EP2203067A1 - Zusammensetzungen und verfahren unter verwendung kohlenstoffhaltiger substanzen - Google Patents

Zusammensetzungen und verfahren unter verwendung kohlenstoffhaltiger substanzen

Info

Publication number
EP2203067A1
EP2203067A1 EP09818485A EP09818485A EP2203067A1 EP 2203067 A1 EP2203067 A1 EP 2203067A1 EP 09818485 A EP09818485 A EP 09818485A EP 09818485 A EP09818485 A EP 09818485A EP 2203067 A1 EP2203067 A1 EP 2203067A1
Authority
EP
European Patent Office
Prior art keywords
composition
carbon
combination
carbonates
bicarbonates
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP09818485A
Other languages
English (en)
French (fr)
Other versions
EP2203067A4 (de
Inventor
Brent R. Constantz
James R. O'neil
Sidney Omelon
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fortera Corp
Original Assignee
Calera Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from PCT/US2008/088318 external-priority patent/WO2009086460A1/en
Priority claimed from PCT/US2009/045722 external-priority patent/WO2009146436A1/en
Priority claimed from PCT/US2009/047711 external-priority patent/WO2009155378A1/en
Priority claimed from PCT/US2009/050223 external-priority patent/WO2010006242A1/en
Priority claimed from PCT/US2009/056573 external-priority patent/WO2010030826A1/en
Application filed by Calera Corp filed Critical Calera Corp
Publication of EP2203067A1 publication Critical patent/EP2203067A1/de
Publication of EP2203067A4 publication Critical patent/EP2203067A4/de
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/10—Lime cements or magnesium oxide cements
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00482—Coating or impregnation materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00732—Uses not provided for elsewhere in C04B2111/00 for soil stabilisation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0075—Uses not provided for elsewhere in C04B2111/00 for road construction
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/52—Sound-insulating materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
    • Y02P40/18—Carbon capture and storage [CCS]

Definitions

  • Entity A small business concern.
  • Relative isotope composition values can be used m a variety of ways to verify the origins of materials m a composition
  • Other substances withm the composition may also be used to verify the origin of the material
  • Such techniques are useful in, e g , confirming that a given composition contains substances sequestered from a particular source, e g , fossil fuels, and such compositions may have a premium value
  • the invention provides a composition that includes carbonates, bicarbonates, or a combination thereof, wherein the carbon in the composition has a relative carbon isotope composition (6 13 C) value less than -26 10 %o
  • the invention provides a composition in which the composition is a synthetic composition
  • the invention provides a composition m which the carbonates, bicarbonate, or combination of carbonates and bicarbonates make up at least 50% of the composition
  • the invention provides a composition m which the composition has a mass of greater than 100 kg
  • the invention provides a composition m which the CO 2 content of the composition is at least 10%
  • the invention provides a composition m which the composition has a negative carbon footprint
  • the invention provides a composition that further includes boron, sulfur, or nitrogen m which the relative isotopic composition of the boron, sulfur, or nitrogen is indicative of a fossil fuel origin
  • the invention provides for a composition m
  • the invention provides a composition m which the calcium to magnesium (Ca/Mg) molar ratio is between 12/1 to 1/15 In some embodiments, the invention provides a composition m which the calcium to magnesium (Ca/Mg) molar ratio is between 5/1 to 1/10 In some embodiments, the invention provides a composition that further includes SOx or a derivative of SOx In some embodiments, the invention provides a composition m which the composition includes a SOx derivative and m which the SOx derivative is a sulfite, a sulfate, or a combination thereof In some embodiments, the invention provides a composition that further includes a metal In some embodiments, the invention provides a composition that includes a metal m which the metal includes lead, arsenic, mercury, or cadmium, or a combination thereof [0004] In some embodiments, the invention provides a building material that includes carbonates, bicarbonates, or a combination thereof,
  • the invention provides a building material m which the component that includes carbonates, bicarbonates, or combination thereof further includes SOx or a derivative thereof In some embodiments, the invention provides a building material in which the component that includes carbonates, bicarbonates, or combination thereof and includes SOx or a derivative thereof includes a sulfate, a sulfite ,or a combination thereof as a derivative of SOx. In some embodiments, the invention provides a building material in which the component comprising carbonates, bicarbonates, or combination thereof further includes a metal In some embodiments, the invention provides a building material that includes a metal in which the metal includes lead, arsenic, mercury or cadmium of combinations thereof.
  • the invention provides a flowable composition that includes carbonates, bicarbonates or a combination of carbonates and bicarbonates, in which the carbon in the carbonates, bicarbonates or combination of carbonates and bicarbonates has a relative carbon isotope composition ( ⁇ 13 C) value less than -5.00 %o, and the viscosity of the composition is between 1 and 2000 cP.
  • the invention provides a flowable composition m which the viscosity if between 10 and 1000 cP.
  • the invention provides a flowable composition m which the composition is a synthetic composition.
  • the invention provides a flowable composition in which the carbonates, bicarbonates, or combination thereof make up at least 10% w/w of the composition. In some embodiments, the invention provides a flowable composition in which the CO 2 content of the composition of at least 10%. In some embodiments, the invention provides a flowable composition in which the composition has a negative carbon footprint. In some embodiments, the invention provides a flowable composition that further includes boron, sulfur, or nitrogen in which the relative isotopic composition of the boron, sulfur, or nitrogen is indicative of a fossil fuel origin In some embodiments, the invention provides a flowable composition m which the carbonates, bicarbonates, or combination thereof include calcium, magnesium or a combination thereof.
  • the invention provides a flowable composition m which the calcium to magnesium (Ca/Mg) molar ratio is between 1/200 and 200/1. In some embodiments, the invention provides a flowable composition m which the calcium to magnesium (Ca/Mg) molar ratio is between 12/1 to 1/15 In some embodiments, the invention provides a flowable composition in which the calcium to magnesium (Ca/Mg) molar ratio is between 5/1 to 1/10 In some embodiments, the invention provides a flowable composition that further includes SOx or a derivative thereof.
  • the invention provides a flowable composition that further includes a metal
  • the invention provides a flowable composition that includes a metal in which the metal includes lead, arsenic, mercury, or cadmium of a combination thereof.
  • the invention provides a synthetic composition that includes carbonates, bicarbonates, or a combination of carbonates and bicarbonates, in which the carbon in the composition has a relative carbon isotope composition (5 13 C) value less than -5 00 %o and the composition is carbon negative.
  • the invention provides a synthetic composition m which the carbonates, bicarbonates, or combination thereof make up at least 50% of the composition.
  • the invention provides a synthetic composition m which the composition has a mass of greater than 100kg In some embodiments, the invention provides a synthetic composition in which the CO 2 content of the composition is at least 10%. In some embodiments, the invention provides a synthetic composition that further includes boron, sulfur, or nitrogen m which the relative isotopic composition of the boron, sulfur or nitrogen is indicative of a fossil fuel origin. In some embodiments, the invention provides a synthetic composition m which the carbonate, bicarbonates, or combination thereof include calcium, magnesium or a combination thereof. In some embodiments, the invention provides a synthetic composition in which the calcium to magnesium (Ca/Mg) molar ratio is between 1/200 and 200/1.
  • Ca/Mg calcium to magnesium
  • the invention provides a synthetic composition m which the calcium to magnesium (Ca/Mg) molar ratio is between 12/1 to 1/15 In some embodiments, the invention provides a synthetic composition in which the calcium to magnesium (Ca/Mg) molar ratio is between 5/1 to 1/10 In some embodiments, the invention provides a synthetic composition that further includes SOx or a derivative thereof. In some embodiments, the invention provides a synthetic composition that further includes a metal. In some embodiments, the invention provides a synthetic composition that further includes a metal m which the metal includes lead, arsenic, mercury, or cadmium or a combination thereof.
  • the invention provides a method of characterizing a synthetic composition that includes determining a relative carbon isotope composition ( ⁇ 13 C) value for the composition. In some embodiments, the invention provides a method of characterizing a synthetic composition in which the composition is a building material, or a material for underground storage In some embodiments, the invention provides a method of characterizing a synthetic composition m which the composition is a cementitious composition, or an aggregate. In some embodiments, the invention provides a method of characterizing a synthetic composition in which the composition is a composition for storage of CO2.
  • the invention provides a method of characterizing a synthetic composition that further includes determining the stability of the composition for release of CO 2 In some embodiments, the invention provides a method of characterizing a synthetic composition that further includes measuring the carbon content for the composition. In some embodiments, the invention provides a method of characterizing a synthetic composition that further includes comparing the ⁇ 13 C value of the composition to another ⁇ 13 C value In some embodiments, the invention provides a method of characterizing a synthetic composition that further includes comparing the ⁇ C value of the composition to another ⁇ C value, in which the other ⁇ 13 C value is a reference ⁇ 13 C value.
  • the invention provides a method of characterizing a synthetic composition that further includes comparing the ⁇ 13 C value of the composition to another ⁇ 13 C value, in which the other ⁇ 13 C value is a value for a possible raw material for the composition. In some embodiments, the invention provides a method of characterizing a synthetic composition that further includes comparing the ⁇ 13 C value of the composition to another ⁇ 13 C value, in which the other ⁇ 13 C value is a value for a fossil fuel, a flue gas derived from the fossil fuel, a water source, or a combination thereof.
  • the invention provides a method of characterizing a synthetic composition that further includes determining whether the composition includes sequestered CO2 from a fossil fuel source based on the comparison of the ⁇ 13 C value of the composition to a reference ⁇ 13 C value. In some embodiments, the invention provides a method of characterizing a synthetic composition that further includes quantifying the amount of carbon dioxide sequestered m the composition.
  • the invention provides a method of fingerprinting a composition that includes determining the values for stable isotopes of a plurality of elements, or the values for the ratios of stable isotopes of a plurality of elements m the composition to determine an isotopic fingerprint for the composition, in which the composition includes carbonates, bicarbonates, or a combination of carbonates and bicarbonates.
  • the invention provides a method of fingerprinting a composition in which the stable isotopes include isotopes of carbon, sulfur, nitrogen or boron or combinations thereof.
  • the invention provides a method of fingerprinting a composition in which the composition is a building material or a material for underground storage
  • the invention provides a method of fingerprinting a composition m which the composition is a composition for storing compounds of elements of at least two of the isotopes so determined.
  • the invention provides a method of fingerprinting a composition that further includes comparing at least two of the values for stable isotopes or at least two of the values for the ratios of stable isotopes, or a combination thereof
  • trie invention provides a method of fingerprinting a composition that further includes determining the probable source of one or more components of the composition based on the isotopic fingerprint of the material
  • the invention provides a method of determining whether or not a composition contains an element sequestered from a fossil fuel source, the method includes determining an isotopic value or ratio of isotopic values for the element, comparing the determined value with a reference isotopic value or ratio of isotopic values, and determining whether the composition contains an element sequestered from a fossil fuel source.
  • the invention provides a method of determining whether or not a composition contains an element sequestered from a fossil fuel source in which the element is carbon, sulfur, nitrogen, or boron
  • the invention provides a method of determining whether or not a composition contains an element sequestered from a fossil fuel source m which the element is carbon and the comparison is a ⁇ 13 C value [0010]
  • a synthetic composition with a neutral or negative carbon footprint comprising carbonates or bicarbonates or a combination thereof, where the carbon m the composition has a relative carbon isotope composition ( ⁇ 13 C) value of -5 00
  • a synthetic composition comprising carbonates or bicarbonates or a combination thereof, where the carbon in the composition has a relative carbon isotope composition ( ⁇ 13 C) value of -22 00 %o or less.
  • such compositions have neutral or negative carbon footprints
  • the carbonates and/or bicarbonates comprise carbonates and/or bicarbonates of beryllium, magnesium, calcium, strontium, barium or radium or combinations thereof
  • the carbonates and/or bicarbonates comprise carbonates and/or bicarbonates of calcium or magnesium or combinations thereof
  • the composition contains calcium and magnesium and the calcium to magnesium (Ca/Mg) molar ratio is between 1/200 and 200/1
  • the calcium to magnesium (Ca/Mg) molar ratio is between 12/1 to 1/15
  • the calcium to magnesium (Ca/Mg) molar ratio is between 5/1 to 1/10
  • a building material comprising a component comprising carbonates or bicarbonates or a combination thereof where the carbon in the carbonates and/or bicarbonates has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o
  • the component comprising carbonates and/or bicarbonates m the building material constitutes at least 5% of the building material
  • the building material is a cementitious material
  • the building material is a mortar, a pozzolamc material, or a supplementary cementitious material or combinations thereof
  • the building material is cement or concrete
  • the building material is non- cementitious
  • the building material is aggregate
  • the aggregate is coarse aggregate
  • the aggregate is fine aggregate
  • the aggregate is reactive aggregate
  • the aggregate is non-reactive or inert aggregate
  • the aggregate is formed or cast aggregate
  • the building material is a roadway material
  • a non-buildmg material comprising a component comprising carbonates or bicarbonates or a combination thereof where the carbon in the carbonates and/or bicarbonates has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o
  • the component comprising carbonates and/or bicarbonates m the non-buildmg material are carbon-neutral or carbon-negative
  • the component comprising carbonates and/or bicarbonates m the non-buildmg material constitutes more than 5% of the building material
  • the non-buildmg material is a household or commercial ceramic product, a paper product, a polymeric product, a lubricant, an adhesive, a rubber product, a chalk, a paint, a personal care product, a cleaning product, a personal hygiene product, a cosmetic, an mgestible product, a liquid mgestible product, a solid mgestible product, an animal mgestible product, an agricultural product, a soil amendment
  • a synthetic composition comprising carbonates or bicarbonates or a combination thereof where the carbon in the composition has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o and the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, and rainfall of normal pH, for at least 1 year
  • the composition has a neutral or negative carbon footprint
  • the composition is a solid precipitate
  • the carbonates and/or bicarbonates comprise carbonates and/or bicarbonates of beryllium, magnesium, calcium, strontium, barium or radium or combinations thereof
  • the carbonates and/or bicarbonates comprise carbonates and/or bicarbonates of calcium or magnesium or combinations thereof
  • the composition contains calcium and magnesium and the calcium to magnesium (Ca/Mg) molar ratio is between 1/200 and 200/1 In some embodiments, the calcium to magnesium (Ca/Mg) molar ratio is between 12/1 to 1
  • a non-buildmg material comprising a component comprising a synthetic composition comprising carbonates or bicarbonates or a combination thereof where the carbon m the composition has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o and the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, and rainfall of normal pH, for at least 1 year
  • the carbonates and/or bicarbonates in the non-bmldmg material are carbon-neutral or carbon-negative
  • at least 5% of the non-buildmg material has a relative carbon isotope composition (6 13 C) value less than -5 00 %o and the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, and rainfall of normal pH, for at least 1 year
  • a synthetic composition including, but not limited to, magnesium carbonate and/or bicarbonate where the carbon m the composition has a relative carbon isotope composition ( ⁇ 13 C) value less than - 5 00 %o and the composition includes, but is not limited to, the mineral phases: magnesite, nesquehonite, hydromagnesite, huntite, magnesium calcite, dolomite, protodolomite or disordered dolomite or combinations thereof.
  • the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, and rainfall of normal pH, for at least 1 year.
  • a synthetic composition including, but not limited to, magnesium carbonate and/or bicarbonate where the carbon m the composition has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o and the composition is in the hydration state of 1,2,3,4,5, or 6 waters of hydration or combinations thereof.
  • the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, and rainfall of normal pH, for at least 1 year.
  • a synthetic composition comprising calcium carbonate or bicarbonate or any combination thereof where the carbon m the composition has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o and the composition includes, but is not limited to, the mineral phases amorphous calcium carbonate, calcite, aragonite, or vaterite or combinations thereof.
  • the composition does not release more than 1% of its total CO2 when exposed to normal conditions of temperature and moisture, and rainfall of normal pH, for at least 1 year.
  • a synthetic composition comprising calcium carbonate or bicarbonate or any combination thereof where the carbon m the composition has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o and the composition is in the hydration state of 1,2,3, or 4 waters of hydration or combinations thereof.
  • the composition does not release more than 1% of its total CO2 when exposed to normal conditions of temperature and moisture, and rainfall of normal pH, for at least 1 year.
  • the product has a neutral or negative carbon footprint
  • the synthetic composition is a building material or a material for underground storage
  • the synthetic composition is a cementitious composition or an aggregate
  • the synthetic composition is a composition for storage of CO 2
  • the method includes the step of determining the stability of the composition for release of CO 2
  • the methods includes the step of determining the carbon content of the composition
  • the method includes the step of comparing the 6 13 C value of the composition to another ⁇ 13 C value, m some cases the other ⁇ 13 C value is a standard ⁇ 13 C values, in other cases a ⁇ 13 C value for a possible raw material for producing the composition
  • the other ⁇ 13 C value used for comparison is that of a raw material that could be a fossil fuel, flue gas derived from the fossil fuel, a water source or a combination thereof
  • 6 13 C value of the composition is a building material or a material for underground storage
  • the synthetic composition is a cementitious composition or an aggregate
  • the synthetic composition is a composition for storage of CO 2
  • the method includes the step of determining the
  • a method of determining whether or not a composition contains an element sequestered from a fossil fuel source comprising determining an isotopic value or a ratio of isotopic values for the element
  • the element is carbon, sulfur, nitrogen or boron
  • the method further comprises the step of comparing the isotopic value or ratio of isotopic values to a standard value
  • the element is carbon and the comparison is a ⁇ 13 C value
  • Figure 1 provides an exemplary carbon sequestration process.
  • Figure 2 provides a diagram of the method of preparing samples for analysis with bench-top instrumentation used to obtain 6 13 C values.
  • Figure 3 provides a diagram of the production of precipitate material from carbon dioxide containing gas and brucite tailings on the laboratory scale. Indicated in the diagram are the materials (gas, liquid, and solid) that were characterized
  • Figure 4 provides a diagram of the production of precipitate material from carbon dioxide containing gas and brucite tailings on a large scale in a 250,000 gallon tank Indicated in the diagram are the materials (gas, liquid, and solid) that were characterized.
  • Figure 5 provides a diagram of the production of precipitate material from carbon dioxide containing gas and brucite tailings in a continuous process. Indicated in the diagram are the materials (gas, liquid, and solid) that were characterized
  • Figure 6 provides a diagram of the production of precipitate material from carbon dioxide containing gas and fly ash m a laboratory scale process. Indicated m the diagram are the materials (gas, liquid, and solid) that were characterized.
  • Figure 7 provides a comparison of 813 C data from literature, the source of the carbon dioxide containing gas, the industrial waste, precipitate, and supernate from a laboratory scale process using brucite tailings as the industrial waste.
  • Figure 8 provides a comparison of 613 C data from literature, the source of the carbon dioxide containing gas, the industrial waste, precipitate, and supernate from a large scale process using brucite tailings as the industrial waste
  • Figure 9 provides a comparison of 613 C data from literature, the source of the carbon dioxide containing gas, the industrial waste, precipitate, and supernate from a continuous process using brucite tailings as the industrial waste
  • Figure 10 provides a comparison of 813 C data from literature, the source of the carbon dioxide containing gas, the industrial waste, precipitate, and supernate from a laboratory scale process using fly ash as the industrial waste
  • the invention provides compositions containing elements with certain relative element isotope composition value or values, and methods for determining the content of compositions in terms of the relative element isotopic value or values.
  • the invention provides compositions, e.g., synthetic compositions containing carbon with a negative relative carbon isotope composition ( ⁇ 13 C) value, and methods for analyzing carbon in a composition to determine ⁇ 13 C values, e.g., to verify that some or all of the carbon in the composition is from a carbon sequestration process.
  • compositions and methods find use m applications where it is desired to use materials that are the product of sequestration of substances whose release into the environment is undesirable, such as carbon dioxide, sulfur oxides, nitrogen oxides, heavy metals, and other substances produced m, e.g., the burning of fossil fuels, and verifying the source of carbon and the like m such materials
  • compositions In further describing the subject of the invention, methods used to measure isotopic ratio values, e g , ⁇ 13 C values and element content, e g , carbon content, m compositions will be presented Methods of tracking or verifying the origin of, e g , carbon, in a composition will also be described Then compositions contaimng elements with certain isotopic ratios, e g , ⁇ 13 C values, will be described
  • the invention provides methods of characterizing a composition by determining its relative isotope composition ratio value
  • various isotopes may be used, all of which have isotopic ratios that may be compared with standard ratios — e g , carbon, oxygen, sulfur, boron, and nitrogen — the following description focuses primarily on carbon, and the relative carbon isotopic ratio, or ⁇ 13 C value
  • the elemental content, e g , carbon content of the composition is determined as well
  • the methods further include verifying that the composition contains carbon from CO 2 that is from a particular source, e g , a fossil fuel source, such as by comparing the value determined for carbon content and relative carbon isotope composition ratio with a standard value, a raw material value, or the like
  • the composition may be a composition m which carbon, e g , carbon dioxide, from
  • the methods include measuring the isotopic value, such as the relative isotope ratio value, for a plurality of elements, e g , two or more of carbon, sulfur, nitrogen, oxygen, and boron, making it possible to isotopically "fingerprint" a particular composition
  • the methods of the invention are useful, e g , to verify that some or substantially all of the carbon and, in some cases, other elements, m a composition originated in a fossil fuel Stable isotopes and isotope fractionation
  • the relative carbon isotope composition (6 13 C) value with units of %o (per mil) is a measure of the ratio of the concentration of two stable isotopes of carbon, namely 12 C and 13 C, relative to a standard of fossilized belemnite
  • C is preferentially taken up by plants during photosynthesis and m other biological processes that use inorganic carbon because of its lower mass
  • the lower mass of 12 C allows for kmetically limited reactions to proceed more efficiently than with 13 C
  • materials that are derived from plant material, e g , fossil fuels have relative carbon isotope composition values that are less than those derived from inorganic sources
  • the carbon dioxide m flue gas produced from burning fossil fuels reflects the relative carbon isotope composition values of the organic material that was fossilized
  • Table 1 lists relative carbon isotope composition value ranges for relevant carbon sources for comparison
  • Material incorporating carbon from burning fossil fuels reflects ⁇ 13 C values that are more like those of plant derived material, i e less, than that which incorporates carbon from atmospheric or non-plant marine sources Verification that the material produced by a carbon dioxide sequestering process is composed of carbon from burning fossil fuels can include measuring the ⁇ 13 C value of the resultant material and confirming that it is not similar to the values for atmospheric carbon dioxide, nor marine sources of carbon
  • the invention provides a method of characterizing a composition comprising measuring its relative carbon isotope composition ( ⁇ 13 C) value.
  • the composition is a composition that contains carbonates, e g., magnesium and/or calcium carbonates. Any suitable method may be used for measuring the ⁇ 13 C value, such as mass spectrometry or off-axis integrated-cavity output spectroscopy (off- axis ICOS)
  • One difference between the carbon isotopes is in their mass. Any mass-discerning technique sensitive enough to measure the amounts of carbon can be used to find ratios of the 13 C to 12 C isotope concentrations. Mass spectrometry is commonly used to find 6 13 C values Commercially available are bench-top off-axis mtegrated- cavity output spectroscopy (off-axis ICOS) instruments that are able to determine 6 13 C values as well. These values are obtained by the differences in the energies in the carbon-oxygen double bonds made by the 12 C and 13 C isotopes in carbon dioxide.
  • off-axis ICOS bench-top off-axis mtegrated- cavity output spectroscopy
  • the ⁇ 13 C value of a carbonate precipitate from a carbon sequestration process serves as a fingerprint for a CO 2 gas source, as the value will vary from source to source, but in most carbon sequestration cases ⁇ 13 C will generally be m a range of -9%o to -35%o.
  • the methods include the measurement of the amount of carbon in the composition. Any suitable technique for the measurement of carbon may be used, such as coulometry. Carbon measurements may be used in some cases to quantitate the amount of carbon dioxide sequestered in a composition. Isotope measurements may be used to verify that the source of the carbon m a composition is what it is claimed to be.
  • a further feature of some embodiments of the invention includes comparing the ⁇ 13 C value for the composition with another ⁇ 13 C value; this other ⁇ 13 C value may be a standard value, a value for a possible raw material in the composition (e.g., coal, oil, natural gas, or flue gas), or any other value that gives useful information for the comparison
  • the ⁇ 13 C value for the composition is compared to a fixed value or range of values, such as a value between -l%o and -50%o, or between -5%o and -4O%o or between -5%o and -35%o, or between -7%o and -4O%o or between -7%o and -35%oor between -9%oand -4O%o or between -9%o and -35%o, or a comparison to a value that is -3%o, -5%o, -6%o, -7%o, -8%o, -9%o, -10°/oo, -1 l
  • a value less than any of the values given herein such as a value less than -7%o, or a value less than -l ⁇ %o, or a value less than -15%o, or a value less than -2O%o, or a value less than - 25%o, or a value less than -3O%o, or a value less than -35%o, a value less than -4O%o.
  • the ⁇ 13 C value for the composition is compared to a value for a possible raw material of the composition
  • the ⁇ 13 C value for the composition may be compared to a ⁇ 13 C value, or a range of ⁇ 13 C values, for a fossil fuel, such as a natural gas, an oil, a coal or a particular type of coal, or such as a flue gas produced from burning a natural gas, an oil, a coal or a particular type of coal
  • a fossil fuel such as a natural gas, an oil, a coal or a particular type of coal
  • a flue gas produced from burning a natural gas, an oil, a coal or a particular type of coal This can be particularly useful in verifying that the composition contains CO 2 from the fossil fuel and/or from the burning of the fossil fuel
  • the ⁇ 13 C value for a coal is -34%o and the ⁇ 13 C value for a composition that is claimed to have sequestered CO 2 from the burning of the coal is equal to or within a certain range of -3
  • Some embodiments further involve quantifying the amount of CO 2 sequestered from a source of CO 2 , e g. a fossil fuel source, in a composition
  • a source of CO 2 e g. a fossil fuel source
  • coulometry may be used to determine the relative amount of carbon in a composition
  • isotopic ratio values may be used to verify that the carbon is wholly or partially of fossil fuel origin It is then a simple calculation to determine the amount of CO 2 (or carbon) sequestered in the composition, given the relative amount of the carbon that is of fossil fuel origin and the total carbon.
  • Other embodiments of the invention include determining isotopic values or isotopic ratios compared to a standard that are similar to 5 13 C values, for elements other than carbon, or in addition to carbon, in a composition
  • Such elements include, but are not limited to, oxygen, nitrogen, sulfur, and boron
  • the isotopic value for any such element, or combination of elements may be measured by techniques similar to those used for carbon.
  • Such techniques and methods of expressing isotopic ratios in comparison with a standard are well-known m the art, e.g , 8 11 B values for boron and ⁇ 34 S values for sulfur.
  • the invention provides methods of isotopically fingerprinting a composition by determining a plurality of isotopic values or isotopic ratio values, or a combination thereof, for the composition. In some embodiments, the quantity of the element or its compounds in the composition is also determined.
  • one or more of the isotopic components of the isotopic fingerprint is used m combination with quantitation of the element/compound represented by the isotope to determine the total amount of the element/compound m the composition that is of a particular origin, e.g., that is of fossil fuel origin
  • isotopic ratios may be altered during combustion and other processing of a fossil fuel (e.g-, for boron and/or sulfur), and these alterations may be taken into account in some embodiments to further refine the verification and/or quantification analysis.
  • the isotopic values or isotopic ratio values, or a combination thereof are determined for two or more of carbon, sulfur, oxygen, nitrogen, and boron.
  • an isotopic fingerprint for carbon and sulfur is determined, e.g., a 5 13 C values for carbon and ⁇ 34 S value for sulfur.
  • an isotopic fingerprint for carbon and boron is determined, e.g., a ⁇ 13 C values for carbon and O 11 B value for boron.
  • an isotopic fingerprint for carbon, sulfur, and boron is determined, e.g., a ⁇ 13 C values for carbon, ⁇ 34 S value for sulfur, and O 11 B value for boron.
  • the isotopic fingerprint may be used to verify the source of the elements m the composition, e.g , in a protocol to verify that the composition contains elements of fossil fuel origin. This is useful because many of the elements, e.g. carbon and sulfur or their oxides or other compounds, are subject to regulation, such as cap and trade systems or other regulatory systems, m various parts of the world.
  • the techniques of the invention may be used, e g , in such a system, to verify and/or quantitate capture of the elements and/or their compounds
  • This verification and/or quantitation can be used to confirm compliance with regulations, to calculate credits or penalties for sequestration of the elements or compounds, e.g., carbon dioxide, sulfur oxides, nitrogen oxides, and any other element or compound subject to regulation for which isotopic measurements may be performed, and for any other suitable use as will be apparent to those of skill m the art.
  • the total amount of carbon dioxide gas coming out of a process is shown to be less than the total amount of carbon dioxide gas entering the process; in addition the origin of the carbon dioxide m the exiting gas may be shown to be the same as that of the gas entering the process and/or a product of the process is show to have sequestered the CO 2 from the gas.
  • Fingerprinting a material correlates the carbon, and/or other elements, contained in the material to a source by measuring and comparing the ratios of stable isotopes of carbon and/or other elements, such as nitrogen and sulfur As users of materials seek to obtain carbon credits when using materials, this method will be useful to prove carbon dioxide sequestration and show a material to be carbon negative.
  • FIG. 1 Shown in figure 1 is a carbon dioxide sequestration process that has three possible sources of carbon. They are: the gas stream that contains CO 2 [100], the air above the solution where the sequestration process takes place [105], and the water or solution [110] of the shown sequestration process, e.g. sea water, brine, or other ionic solution
  • the amount of carbon m each can be measured.
  • the partial pressure of CO 2 gas is measured, e g. using a commercially available gas probe as is known to those skilled in the art.
  • the flow rate of the CO 2 containing gas is also measured or regulated.
  • Air is a mixture of oxygen (O 2 ), nitrogen (N 2 ), CO 2 , water vapor, ozone, and other gases Similar to what is measured for the incoming CO 2 gas stream, to characterize the air m the system [105], the partial pressure of CO 2 IS measured, e.g. using a commercially available probe, and the volume of air is known based upon the dimensions of the reaction vessel. These values for the air in the system give us the amount of carbon contributed by the air.
  • any suitable method e g coulometry, is used to measure the concentration of carbon in the water [110] Both the inorganic and the organic carbon content can be measured using coulometry by varying the digestion liquid In general, the organic carbon does not participate m the reactions and thus is not included m the accounting of carbon in the sequestration process.
  • the amount of carbon m the gas components is determined using a commercially available probe to determine the partial pressure of carbon dioxide in conjunction with the volume of gas m the system
  • the amount of carbon in the liquid and solid components is measured using coulometry.
  • These materials are also characterized by their 5 13 C values using mass spectrometry or off-axis ICOS.
  • the product's 5 13 C value [130] is compared to the value of the incoming CO 2 gas stream [100], to its fingerprint.
  • a 6 13 C for a product that is close to that of the incoming CO 2 is indicative of the fact that the carbon m the product did not come from the water [110] or air [105]
  • Water and air typically have only mildly negative ⁇ 13 C values, not less than -8%o, to be measured in this method of material and process characterization.
  • Comparing the amount of carbon m the incoming components to the amount of carbon in the components resulting from the sequestration process shows whether or not any carbon is unaccounted for. This mass balance m conjunction with the ⁇ 13 C fingerprinting shows that some portion of the CO 2 leaves the incoming gas stream, is not present in the effluent gas stream, and is incorporated into the product
  • the exemplary process shown in figure 1 is a process [115] during which the CO 2 from the incoming gas dissolves [100] into the solution, reacts with ions in the solution, and forms a material which serves to remove the CO 2 from the incoming gas in a form that may be stored over a long term, or that may be converted to such a form.
  • the process may produce a solution, a precipitated material, or a slurry, so long as the ultimate product is suitable for long-term storage
  • the isotopic content or ratio, e g , ⁇ 13 C value, of any component may be measured at any stage of the process in order to obtain both a quantitative and/or qualitative measure of the fate of the original CO 2 .
  • carbon measurements allow the exact quantitation of the fate of the CO 2 .
  • multiple samples may be obtained, either from a material or over time, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 or more than 10 samples may be obtained and analyzed.
  • CO 2 may enter the process from the gas containing CO 2 (e g , flue gas from fossil fuel burning), from the air m contact with the water into which the gas containing CO 2 is being dissolved [105], and from the water itself [110]
  • the ⁇ 13 C value for one, two, or all of these may be measured, and the concentration of CO 2 , and flow rate, of each may also be measured
  • Similar measurements may be made of the effluent gas [120], the air m contact with the drying product of the precipitation step and/or the liquid effluent [125], the product (e g , a solid material contaimng carbonates or a liquid slurry of carbonates and/or bicarbonates) [130], and the liquid effluent [135]
  • Any additional sources or sinks for CO 2 may be similarly tested and accounted
  • the invention provides methods of verifying the source of a composition by determining a ⁇ 13 C value for the composition and an isotopic composition value for one or more of sulfur, boron, or nitrogen
  • isotopic values or combinations of values may be used alone, or the amounts of each element, and/or ratios thereof, may be used (e g , the ratio of carbon to boron, or carbon to sulfur, or sulfur to boron,
  • Other substances that are optionally sequestered m the precipitated composition, or in the solution include one or more of sulfur oxides (SO x , e g , SO 2 and SO 3 ), nitrogen oxides (NO x , e g , NO or NO 2 ), heavy metals such as mercury, radioactive substances, and volatile organic compounds
  • SO x sulfur oxides
  • NO x nitrogen oxides
  • NO or NO 2 nitrogen oxides
  • heavy metals such as mercury
  • radioactive substances such as mercury
  • volatile organic compounds such as mercury
  • the invention include methods of analyzing a sample that include determining a ⁇ 13 C value for the sample and determining a value for one or more of the content of SO x or a derivative thereof, such as a sufate or a sulfite, e
  • the invention includes methods of analyzing a sample that include determining a 6 13 C value for the sample, determining a similar isotopic ratio value for one or more of boron, sulfur, or nitrogen, and determining a value for one or more of the content of SO x or a derivative thereof, such as a sufate or a sulfite, e g , calcium or magnesium sulfate or sulfite, NO x or a derivative thereof, or mercury or a derivative thereof such as mercuric chloride, and comparing the values to reference values, which may be empirically derived from actual samples of known origin, theoretically derived, or derived in any other suitable manner.
  • the relative carbon isotope composition value of the solution during the process can be monitored using, e g , mass spectrometry or off-axis ICOS
  • concentration of CO 2 dissolved into the solution may be calculated from the total alkalinity measurement.
  • a measure of the total alkalinity of a known volume of solution will allow for the carbon dioxide content to be calculated.
  • Monitoring the CO 2 dissolving into the solution while the process is progressing allows adjustments to be made to create the desired sequestration products and is an optional component of the method.
  • this method is equally applicable to a wide variety of other products including but not limited to combustible fuel, environmental analytes, foods, and paint.
  • any material wherein the stable isotope content of source materials can be compared to that of the products can be characterized by this method.
  • ratios of stable isotopes for oxygen ( 16 O and 18 O), nitrogen ( 14 N and 15 N), sulfur ( 32 S and 34 S), hydrogen ( 1 H and 2 H), and/or boron ( 10 B and 11 B) can also be measured, e.g using mass-spectrometry It can also be appreciated that the amounts of these, and any other suitable element, may be measured using a variety of standard laboratory analytical techniques. These values may be used to trace other components m a product. For example, sulfur from flue gas may be traced in a product m an analogous manner to carbon. Similarly, nitrogen may also be traced.
  • the fingerprint is a value for a ratio of stable isotopes m a product (e.g. ⁇ 13 C value). In other embodiments, a plurality of isotope ratios may be used, e.g. 2,3,4,5,6, or more than 6.
  • a fingerprint for a product comprises a value for a stable carbon isotope or ratio values.
  • a fingerprint for a product comprises a value for a stable sulfur isotope or ratio of values.
  • a fingerprint for a product comprises a value for a stable nitrogen isotope or ratio values.
  • a fingerprint for a product comprises a value for a stable boron isotope or ratio values.
  • a combination of values or ratios of values for stable isotopes for more than one element is used.
  • a combination of concentration values or ratios of concentrations for stable isotopes of carbon and sulfur are provided.
  • a combination of values or ratios of values for stable isotopes for more than one element is used.
  • a combination of concentration values or ratios of concentrations for stable isotopes of carbon and nitrogen are provided in some embodiments, a combination of values or ratios of values for stable isotopes for more than one element is used.
  • a fingerprint for a product comprises a 6 13 C value
  • a fingerprint comprises a 6 13 C value and a ⁇ 34 S value.
  • a fingerprint comprises a ⁇ 13 C value and a ⁇ n B value
  • a fingerprint comprises a 5 13 C value and a ⁇ 15 N value.
  • a fingerprint comprises a ⁇ 13 C value, a ⁇ 34 S value, and a ⁇ 15 N value.
  • a fingerprint comprises a ⁇ 13 C value, a 5 34 S value, and a ⁇ ⁇ B value. In some embodiments, a fingerprint comprises a ⁇ 13 C value, a 6 11 B value, and a ⁇ 15 N value Compositions Containing Carbon
  • the invention provides compositions containing carbon with negative relative carbon isotope composition ( ⁇ 13 C) values, e g , synthetic compositions Such values may be indicative of plant-based origins, e g flue gas from burning fossil fuel, and may be used to ve ⁇ fy that the carbon m the composition comes partially or completely from the burning of fossil fuel
  • Compositions that are likely to contain components from flue gas combustion, e g , CO 2 and optionally other components such as sulfur-, nitrogen-, and/or heavy metal-contammg components, are useful as vehicles to sequester such substances from the environment, and may also have other uses such as m the built environment
  • the composition is a synthetic composition Synthetic compositions provided m some embodiments of the invention are typically formed by any synthetic method that produces a product with carbon with a negative ⁇ 13 C value, however, they may be formed by sequestering CO 2 gas m the synthetic composition, e g, the composition may be formed by precipitating material from an
  • compositions of the invention may be a solid mass
  • the composition may be made up of particulate matter, m which individual particles are relatively small, e g , 0 1-1000 microns average diameter, or m some cases even 1000 microns to several centimeters or more m diameter, or combinations thereof, m which case the composition is considered to be the combined mass of the particles m a single batch, lot, container, or the like
  • Compositions of the invention may also have an average density that falls within a certain range, for example, m some embodiments, a composition of the invention has a bulk density of 50
  • compositions of the invention contain strontium, e g , between 0 001% and 5% w/w/ strontium, or between 0 00001% and 1% w/w strontium, or between 0 001% and 0 1% w/w strontium, or between 0 01% and 5% w/w strontium, or between 0 01% and 1% w/w strontium, or between 0 01% and 0 1% w/w strontium, or between 0 1% and 5% w/w strontium, or between 0 1% and 1% w/w strontium
  • compositions of the invention contain boron, e g , between 0 000001% and 2 0% w/w boron, or between 0 00001% and 1% w/w boron, or between 0 0001% and 0 1% w/w boron, or between 0 001% and 1% w/w/w boron, or between
  • carbon containing compositions e g , synthetic carbon containing compositions are provided where the compositions contain carbon having a negative ⁇ 13 C value as described herein, where at least part of the carbon is in the form of carbonates and/or bicarbonates, e g , carbonates and/or bicarbonates of beryllium, magnesium, calcium, strontium, barium or radium or combinations thereof
  • the molar ratio of carbonates to bicarbonates may be any suitable ratio for the process of producing the composition and/or the intended use of the composition, such as.
  • the carbonate/bicarbonate ratio may be 100/1 to 1/100, or 50/1 to 1/50, o, 25/1 to 1/25, or 10/1 to 1/10, or 5/1 to 1/5, or 2/1 to 1/2, or 100/1 to 1/10, or 100/1 to 1/1, or 50/1 to 1/10, or 50/1 to 1/1 or 25/1 to 1/10, or 25/1 to 1/1 or 10/1 to 1/1, or 1/100 to 10/1, or 1/100 to 1/1, or 1/50
  • Ca/Mg ratio ranges are 2/1 to Vi, 3/2 to 2/3, or 5/4 to 4/5. In some embodiments, Ca/Mg ratio ranges are 1/7 to 200/1, 1/15 to 12/10, 1/10 to 5/1, 1/7 to Vi, or 1/9 to 2/5. In some embodiments, Ca/Mg ratio ranges are 1/200 to 1/7, 1/70 to 1/7, or 1/65 to 1/40. In some embodiments, Ca/Mg ranges are 1/3 to 3/1 or Vi to 2/1 In some embodiments, Ca/Mg ranges are 2/1 to all calcium, 3/1 to 200/1, 5/1 to 200/1, or 10/1 to 200/1.
  • a carbon containing composition In some embodiments, other components besides carbon dioxide or compounds derived from carbon dioxide (e.g. carbonates and/or bicarbonates) are included m a carbon containing composition.
  • the carbon found in the composition originates at least in part from the burning of fossil fuel and the production of a flue gas, e g , in an industrial process, and other components of the fossil fuel may also provide additional components of the carbon containing composition.
  • Exemplary components include the combustion gases, e.g., nitrogen oxides (NO x ); sulfur oxides (SO x ) and sulfides; halides such as hydrogen chloride and hydrogen fluoride, particulates such as flyash, cement kiln dust, other dusts and metals including arsenic, beryllium, boron, cadmium, chromium, chromium VI, cobalt, lead, manganese, mercury, molybdenum, selenium, strontium, thallium, or vanadium; and organics such as hydrocarbons and volatile organic compounds (VOCs), radioactive materials, dioxms and PAH compounds.
  • NO x nitrogen oxides
  • SO x sulfur oxides
  • sulfides e.g., sulfur oxides (SO x ) and sulfides
  • halides such as hydrogen chloride and hydrogen fluoride
  • particulates such as flyash, cement kiln dust, other dusts and metals
  • PAH Polynuclear Aromatic Hydrocarbons
  • nitrogen oxides (NO x ) refers to oxides of nitrogen, e.g., nitric oxide (NO) and nitrogen dioxide (NO 2 )
  • sulfur oxides (SO x ) refers to oxides of sulfur, e.g., sulfur dioxide (SO 2 ) and sulfur t ⁇ oxide (SO 3 ).
  • compositions of the invention may include flyash.
  • compositions of the invention contain flyash m an amount of 0.001% w/w - 10.0%, such as 0.01% w/w - 5.0%w/w, such as 0 1% w/w - 5.0% w/w, such as 1.0% w/w-5.0% w/w, such as 1.0% w/w - 4.0% w/w, such as 1.0% w/w - 3.0% w/w, such as 1.0% w/w - 2 5% w/w, such as 0 l%w/w to 2.5%w/w fly ash.
  • compositions of the invention contain one or more mercury compounds, e g., mercuric chloride and/or other mercuric compounds, in an amount of 0.0000001 - 0.1 % w/w, e.g , 0.000001 - 0.1 % w/w, or 0.00001 - 0.1 %, or 0.0000001 - 0.01 %, or 0.0000001 - 0.001, or % 0.0000001 - 0 001 %, or 0.0000001 - 0.00001 %, or 0.000001 - 0.1, or % 0 000001 - 0.01 %, or 0.000001 - 0.001 %, or 0.000001 - 0.0001 %, or 0.000001 - 0.0001 %, or 0.000001 - 0.00001, or % 0.00001 - 0.01 %, or 0.00001 - 0.001 %, or 0 00001 - 0.0001 w/w.
  • mercury compounds e g.,
  • compositions of the invention contain one or more sulfur compounds, e.g., one or more sulfates, sulfites, or combination of sulfates and sulfites, in an amount of 0 01-30% w/w, e g , 0 01-20% w/w, or 0 01-10% w/w, or 0 01-1% w/w, or 0 1-30% w/w, e.g., 0.1-20% w/w, or 0.1-10% w/w, or 0.1-1%, or 1-30% w/w, e.g , 1-20% w/w, 1-10% w/w, or l-5%w/w.
  • sulfur compounds e.g., one or more sulfates, sulfites, or combination of sulfates and sulfites
  • compositions of the invention contain one or more nitrogen compounds, e.g., derivatives of NOx such as nitrates or nitrites, in an amount of 0 01-30% w/w, e.g., 0.01-20% w/w, or 0 01-10% w/w, or 0.01-1% w/w, or
  • compositions may contain one or more of flyash, mercury compounds, sulfur compounds, or nitrogen compounds, e.g., one or more mercury, sulfur, or nitrogen compounds in the weight percentage ranges given above [0078]
  • the invention provides compositions, such as synthetic compositions, containing carbon with ⁇ 13 C value less than -5%o, or less than -10%o, or less than -15%o, or less than -20%o, or less than - 25%o which also include one or more of the following: SO x , NO x ; metals including: arsenic, beryllium, boron, cadmium, chromium, chromium VI, cobalt, lead,
  • the invention provides for carbon containing compositions, e.g, synthetic carbon containing compositions with ⁇ C values less than -15%o that further comprise NO x or derivatives thereof. In some embodiments, the invention provides for carbon containing compositions, e.g, synthetic carbon containing compositions with 6 13 C values less than -15%o that further comprise VOCs or derivatives thereof. More details regarding the inclusion of by-products of industrial processes are given in patent application US 61/156,809, specifically pages 1-2, 19-24, and 32-39, which is hereby incorporated by reference herein in its entirety
  • the carbon found in the composition originates at least in part from the burning of fossil fuel, e.g , coal, and the production of a flue gas, e.g , in an industrial process, and other components of the fossil fuel may also provide additional components of the synthetic carbon containing composition.
  • fossil fuel e.g , coal
  • flue gas e.g
  • other components of the fossil fuel may also provide additional components of the synthetic carbon containing composition.
  • ratios of stable isotopes for oxygen 16 O and 18 O
  • nitrogen 14 N and 15 N
  • sulfur 32 S and 34 S
  • hydrogen 1 H and 2 H
  • boron 10 B and 11 B
  • compositions comprising carbon ⁇ 13 C values less than -5%o that further comprise boron with a ⁇ ⁇ B value of less than -2%o, less than -5%o, less than -7%o, less than -10%o, less than -12%o, less than -14%o , less than -15%o, less than -17%o ,, less than -2O%o j> less than -22%o n less than -25%o, or less than -30%o, sulfur with a ⁇ S value of less than -5%o , or between 0 and +l ⁇ %o , or combinations thereof.
  • These compositions may further contain one or more of a SO x - derived, NO x -derived, or mercury-derived compound, as described further herein
  • the carbon containing compositions e.g, synthetic carbon- contammg composition includes magnesium carbonates or calcium carbonates or combinations thereof.
  • the carbon-containing composition includes dolomite, a carbonate containing both calcium and magnesium having the chemical formula Ca 05 Mg 05 COs 1 and/or protodolomite (amorphous dolomite with calcium to magnesium ratios deviating from 1: 1).
  • Other embodiments contain CaCO 3 as one or more of the minerals calcite, aragomte, or vaterite or as combinations thereof.
  • Some embodiments have hydrated forms of calcium carbonate including: ikaite (CaCO 3 ⁇ oH 2 O), amorphous calcium carbonate (CaCO 3 « H 2 O) or monohydrocalcite (CaCO 3 ⁇ H 2 O) or combinations thereof.
  • Some embodiments contain magnesium carbonates m various stages of hydration where waters of hydration include 1,2,3,4, or more than 4 waters of hydration or combinations thereof, such as no hydration as magnesite (MgCO 3 ) or ternary hydration as nesquehomte (MgCO 3 « 3H 2 O)
  • Other embodiments include versions of more complex versions of magnesium carbonates that include waters of hydration and hydroxide such as artinite (MgCO 3 'Mg(OH) 2 OH 2 O), dypingite (Mg 5 (CO 3 ) 4 (OH) 2 -5H 2 O), or hydromagnesite (Mg 5 (CO 3 ) 4 (OH) 2 *3H 2 O) or combinations thereof.
  • the invention provides for a carbon containing composition, e g, synthetic carbon containing composition comprising carbonates or bicarbonates or combinations thereof where the carbon in the carbonates or bicarbonates has a ⁇ 13 C value less than -5%o, or less than -l ⁇ %o or less than -15%o or less than - 20%o or less than -25%o or less than-30%o or less than -35%o where the composition does not release more than 1%, or 5%, or 10% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 1, 2, 5, 10, or 20 years, or for more than 20 years, for example, for more than 100 years.
  • a carbon containing composition e g, synthetic carbon containing composition comprising carbonates or bicarbonates or combinations thereof where the carbon in the carbonates or bicarbonates has a ⁇ 13 C value less than -5%o, or less than -l ⁇ %o or less than -15%o or less than - 20%o or less than -2
  • the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 1 year. In some embodiments the composition does not release more than 5% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 1 year. In some embodiments the composition does not release more than 10% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 1 year. In some embodiments the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 10 years.
  • the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 100 years. In some embodiments the composition does not release more than 1% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 1000 years.
  • any suitable surrogate marker or test that is reasonably able to predict such stability may be used; e.g , conditions of elevated temperature or pH conditions that are reasonably likely to indicate stability over an extended period in an accelerated test may be used
  • a sample of the composition may be exposed to 50, 75, 90, 100, 120, or 150 0 C for 1, 2, 5, 25, 50, 100, 200, or 500 days at between 10% and 50% relative humidity, and a loss less than 1%, 2%, 3%, 4%, 5%, 10%, 20%, 30%, or 50% of its carbon may be considered sufficient evidence of stability for a given period, e g., for 1, 10, 100, 1000, or more than 1000 years.
  • CO 2 content of the material may be monitored by any suitable method, e g., coulometry.
  • Other conditions may be adjusted as appropriate, including pH, pressure, UV radiation, and the like, again depending on the intended or likely environment It will be appreciated that any suitable conditions may be used that one of skill in the art would reasonably conclude indicate the requisite stability over the indicated time period.
  • any suitable conditions may be used that one of skill in the art would reasonably conclude indicate the requisite stability over the indicated time period.
  • any suitable conditions may be used that one of skill in the art would reasonably conclude indicate the requisite stability over the indicated time period.
  • some carbonate compounds that may be part of a composition of the invention, e g. in a given polymorphic form may be well- known geologically and known to have withstood normal weather for decades, centuries, or even millennia, without appreciable breakdown, and so have the requisite stability.
  • the invention provides for a building material contaimng a component comprising carbonates or bicarbonates or combinations thereof where the carbon in the carbonates and/or bicarbonates has a ⁇ 13 C value less than -5%o, e.g., less than -10%o, such as less than -15%o and in some embodiments less than - 20%o.
  • a "building material,” as that term is used herein, includes any material that is or may be used for a construction purpose, for example, but not limited to, work and home habitats, industrial structures and transportation-related structures such as roads, parking lots and parking structures, as well as environmental structures such as dams, levees, and the like
  • the building material further contains SO x ; NO x ; metals including: arsenic, beryllium, boron, cadmium, chromium, chromium VI, cobalt, lead, manganese, mercury, molybdenum, selenium, strontium, thallium, or vanadium; VOCs; particulates such as fly ash; or radioactive compounds or derivatives thereof, or combinations thereof, as described above.
  • the building material does not release more than 1%, or 5%, or 10% of its total CO 2 when exposed to normal conditions of temperature and moisture, including rainfall of normal pH, for its intended use, for at least 1, 2, 5, 10, or 20 years, or for more than 20 years, for example, for more than 100 years, also as described above.
  • the invention provides for an aggregate, for example, a synthetic aggregate containing a component comprising carbonates or bicarbonates or combinations thereof where the carbon in the carbonates or bicarbonates has a 5 13 C value less than -5%o, e.g., less than -10%o such as less than -15%o and in some embodiments less than -20%o.
  • the aggregate of the invention is a fine aggregate, a coarse aggregate, reactive aggregate, inert or non-reactive aggregate, or a formed or cast aggregate.
  • Reactive aggregate is aggregate which undergoes a chemical reaction such that it bonds to the surrounding material when hydrated.
  • Some embodiments provide for a cement or concrete contaimng a component comprising carbonates or bicarbonates or combinations thereof where the carbon in the carbonates or bicarbonates has a ⁇ 13 C value less than -5%o, e.g., less than -10%o such as less than -15%o and in some embodiments less than -20%o.
  • the invention provides for other cementitious building material such as: mortar, a pozzolanic material, or a supplementary cementitious material or combinations thereof containing a component comprising carbonates or bicarbonates or combinations thereof where the carbon in the carbonates or bicarbonates has a ⁇ 13 C value less than -5%o, e.g., less than -10%o such as less than -15%o and in some embodiments less than -20%o.
  • the invention provides for non- cementitious building material such as.
  • a soil stabilization composition or insulation or combinations thereof containing a component comprising carbonates or bicarbonates or combinations thereof where the carbon in the carbonates or bicarbonates has a 6 13 C value less than -5%o, e.g., less than -10%o such as less than -15%o and in some embodiments less than -20%o.
  • the roadway material may be an asphalt or a paving material
  • the roadway material may be an asphalt or a paving material
  • Some embodiments of the invention provide for non-building materials containing components that include carbonates or bicarbonates or combinations thereof where the carbon m the carbonates and/or bicarbonates has a ⁇ 13 C value less than -5%o, e.g., less than -10%o such as less than -15%o and in some embodiments less than - 20%o.
  • the non-building material includes, a household or commercial ceramic product; a paper product; a polymeric product; a lubricant; an adhesive; a rubber product; a chalk; a paint; a personal care product, a cosmetic, an ingestible product, an agricultural product, or an environmental remediation product.
  • the invention provides for a personal care product that includes a cleaning product or a personal hygiene product
  • the invention provides for an ingestible product that includes a liquid, a solid, or an animal ingestible product containing components that include carbonates or bicarbonates or combinations thereof where the carbon m the carbonates and/or bicarbonates has a 5 13 C value less than -5%o, e.g., less than -10%o such as less than -15%o and in some embodiments less than -2O%o
  • Some embodiments of the invention provide for an agricultural product that includes a soil amendment product or a pesticide containing components that include carbonates or bicarbonates or combinations thereof where the carbon in the carbonates and/or bicarbonates has a ⁇ 13 C value less than -5%o, e.g., less than -10%o such as less than -15%o and in some embodiments less than -2O%o
  • Some embodiments of the invention provide for an environmental remediation product that includes a forest soil restoration product or a product
  • the invention provides for a paint containing components comprised of carbonates or bicarbonates or combinations thereof where the carbon in the carbonates and/or bicarbonates has a ⁇ C value less than -5%o.
  • Building materials of the invention may also have an average hardness that falls within a certain ranges, such as in some embodiments a building material of the invention has an average hardness between 1 and 7 on the Mohs scale of hardness In some embodiments, a building material of the invention has an average hardness of at least 3 on the Mohs scale of hardness In some embodiments, a building material of the invention has an average hardness of at least 4 on the Mohs scale of hardness.
  • a building material of the invention has an average hardness of at least 5 on the Mohs scale of hardness. In some embodiments, a building material of the invention has an average hardness between 1 and 6 on the Mohs scale of hardness, such as between 1 and 5, such as between 2 and 5, such as between 1 and 4, such as between 2 and 6, such as between 2 and 4 on the Mohs hardness scale.
  • the invention provides flowable compositions.
  • the flowable composition is pseudoplastic (i.e., viscosity of the flowable compositions decreases with increasing shear rate).
  • the flowable composition is thixotropic (i e., viscosity decreases over time under constant shear).
  • viscosity and non-Newtonian behavior increases with increasing concentration of solids.
  • the flowable composition that is a slurry has a viscosity at 20 °C greater than 1 cP
  • a flowable composition has a viscosity between 2000 cP to 1 cP, such as 100 cP to 1000 cP, including 150 cP to 500 cP, for example 200 cP to 400 cP.
  • the flowable composition may have a viscosity of 300 cP to 400 cP such as about 380 cP.
  • viscosity may decrease with increasing shear rate
  • viscosity may decrease over time with constant shear.
  • the flowable composition is a slurry comprising solid precipitates and effluent liquid from a carbon sequestration process.
  • the solid precipitates include, but are not limited to, carbonates, bicarbonates, and any combination of carbonates and bicarbonates.
  • the precipitates will have a negative ⁇ 13 C value.
  • the carbonates, bicarbonates, or any combination of carbonates and bicarbonates included m the precipitates will have a ⁇ 13 C value less than (i.e. more negative than) -5 °/00, such as less than -6°/00, less than -I 0 IQQ, less than -8°/00, less than -9°/00, less than -10°/00, less than -15°/00, less than
  • the flowable composition will include other constituents of the industrial flue gas, such as, but not limited to: carbon monoxide, nitrogen oxides (NOx), sulfur oxides (SOx), sulfides, halides, particulate matter such as fly ash and dusts; metals and metal- containing compounds, radioactive materials, and organics.
  • a flowable composition is placed in a repository.
  • a flowable composition is placed in a subterranean geological formation.
  • the geological formation was not suitable for storing super- critical carbon dioxide
  • the geological formation was the source of a component of a carbon dioxide sequestration process used to form part of the flowable composition.
  • the flowable composition is a pumpable composition.
  • a pumpable composition is one such that it can be transported using conduits and pumps from one location to another.
  • the invention provides a flowable composition comprising carbonates, bicarbonates, or a combination thereof wherein the carbon in the carbonates, bicarbonates, or combination thereof has a relative carbon isotope composition ( ⁇ 13 C) value less than -5 00 %o and the viscosity of the composition is between 1 and 2000 cP, e g , between 10 and 1000 cP
  • the composition is a synthetic composition
  • the carbonates, bicarbonates, or combination thereof make up at least 10% w/w of the composition
  • the CO2 content of the composition is at least 10%
  • the composition has a negative carbon footprint
  • the conmposition further comp ⁇ sies boron, sulfur, or nitrogen wherein the relative isotopic composition of the boron, sulfur, or nitrogen is indicative of a fossil fuel origin
  • the conmposition further comp ⁇ sies boron, sulfur, or nitrogen where
  • compositions of the invention include any suitable method by which a carbon with the requisite of 6 13 C value may be made Such methods are described, e g , m US Published Patent Applications Nos 2009/0020044 and 2009/0001020, and US Patent Application No 12/344,019, the disclosures of which are hereby incorporated by reference m their entirety
  • a divalent cation-contammg water may be exposed to flue gas from an industrial source, e g , from a coal-fired power plant or other source where the flue gas contains CO 2 containing carbon primarily or entirely of fossil fuel origin
  • the divalent cation-contammg water may be, e g , seawater, brme, and/or water that has been enriched m divalent cations Protons are removed from the water by addition of base (e g , a hydroxide such as sodium hydroxide or base from industrial waste, brmes, minerals, or other sources) and/or by electrochemical methods,
  • waste streams may be produced from a va ⁇ ety of different types of industrial plants
  • waste streams for the methods include waste streams produced by industrial plants that combust fossil fuels (e g , coal, oil, natural gas) and anthropogenic fuel products of naturally occurring orgamc fuel deposits (e g , tar sands, heavy oil, oil shale, etc )
  • a waste stream suitable for systems and methods of the invention is sourced from a coal-fired power plant, such as a pulverized coal power plant, a supercritical coal power plant, a mass burn coal power plant, a fluidized bed coal power plant, m
  • the waste stream is sourced from gas or oil-fired boiler and steam turbine power plants, gas or oil-fired boiler simple cycle gas turbine power plants, or gas or oil-fired boiler combined cycle gas turbine power plants
  • Industrial waste gas streams may contain carbon dioxide as the primary non-air derived component, or may, especially m the case of coal- fired power plants, contain additional components such as nitrogen oxides (NOx), sulfur oxides (SOx), and one or more additional gases Additional gases and other components may include CO, mercury and other heavy metals, and dust particles (e g , from calcining and combustion processes) Additional components m the gas stream may also include halides such as hydrogen chloride and hydrogen fluoride, particulate matter such as fly ash, dusts, and metals including arsenic, beryllium, boron, cadmium, chromium, chromium VI, cobalt, lead, manganese, mercury, molybdenum, selenium, strontium, thallium, and vanadium, and organics such as hydrocarbons, dioxms, and PAH compounds Suitable gaseous waste streams that may be treated have, m some embodiments, CO 2 present m amounts of 200 ppm to 1,000,000
  • Flue gas temperature may also vary
  • the temperature of the flue gas comprising CO 2 is from O 0 C to 2000 0 C, such as from 6O 0 C to 700 0 C, and including 100 0 C to 400 0 C
  • one or more additional components or co-products (1 e , products produced from other starting materials [e g , SOx, NOx, etc ] under the same conditions employed to convert CO 2 into bicarbonates and/or carbonates) are precipitated or trapped m precipitation material, or m solution or slurry, formed by contacting the waste gas stream comprising these additional components with an aqueous solution comprising divalent cations (e g , alkaline earth metal ions such as Ca 2+ and Mg 2+ ) Sulfates,
  • divalent cations e g , alkaline earth metal ions such as Ca 2+ and Mg 2+
  • a portion of the gaseous waste stream (1 e , not the entire gaseous waste stream) from an industrial plant may be used to produce solutions, slurries, or precipitation material
  • the portion of the gaseous waste stream that is employed m the process may be 75% or less, such as 60% or less, and including 50% and less of the gaseous waste stream
  • substantially (e g , 80% or more) the entire gaseous waste stream produced by the industrial plant is employed m precipitation of precipitation material, solution, or slurry
  • 80% or more, such as 90% or more, including 95% or more, up to 100% of the gaseous waste stream (e g , flue gas) generated by the source may be employed for precipitation of precipitation material
  • Methods of the invention may remove significant portions, or substantially all, of the CO 2 from a given CO 2 source, e g , over 30%, 40%, 50%, 60%, 70%, 80%, 90%, 95%, 99%, or even over 99
  • Methods of the invention include contacting a volume of an aqueous solution of divalent cations with a source of CO 2 and optionally subjecting the resultant solution to conditions that facilitate precipitation
  • a volume of an aqueous solution of divalent cations is contacted with a source of CO 2 while optionally subjecting the aqueous solution to conditions that facilitate precipitation
  • Divalent cations may come from any of a number of different divalent cation sources depending upon availability at a particular location Such sources include industrial wastes, seawater, brines, hard waters, rocks and minerals (e g , lime, penclase, material comprising metal silicates such as serpentine and olivine), and any other suitable source
  • waste streams from various industrial processes provide for convenient sources of divalent cations (as well as m some cases other materials useful m the process, e g , metal hydroxide)
  • waste streams include, but are not limited to, mining wastes, fossil fuel burning ash (e g , combustion ash such as fly ash, bottom ash, boiler slag), slag (e g iron slag, phosphorous slag), cement kiln waste, oil refinery/petrochemical refinery waste (e g oil field and methane seam brines), coal seam wastes (e g gas production brines and coal seam brme), paper processing waste, water softening waste brine (e g , ion exchange effluent), silicon processing wastes, agricultural waste, metal finishing waste, high pH textile waste, and caustic sludge Fossil fuel burning ash, cement kiln dust, and slag, collectively waste sources of metal oxides, further described m U S Patent
  • the aqueous solution of divalent cations comprises magnesium in amounts ranging from 50 to 40,000 ppm, 50 to 20,000 ppm, 100 to 10,000 ppm, 200 to 10,000 ppm, 500 to 5000 ppm, or 500 to 2500 ppm
  • the ratio of Ca 2+ to Mg 2+ (i e , Ca 2+ .Mg 2+ ) m the aqueous solution of divalent cations is between 1.1 and 1.2 5, 1 2 5 and 1.5, 1 5 and 1.10, 1.10 and 1.25, 1 25 and 1.50, 1.50 and 1.100, 1.100 and 1.150, 1.150 and 1.200, 1 200 and 1.250, 1.250 and 1.500, 1.500 and 1.1000, or a range thereof
  • m some embodiments
  • the aqueous solution of divalent cations may comprise divalent cations derived from freshwater, brackish water, seawater, or brine (e g , naturally occurring brines or anthropogenic brines such as geothermal plant wastewaters, desalination plant waste waters), as well as other salmes having a salinity that is greater than that of freshwater, any of which may be naturally occurring or anthropogenic Brackish water is water that is saltier than freshwater, but not as salty as seawater Brackish water has a salinity ranging from about 0 5 to about 35 ppt (parts per thousand)
  • Seawater is water from a sea, an ocean, or any other salme body of water that has a salinity ranging from about 35 to about 50 ppt Brine is water saturated or nearly saturated with salt Brine has a salinity that is about 50 ppt or greater
  • the water source from which divalent cations are derived is a mineral rich (e g , calcium -
  • any of a number of suitable freshwater sources may be used, including freshwater sources ranging from sources relatively free of minerals to sources relatively ⁇ ch m minerals
  • Mmeral- ⁇ ch freshwater sources may be naturally occurring, including any of a number of hard water sources, lakes, or inland seas
  • Some mineral-rich freshwater sources such as alkaline lakes or inland seas (e g , Lake Van m Turkey) also provide a source of pH- modifying agents
  • Mineral-rich freshwater sources may also be anthropogenic
  • a mmeral-poor (soft) water may be contacted with a source of divalent cations such as alkaline earth metal cations (e g , Ca 2+ , Mg 2+ , etc ) to produce a mineral-rich water that is suitable for methods and systems described herein
  • Divalent cations or precursors thereof e g salts, minerals
  • Naturally occurring proton-removmg agents encompass any proton-removmg agents that can be found m the wider environment that may create or have a basic local environment
  • Some embodiments provide for naturally occurring proton-removmg agents including minerals that create basic environments upon addition to solution Such minerals include, but are not limited to, hme (CaO), pe ⁇ clase (MgO), iron hydroxide minerals (e g , goethite and limomte), and volcanic ash Methods for digestion of such minerals and rocks comprising such minerals are provided herein
  • Some embodiments provide for using naturally alkaline bodies of water as naturally occurring proton-removmg agents
  • Examples of naturally alkaline bodies of water include, but are not limited to surface water sources (e g alkaline lakes such as Mono Lake m California) and ground water sources (e g basic aquifers such as the deep geologic alkaline aquifers located at Searles Lake in California)
  • Other embodiments provide for use of deposits from dried alkaline
  • waste streams from various industrial processes may provide proton-removmg agents
  • waste streams include, but are not limited to, mining wastes, fossil fuel burning ash (e g , combustion ash such as fly ash, bottom ash, boiler slag), slag (e g iron slag, phosphorous slag), cement kiln waste, oil refinery/petrochemical refinery waste (e g oil field and methane seam brmes), coal seam wastes (e g oil field and methane seam brmes), coal seam wastes (e
  • Low- voltage electrochemical methods that do not generate chlorine gas are convenient for use m systems and methods of the invention
  • Low-voltage electrochemical methods to remove protons that do not generate oxygen gas are also convenient for use in systems and methods of the invention.
  • low- voltage electrochemical methods generate hydrogen gas at the cathode and transport it to the anode where the hydrogen gas is converted to protons. Electrochemical methods that do not generate hydrogen gas may also be convenient. In some instances, electrochemical methods to remove protons do not generate any gaseous by-byproduct. Electrochemical methods for effecting proton removal are further described m U S Patent Application No 12/344,019, filed 24 December 2008, U.S. Patent Application No. 12/375,632, filed 23 December 2008;
  • electrochemical methods may be used to produce caustic molecules (e g , hydroxide) through, for example, the chlor-alkali process, or modification thereof.
  • Electrodes i.e., cathodes and anodes
  • Electrodes may be present m the apparatus containing the divalent cation- containing aqueous solution or gaseous waste stream-charged (e.g., CO 2 -charged) solution, and a selective barrier, such as a membrane, may separate the electrodes.
  • Electrochemical systems and methods for removing protons may produce by-products (e.g., hydrogen) that may be harvested and used for other purposes. Additional electrochemical approaches that may be used in systems and methods of the invention include, but are not limited to, those described in U.S Provisional Patent Application No. 61/081,299, filed 16 July 2008, and U S. Provisional Patent Application No.
  • Compositions of the invention include bicarbonate and carbonate compositions that may be produced in solution or slurry or by precipitating a calcium and/or magnesium bicarbonate or carbonate composition from a solution of divalent cations
  • the bicarbonate and/or carbonate compound compositions that make up the components of the invention include metastable carbonate compounds that may be precipitated from a solution of divalent cations, such as a saltwater, as described in greater detail below
  • the bicarbonate and/or carbonate compound compositions of the invention include precipitated crystalline and/or amorphous bicarbonate and carbonate compounds.
  • Saltwater-de ⁇ ved bicarbonate and/or carbonate compound compositions of the invention are ones that are derived from a saltwater As such, they are compositions that are obtained from a saltwater m some manner, e g , by treating a volume of a saltwater in a manner sufficient to produce the desired bicarbonate and/or or carbonate compound composition from the initial volume of saltwater
  • the bicarbonate and/or carbonate compound compositions of certain embodiments are produced by,e g , precipitation from a solution of divalent cations (e g , a saltwater) that includes alkaline earth metal cations, such as calcium and magnesium, etc , where such solutions of divalent cations may be collectively referred to as alkaline earth metal-containmg waters
  • saltwater employed m methods may vary as reviewed above, saltwater of interest include brackish water, seawater and brme, as well as other salines having a salinity that is greater than that of freshwater (which has a salinity of less than 5 ppt dissolved salts)
  • calcium rich waters may be combined with magnesium silicate minerals, such as olivine or serpentine, m solution that has become acidic due to the addition on carbon dioxide to form carbonic acid, which dissolves the magnesium silicate, leading to the formation of calcium magnesium silicate carbonate compounds as mentioned above
  • a volume of water is optionally subjected to bicarbonate/carbonate compound precipitation conditions sufficient to produce a solution of bicarbonate and/or carbonate-containing solution which can then be used to produce precipitation material and a mother liquor (i e , the part of the water that is left over after precipitation of the bicarbonate and/or carbonate compound(s) from the saltwater), if desired
  • the resultant precipitation material and mother liquor may collectively make up the bicarbonate and/or carbonate compound compositions of the invention (e g , as a slurry) or may be separated into precipitate and mother liquor, each or both of which may also be compositions of the invention (e g , solid and solution compositions) Any convenient precipitation conditions may be employed, which conditions result m the production of a barcarbonate/carbonate compound composition
  • conditions that facilitate precipitation i e , precipitation conditions
  • Some naturally occurring minerals such as serpentine, contain hydroxide and may be dissolved to yield a source of hydroxide.
  • the addition of serpentine also releases silica and magnesium into the solution, leading to the formation of silica-contaming precipitation material.
  • the amount of proton-removing agent that is added to the reaction mixture or precursor thereof will depend on the particular nature of the proton-removing agent and the volume of the reaction mixture or precursor thereof being modified, and will be sufficient to raise the pH of the reaction mixture or precursor thereof to the desired pH.
  • the pH of the reaction mixture or precursor thereof may be raised to the desired level by electrochemical means as described above Additional electrochemical methods may be used under certain conditions
  • electrolysis may be employed, wherein the mercury cell process (also called the Castner- Kellner process), the diaphragm cell process, the membrane cell process, or some combination thereof is used
  • byproducts of the hydrolysis product e g., H 2 , sodium metal, etc. may be harvested and employed for other purposes, as desired.
  • the pH-elevating approach described in U S. Provisional Patent Application Nos 61/081,299, filed 16 July 2008, and 61/091,729, filed 25 August 2008 may be employed, the disclosures of which are incorporated herein by reference.
  • Additives other than pH -elevating agents may also be introduced into the water in order to influence the nature of the material that is produced
  • certain embodiments of the methods include providing an additive in water before or during the time when the water is subjected to the precipitation conditions.
  • Certain calcium carbonate polymorphs can be favored by trace amounts of certain additives
  • vaterite a highly unstable polymorph of CaC ⁇ 3, which precipitates m a variety of different morphologies and converts rapidly to calcite, can be obtained at very high yields by including trace amounts of lanthanum as lanthanum chloride m a supersaturated solution of calcium carbonate
  • Other additives beside lanthanum that are of interest include, but are not limited to transition metals and the like.
  • the addition of ferrous or ferric iron is known to favor the formation of disordered dolomite (protodolomite) where it would not form otherwise.
  • the nature of the precipitation material can also be influenced by selection of appropriate major ion ratios.
  • Major ion ratios also have considerable influence of polymorph formation
  • aragonite becomes the favored polymorph of calcium carbonate over low-magnesium calcite.
  • low-magnesium calcite is the preferred polymorph.
  • magnesium: calcium ratios can be employed, including, for example, 100: 1, 50.1, 20:1, 10:1, 5:1, 2.1, 1:1, 1:2, 1.5, 1.10, 1.20, 1.50, 1.100, or any of the ratios mentioned above.
  • the magnesiumxalcium ratio is determined by the source of water employed m the precipitation process (e.g., seawater, brme, brackish water, fresh water), whereas in other embodiments, the magnesiumxalcium ratio is adjusted to fall within a certain range [00121] Rate of precipitation also has a large effect on compound phase formation. The most rapid precipitation can be achieved by seeding the solution with a desired phase.
  • a set of precipitation conditions to produce a desired precipitation material from a solution of divalent cations includes, m certain embodiments, the water's temperature and pH, and in some instances, the concentrations of additives and ionic species m the water.
  • Precipitation conditions may also include factors such as mixing rate, forms of agitation such as ultrasonics, and the presence of seed crystals, catalysts, membranes, or substrates
  • precipitation conditions include supersaturated conditions, temperature, pH, and/or concentration gradients, or cycling or changing any of these parameters
  • the protocols employed to prepare bicarbonate and/or carbonate-containing precipitation material according to the invention may be batch or continuous protocols It will be appreciated that precipitation conditions may be different to produce a given precipitation material m a continuous flow system compared to a batch system
  • the methods further include contacting the volume of water that is subjected to the mineral precipitation conditions with a source of CO2 Contact of the water with the source CO2 may occur before and/or during the time when the water is subjected to CO 2 precipitation conditions Accordingly, embodiments of the invention include methods m which the volume of water is contacted with a source OfCO 2 prior to subjecting the volume of saltwater to mineral precipitation conditions Embodiments of the invention include methods m which the volume of saltwater is contacted with a source of CO 2 while the volume of saltwater is being subjected to bicarbonate and/or carbonate compound precipitation conditions Embodiments of the invention include methods m which the volume of water is contacted with a source of a CO 2 both prior to subjecting the volume of saltwater to bicarbonate and/or carbonate compound precipitation conditions and while the volume of saltwater is being subjected to bicarbonate and/or carbonate compound precipitation conditions In some embodiments, the same water may be cycled more than once, wherein
  • Embodiments may include treatment of the mother liquor, where the mother liquor may or may not be present m the same composition as the product
  • the mother liquor may be contacted with a gaseous source of CO 2 in a manner sufficient to increase the concentration of carbonate ion present in the mother liquor
  • Contact may be conducted using any convenient protocol, such as those described above
  • the mother liquor has an alkaline pH, and contact with the CO 2 source is carried out m a manner sufficient to reduce the pH to a range between 5 and 9, e g , 6 and 8 5, including 7 5 to 8 2
  • the treated brine may be contacted with a source of CO 2 , e g , as described above, to sequester further CO 2
  • the mother liquor may be contacted with a gaseous source of CO 2 in a manner sufficient to increase the concentration of
  • the resultant product is separated from the mother liquor to produce separated product Separation of the product can be achieved using any convenient approach, including a mechanical approach, e g , where bulk excess water is drained from the product, e g , either by gravity alone or with the addition of vacuum, mechanical pressing, by filtering the product from the mother liquor to produce a filtrate, etc
  • Separation of bulk water produces, in certain embodiments, a wet, dewatered precipitation material
  • the dewatered precipitation material is more than 5% water, more than 10% water, more than 20% water, more than 30% water, more than 50% water, more than 60% water, more than 70% water, more than 80% water, more than 90% water, or more than 95% water
  • the resultant dewatered precipitation material may then be dried, as desired, to produce a dried product Drying can be achieved by air drying the wet precipitation material Where the wet precipitation material is air dried, air drying may be at room
  • Example 1 Measurement of S 13 C value for a solid precipitate and starting materials
  • This Example demonstrates precipitation of carbonate material from saline solution using bottled carbon dioxide (CO 2 ) and a magnesium rich industrial waste material and determination of ⁇ 13 C values for materials and product The procedure was conducted in a container open to the atmosphere [00132]
  • the starting materials were commercially available bottled CO 2 gas, seawater, and brucite tailings from a magnesium hydroxide production site as the industrial waste source of base
  • the brucite tailings were approximately 85% Mg(OH) 2 , 12% CaCO 3 and 3% SiO 2 as determined by a Rietveld analysis of the x-ray diffraction pattern of a dry aliquot of the tailings
  • a container was filled with locally available seawater (around Santa Cruz, CA) Brucite tailings were added to the seawater, providing a pH (alkaline) and divalent cation concentration suitable for carbonate precipitation and CO 2 gas was sparged into the alkaline
  • This precipitation was conducted m a 250,000 gallon container
  • the starting materials were commercially available bottled CO 2 gas, seawater (from around Santa Cruz, CA), 50% NaOH solution, and brucite tailings as the industrial waste
  • the brucite tailings were approximately 85% Mg(OH) 2 , 12% CaCO 3 and 3% SiO 2 as determined by a Rietveld analysis of the x-ray diffraction pattern of a dry aliquot of the tailings
  • the 250,000 gallon container was partially filled with locally available seawater
  • the carbon dioxide gas was sparged into the sea water through diffusers located at the bottom of the container After CO 2 sparging, the pH of the sea water reached approximately 5 5
  • Brucite tailings were added to the seawater, providing an increase m magnesium concentration and alkalinity suitable for the precipitation of carbonate solids without releasing CO 2 into the atmosphere
  • the CO 2 gas sparging and brucite tailings addition ceased Sodium hydroxide solution was then added to achieve a pH
  • the powder could also have been stored as it was produced, as a carbon-sequestering storage material.
  • the material could have been left in the supernatant solution and stored, optionally after equilibration with atmospheric air, as a slurry, where both the precipitate and the carbonates and bicarbonates in solution serve as carbon-sequestermg materials
  • Other uses for the material are as described herein, and would be apparent to one of skill in the art
  • the carbonate material was characterized using 6 13 C analysis, x-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM).
  • ⁇ 13 C values for the process starting materials, resulting materials and supernatant solution were measured The 6 13 C value for the atmospheric air was not measured, but a value from literature is given in Table 2.
  • the analysis system used was manufactured by Los Gatos Research as described in Example 1.
  • Measurements from the analysis of the CO 2 source, industrial waste (brucite tailings), carbonate precipitate, and supernatant solution are listed in Table 2 and illustrated in Figure 8.
  • the ⁇ 13 C values for the precipitate and supernatant solution were -30 04%o and -34 16%o, respectively.
  • the precipitated carbonate material was more likely to incorporate calcium carbonate from the brucite tailings than the supernatant solution, so the ⁇ 13 C value of the precipitate reflects that by being less negative than that of the supernatant solution.
  • This Example illustrates that ⁇ 13 C values may be used to confirm the primary source of carbon in a carbonate composition as well as in a solution produced from the carbon dioxide.
  • a container was filled with locally available seawater Brucite tailings were added to the seawater, providing a pH (alkaline) and divalent cation concentration suitable for carbonate precipitation without releasing CO 2 into the atmosphere. Flue gas was sparged at a rate and time suitable to precipitate carbonate material from the alkaline seawater solution Sufficient time was allowed for interaction of the components of the reaction, after which the precipitate material was separated from the remaining seawater solution, also known as the supernatant solution, and spray-dried See Figure 5 The resulting powder was suitable, with further processing, for use, e g , as a material in the built environment, such as aggregate for use m a road bed, concrete, or the like.
  • the powder could also have been stored as it was produced, as a carbon-sequestermg storage material.
  • the material could have been left m the supernatant solution and stored, optionally after equilibration with atmospheric air, as a slurry, where both the precipitate and the carbonates and bicarbonates in solution serve as carbon-sequestering materials
  • CO 2 -sequestering and “carbon-sequestering” are synonymous.
  • Other uses for the material are as described herein, and would be apparent to one of skill m the art.
  • ⁇ 13 C values for the process starting materials, resulting precipitate carbonate material and supernatant solution were measured The ⁇ 13 C value for the atmospheric air was not measured, but a value from literature is given in Table 2 and illustrated in Figure 9
  • the analysis system used was manufactured by Los Gatos Research and uses direct absorption spectroscopy to provide ⁇ 13 C and concentration data for gases ranging from 2% to 20% CO 2 , as detailed m Example 1.
  • Measurements from the analysis of the flue gas, industrial waste (brucite tailings), carbonate precipitate, and supernatant solution are listed in Table 2.
  • the ⁇ 13 C values for the precipitate and supernatant solution were - 19.92%o and -24.8%o, respectively.
  • This Example illustrates that ⁇ 13 C values may be used to confirm the primary source of carbon in a carbonate composition when the CO 2 source for the carbonate is combustion, as well as in a solution produced from the carbon dioxide.
  • Example 4 Measurement of O 13 C value for a solid precipitate and starting materials
  • the starting materials were a commercially available bottled mixture of SO 2 and CO 2 gas (SO 2 /CO 2 gas), de-ionized water, and fly ash as the industrial waste.
  • SO 2 /CO 2 gas SO 2 /CO 2 gas
  • a container was filled with de-ionized water Fly ash was added to the de-ionized water after slaking, providing a pH (alkaline) and divalent cation concentration suitable for carbonate precipitation without releasing CO 2 into the atmosphere.
  • SO 2 /CO 2 gas was sparged at a rate and time suitable to precipitate carbonate material from the alkaline solution. Sufficient time was allowed for interaction of the components of the reaction, after which the precipitate material was separated from the remaining solution, also known as the supernatant solution and spray- dried. See Figure 6.
  • the resulting powder was suitable, with further processing, for use, e.g , as a material in the built environment, e.g., as aggregate for use in a road bed, concrete, or the like.
  • the powder could also have been stored as it was produced, as a carbon- sequestering storage material.
  • the material could have been left m the supernatant solution and stored, optionally after equilibration with atmospheric air, as a slurry, where both the precipitate and the carbonates and bicarbonates in solution serve as carbon-sequestermg materials
  • Other uses for the material are as described herein, and would be apparent to one of skill in the art.
  • ⁇ 13 C values may be used to confirm the primary source of carbon in a carbonate composition, when a gas mixture that includes a SO x (SO 2 ) as well as CO 2 is used

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