Method and composition for the analysis of ammonia in soil
The colorimetric analysis method using salicylate, phosphate dibasic heptahydrate, and hypochlorite in soil samples addresses the inefficiencies of traditional ammonia measurement methods, providing precise and efficient ammonia detection by measuring the peak absorption wavelength at 380 to 440 nm.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- PRECISION PLANTING LLC
- Filing Date
- 2026-01-14
- Publication Date
- 2026-07-30
AI Technical Summary
Conventional methods for determining ammonia in soil, such as the Kjeldahl method, are cumbersome and time-consuming, while modern infrared sensors do not effectively address the need for precise ammonia measurement in soil analysis.
A colorimetric analysis method using a sample solution mixed with salicylate, phosphate dibasic heptahydrate, and hypochlorite to measure the peak absorption wavelength of ammonia at 380 to 440 nm, avoiding the use of ferricyanide compounds that obscure the peak absorption.
This method provides enhanced and precise measurement of ammonia levels in soil samples by measuring the peak absorption wavelength, offering improved accuracy and efficiency compared to traditional methods.
Smart Images

Figure IB2026050304_30072026_PF_FP_ABST
Abstract
Description
Attorney Docket No. 25006 / WOMETHODS FOR SOIL ANALYSIS AND COMPOSITIONS THEREOFCROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. Application No. 63 / 750,077, filed 27 January 2025, which is incorporated herein by reference in its entirety.BACKGROUND
[0002] Periodic soil testing is an important aspect of the agricultural arts. Test results provide valuable information on the chemical makeup of the soil, such as plant-available nutrients and other important properties (e.g., levels of nitrogen, magnesium, phosphorous, potassium, pH, etc.) so that various amendments may be added to the soil to maximize the quality and quantity of crop production.
[0003] One conventional method for quantitative determination of nitrogen in chemical substances is the Kjeldahl method developed by Johan Kjeldahl in 1883. The method is a cumbersome and time consuming method utilizing sulfuric acid to reduce and liberate the nitrogen as ammonium sulfate followed by distillation with sodium hydroxide to obtain ammonia. The amount of ammonia present, and thus the amount of nitrogen present in the sample, is determined by back titration.
[0004] Recent improvements in soil testing relate to systems and methods for more dynamically assessing various soil properties. One such recent development utilizes infrared sensors to determine the characteristics and properties of the soil. Examples of such recent improvements and developments in soil assessment can be commercially obtained from Precision Planting, LLC.BRIEF SUMMARY
[0005] This summary is intended merely to introduce a simplified summary of some aspects of one or more implementations of the present disclosure. Further areas of applicability of the present disclosure will become apparent from the detailed description provided hereinafter. This summary is not an extensive overview, nor is it intended to identify key or critical elements of the present teachings, nor to delineate the scope of the disclosure. Rather, its purpose is merely to present one or more concepts in simplified form as a prelude to the detailed description and brief description of the drawings provided below.Attorney Docket No. 25006 / WO
[0006] Aspects of the disclosure are directed to methods and / or compositions for colorimetric analysis of ammonia in a sample. In accordance with an aspect, provided is a method for colorimetric analysis of ammonia in a sample, the method comprising: obtaining a sample solution having ammonia; mixing the sample solution with a salicylate, a phosphate dibasic heptahydrate, and a hypochlorite to form an analyte solution; and measuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution
[0007] According to another aspect, provided is a method for colorimetric analysis of ammonia in a soil sample solution, the method comprising: obtaining a sample solution comprising one or more soil particles and water; extracting ammonia from the one or more soil particles by using an extractant composition; mixing the sample solution with a chelating composition; mixing the sample solution with a salicylate; mixing the sample solution with a phosphate dibasic heptahydrate and a hypochlorite to form an analyte solution; and measuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution.
[0008] In accordance with a further aspect, provided is a composition comprising a soil sample; a chelating agent; a salicylate; a phosphate dibasic heptahydrate and / or a salt thereof; a hypochlorite; and water, wherein the composition is free of sodium ferricyanide.BRIEF DESCRIPTION OF THE DRAWINGS
[0009] The present disclosure will become more fully understood from the detailed description and the accompanying drawings, wherein like elements are labeled similarly and in which:
[0010] FIG. 1 is a flow chart of a method in accordance with an aspect of the disclosure;
[0011] FIG.2 is a flow chart of a method according to another aspect of the disclosure;
[0012] FIG.3 is a graph showing the peak absorption wavelength(s) associated with a colorimetric analysis of a soil sample in accordance with aspects of the disclosure; and
[0013] FIGS. 4 and 5 are a graph showing the peak absorption wavelength(s) associated with the colorimetric analysis of the soil sample shown in FIG. 3.
[0014] It should be understood that the various aspects are not limited to the arrangements and instrumentality shown in the drawings.Attorney Docket No. 25006 / WODETAILED DESCRIPTION
[0015] For illustrative purposes, the principles of the present disclosure are described by referencing various exemplary embodiments thereof. Although certain embodiments of the disclosure are specifically described herein, one of ordinary skill in the art will readily recognize that the same principles are equally applicable to, and can be employed in other compositions and methods. Before explaining the disclosed embodiments of the present disclosure in detail, it is to be understood that the disclosure is not limited in its application to the details of any particular embodiment disclosed herein. The terminology used herein is for the purpose of description and not of limitation.
[0016] In the description of embodiments disclosed herein, any reference to direction or orientation is merely intended for convenience of description and is not intended in any way to limit the scope of the present disclosure. Relative terms such as “lower,” “upper,” “horizontal,” “vertical,”, “above,” “below,” “up,” “down,” “top” and “bottom” as well as derivative thereof (e.g., “horizontally,” “downwardly,” “upwardly,” etc.) should be construed to refer to the orientation as then described or as shown in the drawing under discussion. These relative terms are for convenience of description only and do not require that the apparatus be constructed or operated in a particular orientation. Terms such as “attached,” “affixed,” “connected,” “coupled,” “interconnected,” and similar refer to a relationship wherein structures are secured or attached to one another either directly or indirectly through intervening structures, as well as both movable or rigid attachments or relationships, unless expressly described otherwise.
[0017] As used herein and in the appended claims, the singular forms “a”, “an”, and “the” include plural references unless the context dictates otherwise. The singular form of any class of the ingredients refers not only to one chemical species within that class, but also to a mixture of those chemical species. The terms “a” (or “an”), “one or more” and “at least one” may be used interchangeably herein. The terms “comprising”, “including”, and “having” may be used interchangeably. The term “include” should be interpreted as “include, but are not limited to”. The term “including” should be interpreted as “including, but are not limited to”.
[0018] The abbreviations and symbols used herein, unless indicated otherwise, take their ordinary meaning. The abbreviation “wt.%” means percent by weight with respect to the composition and / or solution. The symbol “°” refers to a degree, such as a temperature degree or a degree of an angle.Attorney Docket No. 25006 / WOThe symbols “h”, “min”, “mL”, “nm”, and “pm” refer to hour, minute, milliliter, nanometer, and micrometer, respectively.
[0019] For readability purposes, the chemical functional groups are in their adjective form; for each of the adjectives, the word “group” is assumed. For example, the adjective “alkyl” without a noun thereafter, should be read as “an alkyl group.”
[0020] Any member in a list of species that are used to exemplify or define a genus, may be mutually different from, or overlapping with, or a subset of, or equivalent to, or nearly the same as, or identical to, any other member of the list of species. Further, unless explicitly stated, such as when reciting a Markush group, the list of species that define or exemplify the genus is open, and it is given that other species may exist that define or exemplify the genus just as well as, or better than, any other species listed.
[0021] The phrases, “a mixture thereof,” “a combination thereof,” or a combination of two or more thereof’ do not require that the mixture include all of A, B, C, D, E, and F (although all of A, B, C, D, E, and F may be included). Rather, it indicates that a mixture of any two or more of A, B, C, D, E, and F can be included. In other words, it is equivalent to the phrase “one or more elements selected from the group consisting of A, B, C, D, E, F, and a mixture of any two or more of A, B, C, D, E, and F.” Likewise, the term “a salt thereof’ also relates to “salts thereof.” Thus, where the disclosure refers to “an element selected from the group consisting of A, B, C, D, E, F, a salt thereof, and a mixture thereof,” it indicates that that one or more of A, B, C, D, and F may be included, one or more of a salt of A, a salt of B, a salt of C, a salt of D, a salt of E, and a salt of F may be included, or a mixture of any two of A, B, C, D, E, F, a salt of A, a salt of B, a salt of C, a salt of D, a salt of E, and a salt of F may be included.
[0022] All components and elements positively set forth in this disclosure can be negatively excluded from the claims. In other words, the compositions and / or solutions of the instant disclosure can be free or essentially free of all components and elements positively recited throughout the instant disclosure. In some instances, the compositions and / or solutions of the present disclosure may be substantially free of non-incidental amounts of the ingredient(s) or compound(s) described herein. A non-incidental amount of an ingredient or compound is the amount of that ingredient or compound that is added into the composition or the solution by itself.
[0023] As used throughout, any ranges disclosed herein are used as shorthand for describing each and every value that is within the range. Any value within the range can be selected as the terminusAttorney Docket No. 25006 / WOof the range. Thus, a range from 1-5, includes specifically 1, 2, 3, 4 and 5, as well as subranges such as 2-5, 3-5, 2-3, 2-4, 1-4, etc. The term “about” when referring to a number means any number within a range of 10% of the number. For example, the phrase “about 2 wt.%” refers to a number between and including 1.8 wt.% and 2.2 wt.%.
[0024] In addition, all references cited herein are hereby incorporated by reference in their entireties. In the event of a conflict in a definition in the present disclosure and that of a cited reference, the present disclosure controls.
[0025] Aspects of the disclosure are directed to methods and / or compositions for colorimetric analysis of ammonia in a sample. It was unexpectedly discovered that certain methods disclosed herein can achieve significantly enhanced measurements for the peak absorption wavelength of ammonia using colorimetric analysis. For instance, the inventors surprisingly discovered that methods disclosed herein can measure the peak absorption wavelength for ammonia at a wavelength of about 380 to about 440 nm and, surprisingly, achieve enhanced peak absorption wavelength measured at such wavelengths. These improvements were further unexpected as many traditional colorimetric analyses employ ferricyanide compounds, which have an absorption wavelength that obscures the peak absorption wavelength associated with the ammonia.
[0026] In accordance with an aspect of the disclosure, provided is a method for colorimetric analysis of ammonia in a sample. Referring to FIG. 1, a non-limiting, example method 100 is provided for the colorimetric analysis of ammonia in a sample solution. As a general overview, method 100 comprises obtaining a sample solution comprising ammonia (see step 110); mixing the sample solution with a salicylate compound, a phosphate dibasic heptahydrate compound, and a hypochlorite compound to form an analyte solution (see step 120); and measuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution (see step 230).
[0027] In step 110, a sample solution containing ammonia is obtained. The sample solution may, in some preferred embodiments, be a soil sample solution comprising one or more soil particles and water. Although the sample solution may comprise soil particle(s) in certain embodiment, in other embodiments the sample solution contains ammonia and / or ammonia containing compounds other than soil particles. For example, the sample solution may have ammonia salts and / or ammonia solubilized in a liquid (e.g., water). In at least one embodiment, the sample solution isAttorney Docket No. 25006 / WOan ammonia standard composition, which may be used for calibrating devices and / or as a reference for comparing the amount of ammonia in a sample.
[0028] In step 120, the sample solution is mixed with a salicylate compound, a phosphate dibasic heptahydrate compound, and a hypochlorite compound to form an analyte solution. The salicylate compound, the phosphate dibasic heptahydrate compound, and / or the hypochlorite compound may be mixed with the sample solution in various orders. For example, in some preferred embodiments, the sample solution is mixed with the salicylate compound prior to mixing with the phosphate dibasic heptahydrate compound and / or the hypochlorite compound. In some embodiments, however, the sample solution is mixed with the salicylate compound and / or the phosphate dibasic heptahydrate compound prior to being mixed with the hypochlorite compound. In at least one embodiment, the salicylate compound, the phosphate dibasic heptahydrate compound, and the hypochlorite compound are mixed with the sample solution at substantially the same time or at the same time.
[0029] The analyte solution may comprise the sample solution, the salicylate compound, the phosphate dibasic heptahydrate compound, the hypochlorite compound, and water. In at least one embodiment, the analyte solution consists essentially of or consists of the sample solution, the salicylate compound, the phosphate dibasic heptahydrate compound, the hypochlorite compound, water, and optionally trace impurities. The analyte solution may include one or more or all of the components described below with regard to the soil composition. For example, the analyte solution may include a phosphate dibasic heptahydrate compound, a hypochlorite compound, an extractant, a chelating agent, and / or water in any of the amounts described below with respect to method 200 and / or the soil composition.
[0030] The analyte solution may also comprise an extractant, a chelating agent, and one or more compound extracted from soil particles. For example, method 100 may include the step of extracting one or more compounds, such as ammonia, from the soil particles. After extracting one or more compounds from the one or more soil particles, method 100 may include removing the one or more soil particles. The soil particle(s) may be removed by way of centrifuge, filtration, sedimentation, and / or flocculation. In at least one embodiment, method 100 includes filtering the sample solution and / or the analyte solution to remove the one or more soil particles. Extractants, chelating agents, and / or compositions thereof that may be used in method 100 are further described below with regard to method 200 and / or the soil compositions disclosed herein.Attorney Docket No. 25006 / WO
[0031] Preferably, the analyte solution is substantially free of or free of a ferricyanide compounds, such as a ferricyanide catalyst. In some embodiments, the analyte solution has less than about 100 ppm, less than about 10 ppm, less than about 5 ppm, or less than about 0.5 ppm of ferricyanide compounds. The analyte solution in at least some preferred embodiments is free of ferricyanide compounds. The analyte solution may additionally be substantially free of or free of cyanide compounds. Preferably, the analyte solution has less than about 100 ppm, less than about 10 ppm, less than about 5 ppm, or less than about 0.5 ppm of cyanide compounds. Certain preferred embodiments of the methods disclosed herein have an analyte solution that is free of cyanide compounds.
[0032] The analyte solution may, additionally or alternatively, be free of phenol compounds. In some embodiments, the analyte solution has less than about 100 ppm, less than about 10 ppm, less than about 5 ppm, or less than about 0.5 ppm of phenol compounds. In at least one preferred embodiment, the analyte solution is free of phenol compounds.
[0033] In step 130, a peak absorption wavelength for ammonia is measured for the analyte solution at a wavelength of about 380 to about 440 nm. The intensity of the peak absorption wavelength generally corresponds to the amount of ammonia in the analyte solution. The peak absorption wavelength for ammonia is typically measured using a colorimetric analysis device for method 100. Method 100 may further comprise determining a background value using the calorimetric analysis device. The background value may be determined prior to analyzing the analyte solution. The background value may then be subtracted from the measured peak absorption wavelength for the analyte solution, e.g., to elucidate the intensity of the peak absorption wavelength for the ammonia. In at least one embodiment, the background value is determined by analyzing the peak absorption wavelengths of a standard solution, which comprises the components of the analyte solution except for the components and / or compounds associated with the ammonia compounds, using the calorimetric analysis device.
[0034] The intensity of the peak absorption wavelength for the analyte solution may, preferably, be measured at a wavelength of about 380 to about 440 nm, about 380 to about 430 nm, about 380 to about 420 nm, about 380 to about 410 nm, about 380 to about 400 nm, about 380 to about 395 nm; from about 385 to about 440 nm, about 385 to about 430 nm, about 385 to about 420 nm, about 385 to about 410 nm, about 385 to about 400 nm, about 385 to about 395 nm; about 390 to about 440 nm, about 390 to about 430 nm, about 390 to about 420 nm, about 390 to about 410 nm,Attorney Docket No. 25006 / WOabout 390 to about 400 nm, about 390 to about 395 nm; about 395 to about 440 nm, about 395 to about 430 nm, about 395 to about 420 nm, about 395 to about 410 nm, about 395 to about 400 nm; about 400 to about 440 nm, about 400 to about 430 nm, about 400 to about 420 nm, about 400 to about 410 nm, or any range or subrange thereof. In at least one embodiment, the peak absorption wavelength for the analyte solution is measured at a wavelength of about 395 ppm. As noted above, the peak absorption wavelength at the above measured wavelengths generally corresponds to the amount of ammonia in the analyte solution.
[0035] The intensity of the peak absorption wavelength for the analyte solution may be measured about 30 seconds to about 60 minutes after the analyte solution is formed. In some embodiments, the method further comprises heating the analyte solution prior to measuring the peak absorption wavelength. The analyte solution may be heated to increase the temperature by about 2°C or more, about 5°C or more, about 8°C or more, about 11°C or more, or about 14°C or more, e.g., for at least 1 minute, at least 3 minutes, at least 6 minutes, or at least 10 minutes.
[0036] When method 100 comprises heating the analyte solution prior to measuring the peak absorption wavelength, the analyte solution may be measured about 30 seconds to about 15 minutes after the salicylate compound, the phosphate dibasic heptahydrate compound, and the hypochlorite compound are mixed with the sample solution to form the analyte solution. For example, in certain embodiments of method 100 comprising heating the analyte solution prior to measuring the peak absorption wavelength, the analyte solution is measured about 30 seconds to about 12 minutes, about 30 seconds to about 10 minutes; about 30 seconds to about 8 minutes, about 30 seconds to about 5 minutes, about 30 seconds to about 4 minutes, about 30 seconds to about 3 minutes, about 30 seconds to about 2 minutes, about 30 seconds to about 1 minute; from about 1 to about 15 minutes, about 1 to about 12 minutes, about 1 to about 10 minutes, about 1 to about 8 minutes, about 1 to about 5 minutes, about 1 to about 4 minutes, about 1 to about 3 minutes, about 1 to about 2 minutes; from about 2 to about 15 minutes, about 2 to about 12 minutes, about 2 to about 10 minutes, about 2 to about 8 minutes, about 2 to about 5 minutes, about 2 to about 4 minutes, about 2 to about 3 minutes; from about 3 to about 15 minutes, about 3 to about 12 minutes, about 3 to about 10 minutes, about 3 to about 8 minutes, about 3 to about 5 minutes, about 3 to about 4 minutes; from about 4 to about 15 minutes, about 4 to about 12 minutes, about 4 to about 10 minutes, about 4 to about 8 minutes, about 4 to about 6 minutes, about 4 to about 5 minutes; from about 6 to about 15 minutes, about 6 to about 12 minutes, about 6 to about 10 minutes, aboutAttorney Docket No. 25006 / WO6 to about 10 minutes, about 6 to about 8 minutes; from about 8 to about 15 minutes, about 8 to about 12 minutes, about 8 to about 10 minutes; from about 10 to about 15 minutes, about 10 to about 12 minutes, or any range or subrange thereof, after the analyte solution is formed.
[0037] In embodiments of method 100 that are free of the step of heating the analyte solution prior to measuring the peak absorption wavelength, the analyte solution may be measured about 5 minutes or more after the salicylate compound, the phosphate dibasic heptahydrate compound, and the hypochlorite compound are mixed with the sample solution to form the analyte solution. For example, in certain embodiments of method 100 that are free of heating the analyte solution prior to measuring the peak absorption wavelength, the analyte solution is measured about 5 to about 50 minutes, about 5 to about 40 minutes, about 5 to about 30 minutes, about 5 to about 20 minutes, about 5 to about 17 minutes, about 5 to about 15 minutes, about 5 to about 13 minutes, about 5 to about 11 minutes, about 5 to about 9 minutes; from about 8 to about 60 minutes, about 8 to about 40 minutes, about 8 to about 30 minutes, about 8 to about 20 minutes, about 8 to about 17 minutes, about 8 to about 15 minutes, about 8 to about 13 minutes, about 8 to about 11 minutes; from about 10 to about 60 minutes, about 10 to about 40 minutes, about 10 to about 30 minutes, about 10 to about 20 minutes, about 10 to about 17 minutes, about 10 to about 15 minutes, about 10 to about 13 minutes; from about 12 to about 60 minutes, about 12 to about 40 minutes, about 5 to about 30 minutes, about 12 to about 20 minutes, about 12 to about 17 minutes, about 12 to about 15 minutes; from about 15 to about 60 minutes, about 15 to about 40 minutes, about 15 to about 30 minutes, about 15 to about 20 minutes; from about 20 to about 60 minutes, about 20 to about 40 minutes, about 20 to about 30 minutes; from about 30 to about 60 minutes, about 30 to about 40 minutes, about 40 to about 60 minutes, or any range or subrange thereof, after the analyte solution is formed.
[0038] With reference is FIG. 2, provided is a non-limiting example method 200 for colorimetric analysis of ammonia in a soil sample. As method 200 is an embodiment of a method for colorimetric analysis of ammonia in a soil sample, method 200 includes one or features that may be incorporated into method 100. Likewise, any of the steps, features, and / or components described with regard to method 100 may be included in method 200, unless otherwise indicated. For brevity, method 200 may omit or refer to one or more steps, features, and / or components disclosed herein with reference to method 100 and / or the soil composition disclosed below. Nevertheless, the steps, features, and / or components of method 100 and the soil composition disclosed below are incorporated by reference into various embodiments of method 200.Attorney Docket No. 25006 / WO
[0039] Method 200 typically comprises obtaining a sample solution comprising one or more soil particles and water (see step 210); extracting ammonia from the one or more soil particles by using an extractant composition (see step 212); mixing the sample solution with a chelating composition (see step 214); mixing the sample solution with a salicylate composition comprising a salicylate compound (see step 220); mixing the sample solution with a phosphate dibasic heptahydrate compound and / or a composition thereof and a hypochlorite compound and / or a composition thereof to form an analyte solution (see step 222); and measuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution (see step 230).
[0040] In step 210, method 200 includes obtaining a sample solution comprising one or more soil particles and water. The sample solution may be a soil sample solution, which may or may not be pretreated. For example, in certain embodiments, the sample solution may have been pretreated by way of grinding or the like to reduce the average particle for the one or more soil particles. The sample solution may be pre-treated by way of filtration, centrifuge, or screening to remove unwanted particles (e.g., small rocks). Step 210 may be similar to and / or include one or more features disclosed with regard to step 110 of method 100.
[0041] In step 212, ammonia is extracted from the one or more soil particles of the sample solution using an extractant composition. For example, an extractant composition may be mixed with the sample solution using a mixer to extract the ammonia from the one or more soil particles in the sample solution. In at least one instance, the extractant composition is mixed with the sample solution using a diaphragm pump, e.g., to thoroughly mix soil particles in the sample solution with the extractant composition. Other apertures that may, in certain embodiments, be used or excluded from method 200 for mixing the extractant composition with the sample solution include homogenizers, stirrers, vortex mixers, and / or the like.
[0042] The extractant composition may comprise one or more extractants, e.g., such as those chosen from halogen inorganic salts. The halogen inorganic salt may comprise a chloride group, a bromide group, an iodide group, or a combination thereof. Preferably, the halogen inorganic salt comprises a chloride group or a bromide group. In some preferred embodiments, the halogen inorganic salt has an anion group consisting of a chloride group or a bromide group. The cation group of the halogen inorganic salt may be selected from alkali metals and / or an alkali earth metal. For example, the halogen inorganic salt may have a cation group selected from potassium, sodium,Attorney Docket No. 25006 / WOcalcium, magnesium, lithium, and a combination thereof. In at least one preferred embodiment, the extractant comprises or consists of potassium chloride. The extractant composition may also include an acid, e.g., such as chloric acid, hydrobromic acid, hydroiodic acid, perchloric acid, hydrochloric acid, nitric acid, acetic acid, and / or sulfuric acid. The acid may comprise or be selected from hydrochloric acid, sulfuric acid, acetic acid, hydrobromic acid, hydroiodic acid, and / or perchloric acid. The acid may have a halogen group that corresponds to the halogen group of halogen inorganic salt. In at least one embodiment, the acid is hydrochloric acid. The halogen inorganic salt may in some embodiment partially or fully ionize in the extractant composition.
[0043] The amount of extractant in the extractant composition may be from about 0.1 M to about 3 M. For instance, the concentration of extractant(s) in the extractant composition may be about 0.1 to about 3 M, about 0.1 to about 1.6 M, about 0.1 to about 1.3 M, about 0.1 to about 1 M, about 0.1 to about 0.8 M; from about 0.15 to about 3 M, about 0.15 to about 1.6 M, about 0.15 to about 1.3 M, about 0.15 to about 1 M, about 0.15 to about 0.8 M; from about 0.2 to about 3 M, about 0.2 to about 1.6 M, about 0.2 to about 1.3 M, about 0.2 to about 1 M, about 0.2 to about 0.8 M; from about 0.5 to about 3 M, about 0.5 to about 1.6 M, about 0.5 to about 1.3 M, about 0.5 to about 1 M; from about 0.8 to about 3 M, about 0.8 to about 1.6 M, about 0.8 to about 1.3 M about 0.8 to about 1 M; from about 1 to about 3 M, about 1 to about 1.6 M, about 1 to about 1.4 M, about 1 to about 1.3 M; from about 1.2 to about 3 M, about 1.2 to about 1.6 M; from about 1.4 to about 3 M, about 1.4 to about 1.8 M, about 1.6 to about 2 M, or any range or subrange thereof. In at least one embodiment, the concentration of extractant(s) in the extractant composition is about 1 M.
[0044] Method 200 may include removing the one or more soil particles from the sample solution, e.g., after extraction of ammonia from the one or more soil particles in step 212. The soil particles may be removed by way of centrifuge, filtration, sedimentation, and / or flocculation as described with regard to method 100.
[0045] In step 214, the sample solution is mixed with a chelating composition. The chelating composition typically comprise one or more chelating agent(s). The chelating agent(s) may comprise or consist of hydroxyethylethylenediaminetriacetic acid (HEDTA), trisodium HEDTA, tripotassium HEDTA, trisodium HEDTA monohydrate, disodium HEDTA, ethylene glycol-bis(0-aminoethyl ether)-N,N,N',N'-tetraacetic acid and / or a salt thereof, diethylenetriaminepentaacetic acid and / or a salt thereof, ethylenediaminetetraacetic acid (EDTA), monosodium EDTA, EDTA disodiumsalt, tetrasodium EDTA, or a combination of two or more thereof. For instance, theAttorney Docket No. 25006 / WOchelating agent(s) may be selected from hydroxyethylethylenediaminetriacetic acid (HEDTA), ethylene glycol-bis(P-aminoethyl ether)-N,N,N',N'-tetraacetic acid, diethylenetriaminepentaacetic acid, a salt thereof, and a combination of two or more thereof. In certain embodiments, the chelating agent(s) may comprise EDTA, EGTA, HEDTA, a salt thereof, or a combination of two or more thereof. In at least one preferred embodiment, the chelating agent(s) is chosen from EDTA, EGTA, a salt thereof, and / or a combination of two or more thereof. The chelating agent(s) disclosed herein may be in the form of a salt. In addition to the chelating agent(s), the chelating composition may include water and / or another carrier, such as a monoalcohol and / or a glycol.
[0046] The chelating composition may include the one or more chelating agent(s) in an amount from about 3 to about 9 wt.%, based on the total weight of the chelating composition. For example, the total amount of chelating agents in the chelating composition may be about 3 to about 9 wt.%, about 3 to about 8 wt.%, about 3 to about 7 wt.%, about 3 to about 6 wt.%; about 5 to about 9 wt.%, about 5 to about 8 wt.%, about 5 to about 7 wt.%; about 6 to about 9 wt.%, about 6 to about 8 wt.%, about 7 to about 9 wt.%, or any range or subrange thereof, based on the total weight of the chelating composition.
[0047] In step 220, the sample solution is mixed with a salicylate composition comprising a salicylate compound. The salicylate compound may be in the form of a salt. Examples of salicylate compounds include sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, or a combination thereof. In at least one embodiment, the salicylate compound is selected from the group consisting of sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, ions thereof, and a combination of two or more thereof. The salicylate composition in at least one preferable embodiment comprises, or consists of, sodium salicylate and / or ions thereof.
[0048] The amount of salicylate compound in the salicylate composition may be from about 0.05 M to about 2.8 M. For instance, the concentration of salicylate compound(s) in the salicylate composition may be about 0.05 M to about 2.5 M, about 0.05 M to about 2.2 M, about 0.05 M to about 1.8 M, about 0.05 M to about 1.4 M, about 0.05 M to about 1 M, about 0.05 M to about 0.8 M; from about 0.05 M to about 2.8 M, about 0.05 M to about 2.5 M, about 0.05 M to about 2.2 M, about 0.05 Mto about 1.8 M, about 0.05 Mto about 1.4 M, about 0.05 M to about 1 M, about 0.05 M to about 0.8 M; from about 0.25 M to about 2.8 M, about 0.25 M to about 2.5 M, about 0.25 M to about 2.2 M, about 0.25 M to about 1.8 M, about 0.25 M to about 1.4 M, about 0.25 M to about 1 M, about 0.25 M to about 0.8 M; from about 0.5 M to about 2.8 M, about 0.5 M to about 2.5 M,Attorney Docket No. 25006 / WOabout 0.5 M to about 2.2 M, about 0.5 M to about 1.8 M, about 0.5 M to about 1.4 M, about 0.5 M to about 1 M; from about 1 M to about 2.8 M, about 1 M to about 2.5 M, about 1 M to about 2.2 M, about 1 M to about 1.8 M, about 1 M to about 1.4 M; from about 1.4 M to about 2.8 M, about 1.4 Mto about 2.5 M, about 1.4 Mto about 2.2 M, about 1.4 Mto about 1.8 M; from about 1.8 M to about 2.8 M, about 1.8 M to about 2.5 M, about 1.8 M to about 2.2 M, about 2.2 M to about 2.8 M, or any range or subrange thereof.
[0049] In step 222, the sample solution is mixed with the sample solution with a phosphate dibasic heptahydrate compound and / or a composition thereof and a hypochlorite compound and / or composition thereof to form an analyte solution. In at least one embodiment, the sample solution is mixed with a composition comprising both the phosphate dibasic heptahydrate compound and the hypochlorite compound. In other embodiments, however, the sample solution is mixed with a composition comprising a phosphate dibasic heptahydrate compound and mixed with a separate composition comprising a hypochlorite compound. The sample solution may be mixed with the composition comprising the phosphate dibasic heptahydrate compound before being mixed with the composition comprising the hypochlorite compound. In at least one embodiment, the sample solution is mixed with a composition comprising the hypochlorite compound before being mixed with the composition comprising a phosphate dibasic heptahydrate compound.
[0050] The hypochlorite compound and / or a composition containing the same may comprise sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, or a combination thereof. For example, the hypochlorite compound and / or a composition thereof may comprise sodium hypochlorite. In some instances, the hypochlorite compound may be selected from the group consisting of sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, ions thereof, and a combination of two or more thereof. The heptahydrate composition may comprise water and / or another carrier, such as a monoalcohol and / or a glycol.
[0051] The composition containing the hypochlorite compound (e.g., a hypochlorite composition) may have a total amount of hypochlorite compound of about 0.4 to about 7 wt.%, based on the total weight of the composition containing the hypochlorite compound. For instance, the total amount of hypochlorite compound in the composition containing the hypochlorite compound may be about 0.4 to about 5 wt.%, about 0.4 to about 4 wt.%, about 0.4 to about 3 wt.%, about 0.4 to about 2 wt.%, about 0.4 to about 1.5 wt.%; from about 0.6 to about 7 wt.%, about 0.6 to about 5 wt.%, about 0.6 to about 4 wt.%, about 0.6 to about 3 wt.%, about 0.6 to about 2 wt.%, about 0.6Attorney Docket No. 25006 / WOto about 1.5 wt.%; from about 0.9 to about 7 wt.%, about 0.9 to about 5 wt.%, about 0.9 to about 4 wt.%, about 0.9 to about 3 wt.%, about 0.9 to about 2 wt.%, about 0.9 to about 1.5 wt.%; from about 1.5 to about 7 wt.%, about 1.5 to about 5 wt.%, about 1.5 to about 4 wt.%, about 1.5 to about 3 wt.%; from about 3 to about 7 wt.%, about 3 to about 5 wt.%, about 3 to about 4 wt.%; from about 4 to about 7 wt.%, about 4 to about 5 wt.%, about 5 to about 7 wt.%, based on the total weight of the composition containing the hypochlorite compound.
[0052] The phosphate dibasic heptahydrate compound and / or a composition containing the same may comprise sodium phosphate dibasic heptahydrate and / or potassium phosphate dibasic heptahydrate. In certain embodiments, phosphate dibasic heptahydrate compound is selected from the group consisting of sodium phosphate dibasic heptahydrate, potassium phosphate dibasic heptahydrate, ions thereof, and a combination of two or more thereof. The phosphate dibasic heptahydrate composition may comprise water and / or another carrier, such as a monoalcohol and / or a glycol.
[0053] The amount of phosphate dibasic heptahydrate compound in the composition containing the same may be from about 0.1 M to about 0.8 M. For instance, the concentration of phosphate dibasic heptahydrate compound present in the composition containing the same may be about 0.1 M to about 0.6 M, about 0.1 M to about 0.4 M, about 0.1 M to about 0.3 M; from about 0.2 M to about 0.6 M, about 0.2 M to about 0.4 M, about 0.2 M to about 0.3 M; from about 0.3 M to about 0.6 M, about 0.3 M to about 0.4 M; from about 0.4 M to about 0.6 M, about 0.4 M to about 0.5 M, or any range or subrange thereof.
[0054] In certain preferred embodiments, method 200 includes the sample solution is mixed with a composition comprising the phosphate dibasic heptahydrate compound, the hypochlorite compound, and a base. The composition comprising the phosphate dibasic heptahydrate compound and the hypochlorite compound preferably includes a base in an amount such that the pH of the composition is about 11 to about 14, about 12 to about 13, or about 13. The base may comprise or be selected from an alkali metal hydroxide, sodium hydroxide, potassium hydroxide, and / or lithium hydroxide. An amount of base can be about 0.1 M to about 1 M.
[0055] In step 230, the peak absorption wavelength for ammonia is measured for the analyte solution at a wavelength of about 380 to about 440 nm, the intensity of the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution. Step 230 may includeAttorney Docket No. 25006 / WOone or more steps, features, and / or components of step 130 and / or be the same as step 130 in some embodiments.
[0056] In accordance with a further aspect, provided is a soil composition comprising a soil sample; a chelating agent; a salicylate; a phosphate dibasic heptahydrate and / or a salt thereof; a hypochlorite; and water, wherein the composition is free of sodium ferricyanide. The soil composition disclosed herein may be the same as the analyte composition disclosed with reference to method 100 and / or method 200. The soil compositions may include one or more features and / or components described herein with regard to method 100 and / or method 200.
[0057] The soil composition typically comprises a soil sample. The soil sample may comprise one or more soil particles. In some preferred embodiments, the soil sample comprises one or more compounds extracted from soil particles, where the one or more extracted compounds include ammonia. For instance, in certain embodiments, the soil sample is free of soil particles, but include one or more compounds extracted from soil particles, where the one or more extracted compounds include ammonia or ammonia containing compounds. Thus, in certain embodiments, the soil composition may be free of soil particles.
[0058] In addition to a soil sample, the soil composition typically comprises one or more chelating agent. The chelating agent(s) may comprise or consist of hydroxyethylethylenediaminetriacetic acid (HEDTA), trisodium HEDTA, tripotassium HEDTA, trisodium HEDTA monohydrate, disodium HEDTA, ethylene glycol-bis(P-aminoethyl ether)-N,N,N',N'-tetraacetic acid and / or a salt thereof, diethylenetriaminepentaacetic acid and / or a salt thereof, ethylenediaminetetraacetic acid (EDTA), monosodium EDTA, EDTA disodiumsalt, tetrasodium EDTA, or a combination of two or more thereof. For instance, the chelating agent(s) may be selected from hydroxyethylethylenediaminetriacetic acid (HEDTA), ethylene glycol-bis(P-aminoethyl ether)-N,N,N',N'-tetraacetic acid, diethylenetriaminepentaacetic acid, a salt thereof, and a combination of two or more thereof. For example, the chelating agent(s) may comprise EDTA, EGTA, HEDTA, a salt thereof, or a combination of two or more thereof. In at least one embodiment, the chelating agent(s) is chosen from EDTA, EGTA, a salt thereof, and / or a combination of two or more thereof. The chelating agent(s) disclosed herein may be in the form of a salt.
[0059] The soil composition may include the one or more chelating agent in an amount from about 3 to about 9 wt.%, based on the total weight of the chelating composition. For example, the total amount of chelating agents in the soil composition may be about 3 to about 9 wt.%, about 3 toAttorney Docket No. 25006 / WOabout 8 wt.%, about 3 to about 7 wt.%, about 3 to about 6 wt.%; about 5 to about 9 wt.%, about 5 to about 8 wt.%, about 5 to about 7 wt.%; about 6 to about 9 wt.%, about 6 to about 8 wt.%, about 7 to about 9 wt.%, or any range or subrange thereof, based on the total weight of the chelating composition.
[0060] The soil composition typically comprises one or more salicylate compound. The salicylate compound may be in the form of a salt. Examples of salicylate compounds include sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, or a combination thereof. In at least one embodiment, the salicylate compound is selected from the group consisting of sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, ions thereof, and a combination of two or more thereof. The salicylate composition in at least one preferably embodiment comprises, or consists of, sodium salicylate and / or ions thereof.
[0061] The soil composition also preferably comprises one or more phosphate dibasic heptahydrate compound. The phosphate dibasic heptahydrate compound may comprise sodium phosphate dibasic heptahydrate and / or potassium phosphate dibasic heptahydrate. In certain embodiments, phosphate dibasic heptahydrate compound is selected from the group consisting of sodium phosphate dibasic heptahydrate, potassium phosphate dibasic heptahydrate, ions thereof, and a combination of two or more thereof.
[0062] The phosphate dibasic heptahydrate compound may be present in the soil composition in a concentration of up to about 0.05 M. For example, the concentration of phosphate dibasic heptahydrate compound(s) in the soil composition may be up to about 0.04 M, up to about 0.035 M; from about 0.01 to about 0.05 M, about 0.02 to about 0.05 M, about 0.03 to about 0.05 M, about 0.035 to about 0.05 M, about 0.04 to about 0.05 M; from about 0.01 to about 0.045 M, about 0.02 to about 0.045 M, about 0.03 to about 0.045 M, about 0.035 to about 0.045 M, about 0.04 to about 0.045 M; from about 0.01 to about 0.04 M, about 0.02 to about 0.04 M, about 0.03 to about 0.04 M, about 0.035 to about 0.04 M; from about 0.01 to about 0.035 M, about 0.02 to about 0.035 M, about 0.03 to about 0.035 M; from about 0.01 to about 0.03 M, about 0.02 to about 0.03 M, or any range or subrange thereof.
[0063] The soil composition also typically comprises one or more hypochlorite compound. Examples of hypochlorite compounds include sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, or a combination thereof. Preferably, the heptahydrate compound and / or a composition thereof may comprise sodium hypochlorite. In some instances,Attorney Docket No. 25006 / WOthe heptahydrate compound is selected from the group consisting of sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, ions thereof, and a combination of two or more thereof.
[0064] The amount of hypochlorite compound in the soil composition may be from about 0.3 to about 0.6 wt.%, based on the total weight of the soil composition. In some instances, the soil composition has a total amount of hypochlorite compound of about 0.15 to about 0.6 wt.%, about 0.15 to about 0.55 wt.%, about 0.15 to about 0.5 wt.%, about 0.15 to about 0.45 wt.%, about 0.15 to about 0.4 wt.%, about 0.15 to about 0.35 wt.%, about 0.15 to about 0.3 wt.%; from about 0.2 to about 0.6 wt.%, about 0.2 to about 0.55 wt.%, about 0.2 to about 0.5 wt.%, about 0.2 to about 0.45 wt.%, about 0.2 to about 0.4 wt.%, about 0.2 to about 0.35 wt.%; from about 0.25 to about 0.6 wt.%, about 0.25 to about 0.55 wt.%, about 0.25 to about 0.5 wt.%, about 0.25 to about 0.45 wt.%, about 0.25 to about 0.4 wt.%; from about 0.3 to about 0.6 wt.%, about 0.3 to about 0.55 wt.%, about 0.3 to about 0.5 wt.%, about 0.3 to about 0.45 wt.%; from about 0.35 to about 0.6 wt.%, about 0.35 to about 0.55 wt.%, about 0.35 to about 0.5 wt.%; from about 0.4 to about 0.6 wt.%, about 0.4 to about 0.55 wt.%; from about 0.45 to about 0.6 wt.%, or any range or subrange thereof, based on the total weight of the soil composition.
[0065] The soil composition generally comprises water. The total amount of water in the soil composition may be from about 40 to about 98 wt.%, based on the total weight of the soil composition. For example, the soil composition may comprise water in an amount from about 40 to about 98 wt.%, about 50 to about 98 wt.%, about 60 to about 98 wt.%, about 70 to about 98 wt.%, about 80 to about 98 wt.%, about 90 to about 98 wt.%; from about 40 to about 95 wt.%, about 50 to about 95 wt.%, about 60 to about 95 wt.%, about 70 to about 95 wt.%, about 80 to about 95 wt.%, about 90 to about 95 wt.%; from about 40 to about 92 wt.%, about 50 to about 92 wt.%, about 60 to about 92 wt.%, about 70 to about 92 wt.%, about 80 to about 92 wt.%, about 85 to about 92 wt.%; from about 40 to about 85 wt.%, about 50 to about 85 wt.%, about 60 to about 85 wt.%, about 70 to about 85 wt.%, about 80 to about 85 wt.%; from about 40 to about 80 wt.%, about 50 to about 80 wt.%, about 60 to about 80 wt.%, about 70 to about 80 wt.%; from about 40 to about 70 wt.%, about 50 to about 70 wt.%, about 60 to about 70 wt.%; from about 40 to about 60 wt.%, about 50 to about 60 wt.%, or any range or subrange thereof, based on the total weight of the soil composition.Attorney Docket No. 25006 / WO
[0066] Preferably, the soil composition is substantially free of or free of a ferricyanide compounds, such as a ferricyanide catalyst. In some embodiments, the soil composition has less than about 100 ppm, less than about 10 ppm, less than about 5 ppm, or less than about 0.5 ppm of ferricyanide compounds. The soil composition in some preferred embodiments is free of ferricyanide compounds. The soil composition may additionally be substantially free of or free of cyanide compounds. Preferably, the soil composition has less than about 100 ppm, less than about 10 ppm, less than about 5 ppm, or less than about 0.5 ppm of cyanide compounds. In certain preferred embodiments, the soil composition is free of cyanide compounds.
[0067] The soil composition may, additionally or alternatively, be free of phenol compounds. In some embodiments, the soil composition has less than about 100 ppm, less than about 10 ppm, less than about 5 ppm, or less than about 0.5 ppm of phenol compounds. In at least one preferred embodiment, the soil composition is free of phenol compounds.
[0068] In accordance with further aspects of the disclosure, provided is the use of a composition (such as a soil composition disclosed herein and / or analyte composition disclosed herein) for colorimetric analysis of ammonia in the soil sample. In certain embodiments, the composition (e.g., soil composition and / or analyte composition) is used for measuring a peak absorption wavelength at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in composition.
[0069] The methods and compositions disclosed herein are usable with and may form part of an overall agricultural sampling and analysis systems, such as but not limited to those described in U.S. Patent Application Publication No. 2018 / 0124992A1, PCT Publication Nos. W02020 / 012369, W02020 / 148640, W02021 / 171120, WO2021 / 171121, W02021 / 220082, W02021 / 220083, WO2021 / 220084, W02021 / 220085, W02022 / 013623, WO2022 / 013624, WO2022 / 013625, W02022 / 013626, WO2022 / 013627, WO2022 / 013628, WO2022 / 013629, W02022 / 013630, W02022 / 013631, WO2022 / 013632, WO2022 / 013633, WO2022 / 243792, WO2022 / 243793, WO2022 / 243794, WO2022 / 243795, WO2022 / 243796, WO2022 / 243797, WO2022 / 243806, WO2022 / 243807, WO2022 / 243808, WO2022 / 243809, WO2022 / 259071, WO2022 / 259073, WO2022 / 259074, WO2022 / 269388, WO2023 / 031725, WO2023 / 031726, WO2023 / 031727, W02023 / 042032, W02023 / 042033, W02023 / 042035, W02023 / 042036, W02023 / 042037, W02023 / 042038, W02023 / 042039, WO2023 / 161727, WO2023 / 161728, WO2023 / 170480, WO2023 / 170482, WO2023 / 227959, WO2023 / 227960, WO2023 / 248015,Attorney Docket No. 25006 / WOWO2023 / 248016, WO2024 / 023728, WO2024 / 023729, W02024 / 023730, WO2024 / 023731, United States Application Nos. 63 / 676226, filed 26-Jul-2024, 63 / 552730, filed 13-Feb-2024, 63 / 559305, filed 29-Feb-2024, 63 / 559308, filed 29-Feb-2024, 63 / 559316, filed 29-Feb-2024, 63 / 665406, filed 28-Jun-2024, 63 / 669007, filed 09-Jul-2024, 63 / 675398, filed 25-Jul-2024, 63 / 675875, filed 26-Jul-2024, 63 / 675919, filed 26- Jul-2024, 63 / 676087, filed 26-Jul-2024, 63 / 676426, filed 28-Jul-2024, 63 / 679437, filed 05-Aug-2024, and PCT Application Nos. PCT / IB2024 / 051283, filed 12-Feb-2024, PCT / IB2024 / 051820, filed 26-Feb-2024, PCT / IB2024 / 058213 , filed 23-Aug-2024, PCT / IB2024 / 058336, filed 28-Aug-2024, PCT / IB2024 / 058337, filed 28-Aug-2024, PCT / IB2024 / 058338, filed 28-Aug-2024, PCT / IB2024 / 059313, filed 25-Sep-2024, PCT / IB2024 / 059314, filed 25-Sep-2024, PCT / IB2024 / 059315, filed 25-Sep-2024, PCT / IB2024 / 059316, filed 25-Sep-2024.EXAMPLEExample 1
[0070] A soil sample was evaluated pursuant a non-limiting, example method according to aspects of the disclosure. Specifically, a soil sample containing soil particles was mixed with a solution containing 1 M of potassium chloride to extract nutrients and compounds from the soil particles. The solution containing the soil particles was then filtered to remove the soil particles and obtain a soil extraction solution.
[0071] A 1.5 mb sample of the soil extraction solution was pipetted into a test tube. A 200 pL sample of a chelating solution containing 6 wt.% of sodium ED TA solution with the remainder being water was then added to the test tube and mixed. A 200 pL sample of sodium salicylate solution was then added and mixed into the solution in the test tube. Subsequently, a 200 pL sample of a buffered sodium hypochlorite solution was added and mixed into the solution in the test tube to form an analyte sample solution.
[0072] After 2 minutes, the analyte sample solution was evaluated at room temperature (e.g., about 20°C) using a colorimetric analysis device, such as a Cary™ 100 or a Cary™ 3500 from Agilent. The analyte sample solution was evaluated at room temperature (e.g., about 20°C) about 10 minutes after the buffered sodium hypochlorite solution was added to the test tube solution. Further, the analyte sample solution was evaluated over an absorption wavelength of 370 to 730Attorney Docket No. 25006 / WOnm. A background value of absorbance was collected before the sodium hypochlorite solution was added.
[0073] A summary of the colorimetric analysis for the ammonia in the soil sample is shown in FIGS. 3-5. As seen in FIGS. 3-5, the absorbance of the ammonia in the soil sample at the 385 to 400 nm was unexpectedly about 300% greater than at 645 to 655 nm. The significantly greater peak absorption wavelength for ammonia at a wavelength of 385 to 400 nm as compared to a wavelength of 645 to 655 nm was further surprising as many traditional colorimetric analyses employ ferricyanide compounds, which have an absorption wavelength over the wavelengths of 385 to 400 nm, thereby obscuring the peak absorption wavelength associated with the ammonia.
[0074] The following are nonlimiting examples.
[0075] Example 1 - a method for colorimetric analysis of ammonia in a sample, the method comprising obtaining a sample solution comprising ammonia; mixing the sample solution with a salicylate compound, a phosphate dibasic heptahydrate compound, a base, a chelating composition, and a hypochlorite compound to form an analyte solution; and measuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution.
[0076] Example 2 - the method according to Example 1, wherein the sample solution is mixed with the salicylate compound before the phosphate dibasic heptahydrate compound or the hypochlorite compound is added into the sample solution.
[0077] Example 3 - the method according to Example 1 or Example 2 further comprising: extracting the ammonia from the sample solution by mixing the sample solution with an extractant composition.
[0078] Example 4 - a method for colorimetric analysis of ammonia in a soil sample, the method comprising: obtaining a sample solution comprising one or more soil particles and water; extracting ammonia from the one or more soil particles by using an extractant composition; mixing the sample solution with a chelating composition; mixing the sample solution with a salicylate composition comprising a salicylate compound; mixing the sample solution with a phosphate dibasic heptahydrate compound and a hypochlorite compound to form an analyte solution; and measuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution.Attorney Docket No. 25006 / WO
[0079] Example 5 - the method according to any foregoing Example, wherein the method is free of employing a ferricyanide compound.
[0080] Example 6 - the method according to any foregoing Example, wherein the method is free of employing a cyanide compound.
[0081] Example 7 - the method according to any foregoing Example, wherein the method is free of phenol compounds.
[0082] Example 8 - the method according to any one of Example 3 to Example 7, wherein the extractant composition comprises a halogen inorganic salt.
[0083] Example 9 - the method according to Example 8, wherein the halogen inorganic comprises a chloride group, a bromide group, an iodide group, or a combination thereof.
[0084] Example 10 - the method according to Example 9, wherein the halogen inorganic comprises a chloride group and an alkali metal and / or an alkali earth metal.
[0085] Example 11 - the method according to any one of Example 3 to Example 10, wherein the extractant composition comprises potassium chloride.
[0086] Example 12 - the method according to Example 11, wherein the potassium chloride is present in a molarity of about 0.1 M to about 3 M, preferably about 0.5 to about 1.5 M or about IM.
[0087] Example 13 - the method according to any foregoing Example, wherein the chelating composition comprises an EDTA, an EGTA, a salt thereof, or a combination of two or more thereof.
[0088] Example 14 - the method according to any foregoing Example, wherein the chelating composition is present in an amount from about 3 to about 9 wt.%, based on a total weight of a final composition.
[0089] Example 15 - the method according to any foregoing Example, wherein the salicylate compound is selected from sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, and a combination thereof.
[0090] Example 16 - the method according to any foregoing Example, wherein the salicylate compound comprises sodium salicylate.
[0091] Example 17 - the method according to any foregoing Example, wherein the hypochlorite compound is selected from sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, and a combination thereof.Attorney Docket No. 25006 / WO
[0092] Example 18 - the method according to any foregoing Example, wherein the hypochlorite compound comprises sodium hypochlorite.
[0093] Example 19 - the method according to any foregoing Example, wherein the phosphate dibasic heptahydrate compound comprises sodium phosphate dibasic heptahydrate or potassium phosphate dibasic heptahydrate.
[0094] Example 20 - the method according to any foregoing Example, wherein the measuring the peak absorption wavelength for the analyte solution occurs about 10 minutes or more after the salicylate compound, the phosphate dibasic heptahydrate compound, and the hypochlorite compound are mixed with the sample solution.
[0095] Example 21 - the method according to any one of Example 1 to Example 19 further comprising: heating the analyte solution prior to measuring the peak absorption wavelength.
[0096] Example 22 - the method according to Example 21, wherein the measuring of the peak absorption wavelength for the analyte solution occurs about 30 seconds to about 15 minutes after the analyte solution is formed.
[0097] Example 23 - the method according to any foregoing Example, wherein the peak absorption wavelength for the analyte solution is measured at a wavelength of about 385 to about 400 nm.
[0098] Example 24 - the method according to any foregoing Example, wherein the peak absorption wavelength for the analyte solution is measured at a wavelength of about 395 nm.
[0099] Example 25 - the method according to any foregoing claim, wherein the base is present in an amount such that the analyte solution has a pH of about 11 to about 14 or about 12 to about 13.
[0100] Example 26 - the method according to any foregoing claim, wherein the base is present in an amount of about 0.1 M to about 1 M.
[0101] Example 27 - a soil composition comprising: a soil sample; a chelating agent; a salicylate compound; a phosphate dibasic heptahydrate compound; a hypochlorite compound; and water, wherein the composition is free of sodium ferricyanide.
[0102] Example 28 - the soil composition according to Example 27, wherein the soil sample comprises one or more soil particle.Attorney Docket No. 25006 / WO
[0103] Example 29 - the soil composition according to Example 27 or Example 28, wherein the soil sample comprises one or more compounds extracted from soil particles, the one or more compounds comprising ammonia.
[0104] Example 30 - the soil composition according to any one of Example 27 to Example 29, wherein the soil composition is substantially free of or free of ferricyanide compounds.
[0105] Example 31 - the soil composition according to any one of Example 27 to Example 30, wherein the soil composition is substantially free of or free of cyanide compounds.
[0106] Example 32 - the soil composition according to any one of Example 27 to Example 31, wherein the soil composition is substantially free of or free of phenol compounds.
[0107] Example 33 - the soil composition according to any one of Example 27 to Example 31, wherein the chelating composition comprises an EDTA, an EGTA, a salt thereof, or a combination of two or more thereof.
[0108] Example 34 - the soil composition according to any one of Example 27 to Example 33, wherein the chelating composition is present in an amount from about 3 to about 9 wt.%, based on a total weight of the soil composition.
[0109] Example 35 - the soil composition according to any one of Example 27 to Example 34, wherein the salicylate compound is selected from sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, ions thereof, and a combination of two or more thereof.
[0110] Example 36 - the soil composition according to any one of Example 27 to Example 35, wherein the salicylate compound comprises sodium salicylate.
[0111] Example 37 - the composition according to any one of Example 27 to Example 36, wherein the hypochlorite compound is selected from sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, ions thereof, and a combination of two or more thereof.
[0112] Example 38 - the composition according to any one of Example 27 to Example 37, wherein the hypochlorite compound comprises sodium hypochlorite.
[0113] Example 39 - the composition according to any one of Example 27 to Example 38, wherein the phosphate dibasic heptahydrate compound comprises sodium phosphate dibasic heptahydrate.Attorney Docket No. 25006 / WO
[0114] Example 40 - the composition according to any one of Example 27 to Example 39, wherein the base is present in an amount such that the composition has a pH of about 11 to about 14 or about 12 to about 13.
[0115] Example 41 - the composition according to any one of Example 27 to Example 39, wherein the base is present in an amount of about 0.1 M to about 1 M.
[0116] Example 42 - use of the composition according to any one of Example 27 to Example 41 for colorimetric analysis of ammonia in the soil sample.
[0117] Example 43 - use of the composition according to any one of Example 27 to Example 41 for measuring a peak absorption wavelength at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in composition.
Claims
Attorney Docket No. 25006 / WOCLAIMSWhat is Claimed is:
1. A method for colorimetric analysis of ammonia in a sample, the method comprising obtaining a sample solution comprising ammonia;mixing the sample solution with a salicylate compound, a phosphate dibasic heptahydrate compound, a base, a chelating composition, and a hypochlorite compound to form an analyte solution; andmeasuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution.
2. The method according to claim 1 , wherein the sample solution is mixed with the salicylate compound before the phosphate dibasic heptahydrate compound or the hypochlorite compound is added into the sample solution.
3. The method according to claim 1 or claim 2 further comprising:extracting the ammonia from the sample solution by mixing the sample solution with an extractant composition.
4. A method for colorimetric analysis of ammonia in a soil sample, the method comprising:obtaining a sample solution comprising one or more soil particles and water; extracting ammonia from the one or more soil particles by using an extractant composition;mixing the sample solution with a chelating composition;mixing the sample solution with a salicylate composition comprising a salicylate compound;mixing the sample solution with a phosphate dibasic heptahydrate compound, a base, and a hypochlorite compound to form an analyte solution; andmeasuring a peak absorption wavelength for the analyte solution at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in the analyte solution.
5. The method according to any foregoing claim, wherein the method is free of employing a ferricyanide compound.Attorney Docket No. 25006 / WO6. The method according to any foregoing claim, wherein the method is free of employing a cyanide compound.
7. The method according to any foregoing claim, wherein the method is free of phenol compounds.
8. The method according to any one of claim 3 to claim 7, wherein the extractant composition comprises a halogen inorganic salt.
9. The method according to claim 8, wherein the halogen inorganic comprises a chloride group, a bromide group, an iodide group, or a combination thereof.
10. The method according to claim 9, wherein the halogen inorganic comprises a chloride group and an alkali metal and / or an alkali earth metal.
11. The method according to any one of claim 3 to claim 10, wherein the extractant composition comprises potassium chloride.
12. The method according to claim 11, wherein the potassium chloride is present in a molarity of about 0.1 M to about 3 M, preferably about 0.5 to about 1.5 M or about 1 M.
13. The method according to any foregoing claim, wherein the chelating composition comprises an EDTA, an EGTA, a salt thereof, or a combination of two or more thereof.
14. The method according to any foregoing claim, wherein the chelating composition is present in an amount from about 3 to about 9 wt.%, based on a total weight of a final composition.
15. The method according to any foregoing claim, wherein the salicylate compound is selected from sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, and a combination thereof.
16. The method according to any foregoing claim, wherein the salicylate compound comprises sodium salicylate.
17. The method according to any foregoing claim, wherein the hypochlorite compound is selected from sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, and a combination thereof.
18. The method according to any foregoing claim, wherein the hypochlorite compound comprises sodium hypochlorite.Attorney Docket No. 25006 / WO19. The method according to any foregoing claim, wherein the phosphate dibasic heptahydrate compound comprises sodium phosphate dibasic heptahydrate or potassium phosphate dibasic heptahydrate.
20. The method according to any foregoing claim, wherein the measuring the peak absorption wavelength for the analyte solution occurs about 10 minutes or more after the salicylate compound, the phosphate dibasic heptahydrate compound, and the hypochlorite compound are mixed with the sample solution.
21. The method according to any one of claim 1 to claim 19 further comprising:heating the analyte solution prior to measuring the peak absorption wavelength.
22. The method according to claim 21, wherein the measuring of the peak absorption wavelength for the analyte solution occurs about 30 seconds to about 15 minutes after the analyte solution is formed.
23. The method according to any foregoing claim, wherein the peak absorption wavelength for the analyte solution is measured at a wavelength of about 385 to about 400 nm.
24. The method according to any foregoing claim, wherein the peak absorption wavelength for the analyte solution is measured at a wavelength of about 395 nm.
25. The method according to any foregoing claim, wherein the base is present in an amount such that the analyte solution has a pH of about 11 to about 14 or about 12 to about 13.
26. The method according to any foregoing claim, wherein the base is present in an amount of about 0.1 M to about 1 M.
27. A soil composition comprising:a soil sample;a chelating agent;a salicylate compound;a phosphate dibasic heptahydrate compound;a base;a hypochlorite compound; andwater,wherein the composition is free of sodium ferricyanide.
28. The soil composition according to claim 27, wherein the soil sample comprises one or more soil particle.Attorney Docket No. 25006 / WO29. The soil composition according to claim 27 or claim 28, wherein the soil sample comprises one or more compounds extracted from soil particles, the one or more compounds comprising ammonia.
30. The soil composition according to any one of claim 27 to claim 29, wherein the soil composition is substantially free of or free of ferricyanide compounds.
31. The soil composition according to any one of claim 27 to claim 30, wherein the soil composition is substantially free of or free of cyanide compounds.
32. The soil composition according to any one of claim 27 to claim 31, wherein the soil composition is substantially free of or free of phenol compounds.
33. The soil composition according to any one of claim 27 to claim 32, wherein the chelating composition comprises an EDTA, an EGTA, a salt thereof, or a combination of two or more thereof.
34. The soil composition according to any one of claim 27 to claim 33, wherein the chelating agent is present in an amount from about 3 to about 9 wt.%, based on a total weight of the soil composition.
35. The soil composition according to any one of claim 27 to claim 34, wherein the salicylate compound is selected from sodium salicylate, potassium salicylate, zinc salicylate, calcium salicylate, ions thereof, and a combination of two or more thereof.
36. The soil composition according to any one of claim 27 to claim 35, wherein the salicylate compound comprises sodium salicylate.
37. The composition according to any one of claim 27 to claim 36, wherein the hypochlorite compound is selected from sodium hypochlorite, potassium hypochlorite, zinc hypochlorite, calcium hypochlorite, ions thereof, and a combination of two or more thereof.
38. The composition according to any one of claim 27 to claim 37, wherein the hypochlorite compound comprises sodium hypochlorite.
39. The composition according to any one of claim 27 to claim 38, wherein the phosphate dibasic heptahydrate compound comprises sodium phosphate dibasic heptahydrate.
40. The composition according to any one of claim 27 to claim 39, wherein the base is present in an amount such that the composition has a pH of about 11 to about 14 or about 12 to about 13.Attorney Docket No. 25006 / WO41. The composition according to any one of claim 27 to claim 39, wherein the base is present in an amount of about 0.1 M to about 1 M.
42. Use of the composition according to any one of claim 27 to claim 41 for colorimetric analysis of ammonia in the soil sample.
43. Use of the composition according to any one of claim 27 to claim 41 for measuring a peak absorption wavelength at a wavelength of about 380 to about 440 nm, the peak absorption wavelength corresponding to the amount of ammonia in composition.