carbonate compounds. Artificial soil prepared with Basalt can be used to successfully grow high-consumption species such as Tomato plants. As Basalt, a Silicate-based rock, is able to react with Calcium Hydroxide and Leonardite to form new products (which are very different to those formed prior to Basalt addition) suggests that Silicate compounds are involved in the reaction. The reduction in weight in conjunction with the different particle distribution suggests the Basalt is actively reacting and reducing in overall size. As Bentonite is a phyllosilicate compound, which is a sub-category of Silicates, they share a similar chemical structure and the same functional groups available for reaction. Almost identical particles have been found in Bentonite and Basalt preparations with all pH neutralised samples displaying a similar sheen and hue not seen in other samples.

[0374] 20-40% Experiments (Example 15): Increasing concentration of the Calcium Humate I Fulvate solution reduces the amount of energy required to crush Basalt. 20% solution required significantly more force than 30% and 40% solution to crush into a fine paste. The 20% was darkest in colour but had the largest quantity of Basalt remaining. The 30% was lighter in colour with a smaller quantity of Basalt remaining compared to the 20% but larger particle size. The 40% had very small particles of Basalt remaining with the vast majority of product forming a uniform, smooth chocolate brown solid. The final product has high levels of clay-like material that retains water for long periods of time, even when exposed to open air.

[0375] Basalt Comparisons (Example 16): Surface deposition is not pH dependent. Each reactant and step within the chemical reaction produces unique products with distinct characteristics that are easily identifiable. Shows clear evidence of product deposition on the surface of processed Basalt. Plain Basalt is dark in colour with crystal protrusions and brightly coloured phenocrysts. The crystal protrusions are noticeably transparent with little to no inclusions. High pH samples (Post washing) show clear evidence of crystal deposition, displaying a brown or white colour with inclusions. Low pH samples show increased levels of deposition with the crystals becoming a darker brown colour and with more regular dark inclusions. ‘White’ rocks found in the Basalt samples are largely a cream-beige colour with intermittent patches of dark inclusions.

[0376] Post-reaction at high pH the ‘white’ rocks have clearly reduced in size and show an increase in the quantity of dark inclusions suggesting they were formed during the reaction and not from the starter materials.

[0377] Post-neutralisation with phosphoric acid produces a much more diverse mix of particles. A few of the particles seem largely unaffected, however the majority are different in colour and composition. The resulting products are clearly darker with a more yellow-beige base colouration with patches of more orange or an off-purple colour. Some also appear like glass. All particles show clear evidence of large amounts of dark inclusions suggesting that they have been formed due to the chemical process.

[0378] Unreacted Basalt dust (<1mm) is a mix of transparent, white, coloured and dark crystals. Most of the Basalt particles have large amounts of transparent or white crystals protruding from the surface. Whilst there are some particles displaying dark inclusions, vast majority are transparent crystals without any inclusions. There are some coloured crystals, which are uniform in colour without any inclusions.

[0379] Reacted Basalt Dust (High pH) displays brown-coloured crystals with dark inclusions as a lattice structure. There are clear signs of new crystal formation which are yellow, white or orange coloured. High magnification shows that the crystals are coagulating to form new crystal complexed with regular dark inclusions of various colours.

[0380] Reacted Basalt Dust (Low pH) forms a largely uniform product comprising of golden- brown crystals intermixed with regular dark inclusions. This suggests a regular crystal complex is being formed post neutralisation.

[0381] All evidence collected suggests unique products are being formed depending on the reactants and at each stage throughout the process.

[0382] Basalt Weight and Surface Effects (Example 17) - Basalt post-processes are visually different from each other. Plain washed Basalt, Basalt only samples, Calcium Hydroxide sample, Acid wash samples and the hand-swirled sample all had Basalt that is light grey with large obvious sections of white. All other samples, which reacted with Leonardite, became noticeably darker with fewer white phenocrysts. 3- day samples are brown in colour whilst the 1 -week samples become very dark brown with few white phenocrysts.

[0383] Demonstrates that the Calcium Hydroxide and Leonardite combination provides a lubricating effect to the Basalt during the mixing phase, reducing the amount of energy required for mixing and allowing for a much lower RPM.

[0384] Shows that Calcium Hydroxide alone does not have a large impact on Basalt and does not show significant levels of deposition. Where deposition has occurred, it is clearly Calcium Hydroxide.

[0385] Shows that the paddle mixer creates a higher quantity of particles below 2mm suggesting a grinding action.

[0386] Shows clear differences between Leonardite and Calcium Hydroxide samples when compared to samples that did not include such ingredients. Washed, Acid Soaked and Calcium Hydroxide only samples were a light grey colour with large white phenocrysts. Samples with Leonardite and Calcium Hydroxide included became light or dark brown with samples longer in solution producing much darker Basalt (3- days vs 1-week)

[0387] All samples mixed using the overhead mixer showed a reduction in overall weight. 3-8% reduction for samples reacted with both Calcium Hydroxide and Leonardite at 75RPM and 120RPM. 6-14% reduction in overall weight for plain samples mixed between 90-200RM

[0388] Acid soak samples (1 minute and 2 hours) reduced the overall weight by 1.5% and 3.1 % respectively. The Magnetic Stirrer and Hand swirled samples showed an increase in overall weight by 1 % and 2% respectively. The hand swirled sample remained a very light colour with noticeable white phenocrysts whilst the magnetic stirrer sample was significantly darker without as many white phenocrysts suggesting movement of the reactants is necessary for higher rates of reaction.

[0389] Basalt Particle Size Distribution (Example 18) - Concentration, total time in aqueous phase, time of active mixing and method of mixing all affect the final particle distribution. Movement of the reactants is essential for the reduction of Basalt particle size to occur sufficiently. Non-movement causes deposition and aggregation of smaller particles. Movement and time affect the final particle distribution with higher RPM and longer reaction times showing more significant particle reduction. Time is also a factor even when the same amount of active mixing was used suggesting the rest periods were still causing a reaction.

[0390] The particle distribution is affected by both the high pH and neutralisation step. Samples mixed using the overhead mixer suggest the neutralisation step has the largest impact on particle reduction whereas the magnetic stirrer and hand-swirled samples suggest that the high pH phase is where the particle size reduction is occurring. This may also be due to the magnetic stirrer and hand-swirl samples being sealed from the atmosphere whereas the overhead mixer samples were exposed during active mixing and only sealed during the rest periods. It may be that the formation of carbonate compounds was reducing the reduction rate or was skewing the data of the high pH phase which was then eliminated in the neutralisation step.

[0391] Samples reacted with both Calcium Hydroxide and Leonardite showed significant increases in 2-4mm compared to non-Leonardite samples, especially notable due to the significantly slower RPM used for samples with both Leonardite and Calcium Hydroxide as reactants (75RPM for Sample with Leonardite vs 120RPM for plain Basalt and RO water). The different final distributions formed suggest different mechanisms causing the particle size reduction and a reduction in the energy required to reduce the Basalt.

[0392] Bentonite vs Basalt Dust Comparison (Example 19) - Both Bentonite (a Phyllosilicate clay) and Basalt (Silicate compounds) are reacting with the Calcium Humate I Fulvate solution to form new products. The resultant products are similar in composition and morphology across all preparations when compared.

[0393] When comparing the macro-samples, the Bentonite and Basalt dust formed relatively uniform clay-like compounds with characteristic cracking resulting from the drying step. The Basalt rock sample is considerably darker and is lumpier suggesting a different structure.

[0394] Demonstrates that similar products are produced by Bentonite, Basalt dust and washed Basalt rocks post-pH reduction suggesting a common chemical pathway interacting with both Phyllosilicates and other Silicate-based compounds. The particles show clear evidence of forming larger crystal lattices with regular dark inclusions. Whilst there are differences between Bentonite and Basalt preparations, comparable particles were found in all samples suggesting similar chemical pathways. There is a clear difference between unreacted Bentonite I Basalt vs reacted, low pH samples.

[0395] Following the Chemical Route (Example 20) - It is clear that the process is forming unique products dependent on the reactants used and pH. New crystals and crystal complexes with different colouration and regular dark inclusions are formed which are not usually seen in the raw materials.

[0396] Demonstrates clear physical changes throughout the various steps and are visually very different to the starting materials. Calcium Hydroxide and Leonardite will only react with sufficient movement and form an off-purple-coloured solution with obvious dark particles suspended throughout. After the addition of Basalt, the solution becomes a very dark brown colour.

[0397] Calcium Hydroxide is a white solid when dry and a largely transparent circular compound when viewed in aqueous under the microscope. Calcium Humate solution is comprised of opaque white crystals interspersed between translucent-transparent particles with coloured and dark inclusions. There is clear evidence of unreacted Leonardite and carbonate formation. Some large particles have formed that are clearly products of the reaction due to the high concentration of dark inclusions not seen in unreacted material.

[0398] When the Calcium Humate / Fulvate solution is neutralised with Phosphoric acid, the reaction produces pale yellow crystal complexes with regular dark inclusion of various shades and colour. Drying the sample produces a darker product with more white particles forming on the exposed surfaces (carbonates). On some occasions the dried Calcium Humate I Fulvate solution has a reddish hue. Addition of Basalt produced a very different product which is darker and more uniform in the distribution of dark inclusion at high pH. The colour is closer to a yellow beige. The particles formed are very different to those formed without Basalt. Higher magnification shows yellow particles with coloured and dark inclusions.

[0399] Post-neutralisation with Phosphoric acid produces a variety of particles with different colours and morphology. The product’s clay layer takes on a golden-brown colour with regular dark inclusions whilst the larger particles have a golden-yellow-brown colouration. Some particles are uniform in colour but still display inclusions (Green, Yellow, Orange, Red, Purple). When comparing the samples that used Bentonite instead of Basalt, similar crystals are found across both samples suggesting the same reaction pathways are occurring

[0400] Artificial vs Natural Soil Comparison (Example 21) - The artificial soil preparations show similar particle formations to those found in natural samples with the majority of particles being comprised on multiple small crystals intermixed with darker inclusions. Some natural samples have very little dark inclusions suggesting lower levels of organic matter. Note - The red soil in Malta is known fortheir low carbonate and high iron-based silicate compound content. Pale and white soils are carbonate rich.

[0401] The natural samples taken from various site around Malta typically have a distinctive red hue but a largely formed of crystals with dark inclusions. Excluding the colour, the particles produced throughout the process display similar morphology and characteristics.

[0402] Similar crystals were found in all low-pH samples irrespective of using aggregate or clay. The crystals found were comparable to some crystals found in natural soil. The Bentonite samples with additional organic matter are more comparable to the natural samples indicating that the variety of available ions and reactant material will affect the end products chemical composition.

[0403] Growth T esting (Example 22) - The products formed by reacting Basalt with Calcium Hydroxide, Leonardite and Phosphoric acid are sufficient for plant growth, even at a 0.1 % (w / w) concentration.

[0404] This demonstrates that the artificial soil comprised of just Basalt, Leonardite, Calcium Hydroxide and Phosphoric acid can be used to grow plants. The results show that even just a 0.1% (w / w) Calcium Hydroxide and Leonardite mix is sufficient to grow plants. This test demonstrates that the addition of organic matter, bacteria and fungi can provide better results than ‘supersoil’ at a 10% concentration. With a more complex recipe, it will be possible to create a fertile soil sufficient for long term growth. The results show that the process is producing plant available nutrients from the raw materials although quantity is yet to be determined. Due to the small pots used, overcrowding and insufficient light, further testing would be required to determine the true suitability for long-term plant health.

[0405] Example 23 - Theoretical Chemical Pathway Calcium Hydroxide (aq) in water form Calcium 2+ ions and 2 x OH- ions. Some of the Hydroxide ions are likely neutralised by the deprotonation of the Humic substances and later Silicate minerals (e.g. Aluminosilicate, Phyllosilicates etc.) but not enough to affect the pH. Following weathering pathways for Feldspars suggest that they may react to form Kaolinite or some other clay mineral.

[0406] The Humic substance’s Hydroxyl groups are deprotonated under alkaline conditions. This causes the macro-structure of the Leonardite to breakdown thereby allowing the Humic acid and Fulvic acid to be released and become reactive. Calcium then bonds to the free Oxygen sites from the aforementioned Hydroxyl groups creating Calcium Humate I Fulvate. These crystals then start to arrange themselves into a larger crystal complex likely reflecting the different charges. When watching the Calcium-Humate dry at high pH, the solution appears as a relatively uniform composition in the aqueous state and then appears to separate into light and dark crystals later. This could be due to the CO2 from the air reacting with the Water and Hydroxide ions to form Carbonate compounds. These appear to have a much higher reflectance and white colour making them more visible against the darker Calcium- Humate I Fulvates. It may also be caused by the chelation of the Calcium-Humates I Fulvates into larger complexes.

[0407] The clay species (Phyllosilicates) are layers of tetrahedral Silica sheets, with 2:1 Phyllosilicates also containing octahedral Alumina sheets, with exposed Hydroxyl groups on the outside and edges in the form of Silanol and Aluminol. Under alkaline pH conditions, deprotonation of the Hydroxyl, Silanol and Aluminol groups occur. These are then able to bond with Calcium in the Calcium Humate I Fulvate molecule. The same process appears to occur on other Silicate-based minerals.

[0408] When using crushed aggregate rocks, the exposed mineral crystals (Biotite I Feldspar etc.) within the crushed primary rock species are also able to become a reactant. Most constituent parts of a rock species are various forms of Silicate-based compounds. The primary Silicate compounds found in rock are Quartz and Feldspars. Following weathering pathways for Feldspars suggest that they may react to form Kaolinite or some other clay mineral. This is likely due to Hydroxy attack. Where metal oxides are present, the likely reaction pathways are Calcium replacing weaker cations or dissociative pressures from the extreme pH. Constant movement is required due to the Calcium-Humate I Fulvate’s ability to form crystal complexes. Without sufficient movement, these crystals will start to form a barrier layer around the sand and silt particles therefore reducing the potential for further layers of the rock to be exposed to Hydroxide and Calcium ions. As more protons and cations are released into the aqueous solution, these further reduce the Hydroxide potential, bond with the free oxygen sites while others will be incorporated into the new product mineral crystals giving a distinctive colour change. The newly released cations may also form different crystal compounds altogether, distinct from the bulk product. Due to the different charges within the product crystals, they bond together and form larger silt I sand sized particles even in a high pH state. The same process also affects clays, e.g. Bentonite, Kaolinite etc., with increased surface area reducing the reaction time required. Hydrated crystals may also form and interaction with CO2 will form carbonate compounds.

[0409] During the neutralisation step, the aqueous Hydroxide ions will bond with the protons released from the acid forming Water. The conjugate base will then react with the free cations forming new salts such as, but not limited to, Calcium Phosphate. The remaining Calcium ions, and other free cations, will aid the flocculation of the product crystals into larger complex particles. Free cations may also interact with Carbon Dioxide, if present, to form carbonate compounds.

[0410] When the final product is dehydrated, the particles are brought into closer proximity and bond together, either through ionic or hydrogen bonding, to form a continuous mass with similar strength to a dense mud clod. This can be broken into smaller pieces, sieved and crushed to form a very fine dust or left in a larger size. When rewetted, unless there is sufficient pressure, the macro-structure will remain intact.

[0411] When broken into constituent crystals, there are clearly Humic and I or Iron-based substances entrapped in the product crystals. The crystals display distinctive colour changes throughout the process. The post-neutralisation samples show high uniformity, typically comprising gold / brown / yellow-coloured crystals intermixed with regular dark inclusions, suggesting a stable complex is being formed. This is likely caused by the respective charges of the constituent compounds. It is likely that Calcium Humate and Calcium Fulvate crystals are forming larger complexes and then being entrapped within the larger crystals during formation.

Claims

CLAIMS1 . A composition comprising:(i) a silicate compound,(ii) one (or more) humate(s) and / or fulvate(s), and(iii) one or more divalent metal ions.

2. A composition according to claim 1 wherein the silicate compound is from a natural source, such as natural rock, or is naturally occurring.

3. A composition according to claim 1 or 2, wherein the silicate compound is selected from clay and basalt, or a combination thereof.

4. A composition according to any of claims 1 to 3 wherein (at least part (i) and part (ii) of) the composition is chemically (e.g. ionically) bonded.

5. A composition according to any of claims 1 to 4 wherein the silicate compound (e.g. clay) comprises, or is a type of, phyllosilicate and / or aluminosilicate and / or tetrasilicate, preferably wherein it comprises, or is a type of, phyllosilicate.

6. A composition according to claim 5 wherein the phyllosilicate and / or aluminosilicate and / or tetrasilicate comprises bentonite, kaolinite, mica, smectite, vermiculite and / or chlorite, preferably bentonite.

7. A composition according to any of claims 1 to 6 wherein the divalent metal ions are used to chemically (e.g. ionically) bond the silicate compound to the one or more humates and / or fulvates.

8. A composition according to any of claims 1 to 7 wherein the divalent metal ions comprise zinc, zirconium, iron, scandium, yttrium and / or lanthanum.

9. A composition according to any of claims 1 to 8 wherein the divalent metal ions comprise alkaline earth metal ions, such as calcium.

10. A composition according to claim 9 wherein the one or more humates and / or fulvates comprise alkaline earth metal humates and / or fulvates.

11. A composition according to claim 10 wherein the composition comprises one or both of:(a) calcium humate and / or calcium fulvate, and(b) magnesium humate and / or magnesium fulvate.

12. A composition according to any of claims 1 to 11 wherein the composition further comprises water.

13. A composition according to any of claims 1 to 12 wherein the composition further comprises rock, preferably wherein the rock comprises one or more minerals, such as basalt (if not already present) and / or granite (e.g. basalt and granite in a ratio from between 0.1 :1 and 1 :0.1).

14. A composition according to any of claims 1 to 13 wherein the composition further comprises one or more of: organic matter, fauna, and microorganisms.

15. A composition according to any of claims 1 to 14 wherein the composition: is fertile, and / or does not disperse (or is insoluble) in water.

16. An artificial soil comprising a composition of any of claims 1 to 15.

17. A method of making a composition according to any of claims 1 to 15 or an artificial soil according to claim 16 wherein the method comprises:(a) extracting one or more humates and / or fulvates from a natural source, and(b) combining the one or more humates and / or fulvates with a silicate compound.

18. A method according to claim 17, wherein the silicate compound is derived from or comprises crushed aggregate and / or rock.

19. A method according to claim 17 or 18, wherein the one or more humates and / or fulvates are chemically (e.g ionically) bonded to the silicate compound in step(b), optionally using divalent metal ions.

20. A method according to any of claims 17 to 19 wherein the one or more humates and / or fulvates are extracted by an exothermic reaction, such as an acidbase reaction (e.g. alkali extraction).21 . A method according to claim 20 wherein the acid-base reaction takes place between one or more humic acids and / or fulvic acids present in the natural source and one or more alkaline earth metal compounds.

22. A method according to claim 21 wherein the one or more alkaline earth metal compounds have a pH > 7.

23. A method according to any of claims 20 to 22 wherein the acid-base reaction takes place in the presence of water.

24. A method according to any of claims 17 to 23 wherein the natural source is leonardite or compost.

25. A method according to any of claims 17 to 24 wherein the method further comprises, after steps (a) and (b) one or more of steps:(c) reducing the pH by reacting with an acid (optionally, wherein the pH is reduced to less than 7),(d) adding rock,(e) adding organic matter,(f) adding fauna, and(g) adding microorganisms.

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