HORTICULTURAL HYDROGELS
20240324530 ยท 2024-10-03
Inventors
Cpc classification
A01G22/05
HUMAN NECESSITIES
International classification
Abstract
The present disclosure relates to horticultural hydrogels for growing plants and/or fungi, and more particularly to hydrogel-based substrates for the germination, growth, and/or sporulation of those plants and/or fungi.
Claims
1. A horticultural hydrogel comprising: carrageenan; water; and fertilizer; the horticultural hydrogel being opaque and including: hardness of more than 150 g/cm.sup.2; cohesiveness of more than 75%; springiness of 92% to 100%; electrical conductivity of 2.3 to 8.5; and a pH between 5.2 and 8.5.
2. The horticultural hydrogel of claim 1, wherein the horticultural hydrogel further comprises carbon and is not opaque.
3. The horticultural hydrogel of claim 1, further comprising microcrystalline cellulose.
4. The horticultural hydrogel of claim 3, wherein the plant is kale, spinach, butter lettuce, bok choy, or crunchy lettuce.
5. The horticultural hydrogel of claim 3, wherein the plant is a berry, pepper, or herb, such as: raspberry, strawberry, blackberry, blueberry, bell peppers, sweet peppers, basil, thyme, or sage.
6. The horticultural hydrogel of claim 1, wherein the horticultural hydrogel includes 97% to 99% water.
7. The horticultural hydrogel of claim 1, wherein water content of the horticultural hydrogel remains unchanged after 90 days in ambient conditions.
8. The horticultural hydrogel of claim 1, wherein the horticultural hydrogel is freeze dried and reconstituted to have a water content of 97% to 99%.
9. The horticultural hydrogel of claim 1, wherein the horticultural hydrogel is frozen to below 32? F. and thawed to at least 65? F. at least one time.
10. The horticultural hydrogel of claim 1, wherein the horticultural hydrogel may lose water content such that a new water content is 60% and may be rehydrated to a water content of 97% to 99%.
11. The horticultural hydrogel of claim 1, wherein the hardness further allows for an automated robotic part to manipulate the horticultural hydrogel without compromising the integrity of the horticultural hydrogel.
12. The horticultural hydrogel of claim 1, wherein the horticultural hydrogel exhibits a germination rate for a spinach seed that is at least twice as high as a spinach seed germinated in soil, peat, or coir.
13. The horticultural hydrogel of claim 1, comprising: 0.8% to 1.7% carrageenan; 96% to 99% water; 0.1% to 0.2% fertilizer; optionally, 0.01% to 0.1% microcrystalline cellulose; and optionally, 0.005% to 0.015% acid.
14. The horticultural hydrogel of claim 13, wherein the acid is phosphoric acid or citric acid.
15. The horticultural hydrogel of claim 13, further comprising carbon.
16. The horticultural hydrogel of claim 15, wherein the horticultural hydrogel is not opaque.
17. A horticultural hydrogel comprising: carrageenan; water; and fertilizer; the horticultural hydrogel being opaque and including: hardness of 400 g/cm.sup.2 to 1300 g/cm.sup.2; cohesiveness of 75% to 90%; springiness of 92% to 100%; electrical conductivity of 3.5 to 8.5; and a pH between 5.5 and 8.5, wherein a seed placed within the horticultural hydrogel will have at least a 20% increase in plant mass relative to the plant grown in coir or peat.
18. The horticultural hydrogel of claim 1, further comprising microcrystalline cellulose.
19. A method of preparing a horticultural hydrogel plug comprising the steps of: mixing carrageenan, fertilizer, and, optionally, carbon and microcrystalline cellulose to form a mixture; heating the mixture to at least 85? C. while mixing to form a homogeneous mixture; cooling the homogeneous mixture to less than 70? C.; and pouring the homogeneous mixture into a gel plug mold to form a horticultural hydrogel plug, wherein the horticultural hydrogel plug includes: hardness of more than 150 g/cm.sup.2; cohesiveness of more than 75%; springiness of 92% to 100%; electrical conductivity of 2.3 to 8.5; and a pH between 5.2 and 8.5.
20. The method of claim 19, further comprising the step of adjusting the pH with citric acid or phosphoric acid.
Description
BRIEF DESCRIPTION OF THE FIGURES
[0065] The disclosure will be better understood, and features, aspects, and advantages other than those set forth above will become apparent when consideration is given to the following detailed description thereof. Such detailed description refers to the following drawings.
[0066]
[0067]
[0068]
[0069]
DETAILED DESCRIPTION
Definitions
[0070] Unless otherwise defined, all terms of art, notations and other scientific terms or terminology used herein are intended to have the meanings commonly understood by those of skill in the art to which this disclosure pertains. In some cases, terms with commonly understood meanings are defined herein for clarity and/or for ready reference, and the inclusion of such definitions herein should not necessarily be construed to represent a substantial difference over what is generally understood in the art. Many of the techniques and procedures described or referenced herein are well understood and commonly employed using conventional methodology by those skilled in the art.
[0071] The singular form a, an, and the include plural references unless the context clearly dictates otherwise. For example, the term a cell includes one or more cells, including mixtures thereof.
[0072] Ambient temperature as used herein is a temperature of between 18? C. to 24? C. and a relative humidity of between 60% to 95%.
[0073] As used herein, biofertilizers are microbial fertilizers that supply the plant with nutrients and thereby can promote plant growth in the absence of chemical fertilizers. Non-limiting examples of microbial isolates that can directly promote plant growth and/yield include N2-fixing bacteria Rhizobium and Bradyrhizobium species that, through symbiotic nitrogen fixation, can form nodules on roots of leguminous plants, in which they convert atmospheric N2 into ammonia which, in contrast to atmospheric N2, can be used by the plant as a nitrogen source. Other examples include Azospirillum species, which are free-living N2-fixers that can fertilize and increase yield of cereal crops such as wheat, sorghum, and maize. Despite Azospirillum's N2-fixing capacity, the yield increase caused by inoculation by Azospirillum is often attributed to increased root development and thus to increased rates of water and mineral uptake. In this respect, several rhizobacteria like Azotobacter spp. have been reported to be capable of producing a wide array of phytohormones (e.g., auxins, cytokinins) and enzymes (e.g., pectinase). Many of these phytohormones and enzymes have been shown to be intimately involved in the infection process of symbiotic bacteria-plant associations which have a regulatory influence on nodulation by Rhizobium. Biofertilizers can also affect the plant growth and development by modifying nutrient uptake. They may alter nutrient uptake rates, for example, by direct effects on roots, by effects on the environment which in turn modify root behavior, and by competing directly for nutrients (Gaskins et al., Agricult. Ecosyst. Environ. 12:99-116, 1985). Some factors by which Biofertilizers may play a role in modifying the nutrient use efficiency in soils include, for example, root geometry, nutrient solubility, nutrient availability by producing plant congenial ion form, partitioning of the nutrients in plant and utilization efficiency. For example, a low level of soluble phosphate can limit the growth of plants. Some plant growth-promoting microbes are capable of solubilizing phosphate from either organic or inorganic bound phosphates, thereby facilitating plant growth. Several enzymes of microbial origin, such as nonspecific phosphatases, phytases, phosphonatases, and C-P lyases, release soluble phosphorus from organic compounds in soil. For example, an increased solubilization of inorganic phosphorus in soil has been found to enhance phosphorus uptake in canola seedling using Pseudomonas putida as well as increased sulfur-oxidation and sulfur uptake (Grayston and Germida, Can. J. Microbiol. 37:521-529, 1991; Banerjee, Phytochemicals and Health, vol. 15, May 18, 1995).
[0074] Biostimulants, as used herein, can produce substances that stimulate the growth of plants in the absence of pathogens. For example, the production of plant hormones is a characteristic of many plant-associated microorganisms. Some microorganisms can also produce secondary metabolites that affect phytohormone production in plants. Probably, the best-known example is hormone auxin, which can promote root growth. Other examples include pseudomonads which have been reported to produce indole acetic acid (IAA) and to enhance the amounts of IAA in plants, thus having a profound impact on plant biomass production (Brown, Annual Rev. Phytopathology, 68:181-197, 1974). For example, Tien et al. (Applied Environmental Microbiol., 37:1016-1024, 1979) reported that inoculation of nutrient solutions around roots of pearl millet with Azospirillum brasiliense resulted in increased shoot and root weight, an increased number of lateral roots, and all lateral roots were densely covered with root hairs. Plants supplied with combinations of IAA, gibberellins and kinetin showed an increase in the production of lateral roots similar to that caused by Azospirilla. Additionally, some rhizobacteria, such as strains of the bacterial species B. subtilis, B. amyloliquefaciens, and Enterobacter cloacae, promote plant growth by releasing volatile organic compounds, VOCs. The highest level of growth promotion has been observed with 2,3-butanediol and 3-hydroxy-2-butanone (also referred to as acetoin) as elicitors of induced systemic resistance. The cofactor PQQ has been described as a plant growth promoter, which acts as an antioxidant in plants. Other examples of biostimulants, as contemplated by the present disclosure, include products listed at https: growerssecret.com. Particularly, Grower's Secret Professional, Seaweed Powder 0-0-16, Soluble Corn Steep Powder 7-6-4, Granule's 8-3-1, Nitrogen 16-0-0, Liquid Nitrogen 8-0-0, Grower's Secret Microbes, Phosphorous 0-9-0, Seaweed Powder 0-0-16, or VitalVit Micronutrients. Other biostimulants include silica, amino acids, or agriculturally relevant enzymes.
[0075] Carbon as used in the present disclosure includes charcoal. Carbon may be commercially sourced such as through General Carbon, Fisher Scientific and VWR.
[0076] Carrageenan is an anionic polymer, a sulfated linear polysaccharide. Carrageenans have been classified into three different types, namely, ?-carrageenan, ?-carrageenan, and ?-carrageenan on the basis of the degree of sulfation. Carrageenan, as is contemplated in the present disclosure, refers to kappa carrageenan, which as the highest hydro-gel forming efficiency. The source may be purchased commercially such as Ricogel, Marcel, W-Hydrocolloids or CP Kelco. Carrageenan can also be purified from red algae as is known by those skilled in the art.
[0077] Fertilizer as used in the present disclosure provides nutrients such as phosphorus, nitrogen, carbon, hydrogen, oxygen, potassium, calcium, magnesium, sulfur, iron, boron, copper, manganese, zinc, molybdenum, chlorine, cobalt, or nickel whether synthetic or organic. Suitable fertilizers may be commercially sourced, such as Miracle-Gro water soluble plant food vegetable and herbs, Clonex, Dyna-Gro, M&S (Murashige and Skoog) or FloraMicro. As used herein fertilizer, which generally are classified according to their NPK content. NPK is common terminology used in the fertilizer industry and stands for: (1)Nthe amount of nitrogen in the formulation as N; (2) Pthe amount of phosphorus in the formulation as P.sub.2O.sub.5; and (3) Kthe amount of potassium in the formulation as K.sub.2O. In other words, the N refers to nitrogen-containing compounds that are added to the soil and are utilized by the particular plant to satisfy its nitrogen requirement. The P refers to phosphorus-containing compounds that are added to the soil and are utilized by the particular plant to satisfy its phosphorus requirement (a nutrient required for plant growth). K refers to potassium-containing compounds that are added to the soil and are utilized by the particular plant to satisfy its potassium requirement (another nutrient essential for plant growth). Besides these nutrients, namely nitrogen, phosphorus and potassium, which are normally provided by the addition of fertilizers that typically are known as NPK fertilizers, other nutrients can also be provided by the addition of fertilizers to the soil. Typical nutrients are calcium, magnesium, sulfur, iron, zinc, manganese, copper, boron, and molybdenum. The term fertilizer as used herein, unless expressly indicated otherwise, refers to NPK fertilizers, that is, fertilizers that include one or more of the nutrients (nitrogen, phosphorus and potassium).
[0078] Cohesiveness defines the cohesive properties of a polymer find direct expression in its solubility in organic liquids. The cohesive properties of a substance are expressed quantitatively in the cohesive energy. This quantity is closely related to the internal pressure, a parameter appearing in the equation of state of the substance.
[0079] Hardness is the resistance of a material to permanent indentation or maximum force of the gel. Hardness can be measured in g/cm.sup.2.
[0080] A hydrogel is a crosslinked hydrophilic polymer that does not dissolve in water. They are highly absorbent yet maintain well defined structures.
[0081] Organic means components that have been certified as organic from the USDA National Organic Program.
[0082] Organic materials means carbon-based materials such as soil, wood or wood components (e.g., shavings), peat, coir, and other natural materials.
[0083] Plant or plant part includes all parts of the plant, including: root, stem, meristem, seed, leaf, cotyledons, and the like.
[0084] Plant plugs (commonly referred to as in vitro plugs) as used herein are generally relatively small shaped bodies composed of a growth medium that serve for the cultivation and propagation of plants in a very early developmental stage. Plant plugs generally have a consistency which allows a manual or machine transfer of the plugs into other cultivation vessels or transport or processing units. Owing to their small size and transferability, plant plugs can be suitable for medium- and high-throughput methods in plant cultivation and can also be used for the space-saving transport of plants in an early developmental stage.
[0085] Polysaccharide as used herein, means a carbohydrate (e.g. starch, cellulose, or glycogen) whose molecules consist of a number of sugar molecules bonded together. Polysaccharides include gellan.
[0086] As used herein soil means either man-made or naturally occurring unconsolidated mineral or organic material on the immediate surface of the Earth that serves as a natural medium for the growth of land plants. Soil used for indoor growing is generally sterilized and devoid of added living biologic material.
[0087] Springiness is s the rate at which a deformed material goes back to its undeformed condition after deforming force is removed. It is a measurement of elastic recovery and has a unit of percent (%).
[0088] Water includes purified, distilled and reverse osmosis (RO) water, which may be charged as in some preferred embodiments of the present disclosure.
[0089] All publications and patent applications mentioned in this specification are herein incorporated by reference to the same extent as if each individual publication or patent application was specifically and individually indicated to be incorporated by reference.
[0090] No admission is made that any reference constitutes prior art. The discussion of the references states what their authors assert, and the applicants reserve the right to challenge the accuracy and pertinence of the cited documents. It will be clearly understood that, although a number of prior art publications are referred to herein, this reference does not constitute an admission that any of these documents forms part of the common general knowledge in the art.
[0091] The discussion of the general methods given herein is intended for illustrative purposes only. Other alternative methods and embodiments will be apparent to those of skill in the art upon review of this disclosure
[0092] As shown in
[0093] As shown in
[0094]
[0095]
TABLE-US-00001 TABLE 1 varieties of lettuce grown on the horticultural hydrogels and other substrates using various watering. Average Wet Weight and Standard Deviation (g) Version Lot Species Days Watering HYPERroots Rockwool Peat Coir Ihort 2.0 HYP- Fairly 14 E&F 1.05 4.67 0.56 2.67 0.62 2.47 0.55 1.82 1768 Lettuce 39 22 17 18 6 13 7 11 3 2.0 HYP- Five 14 E&F 0.25 0.1 0.2 0.8 0.21 0.79 1769 Star Lettuce 25 1.3 0.73 0.8 2.0 HYP- Crunchy 14 NFT 58.4 89.74 34.9 73.05 35.01 65.5 1770 Lettuce 38 192 32 178 45 132 61 2.0 HYP- Fairly 14 Misted 0.81 0.23 0.1 0.04 0.3 0.09 0.32 0.11 1773 Lettuce 2.0 HYP- Aroma 2 14 Zip 0.18 0.55 0.06 0.15 0.07 0.1 0.06 0.15 1777 (basil) Towers 32 2.74 0.72 0.49 0.71 2.0 HYP- Mizuna 14 Zip 0.44 0.55 0.15 0.49 0.18 0.41 0.19 0.48 1778 Towers 21 2.77 2.41 2.73 1.31 2.97 1.44 3.02 0.98 2.0 HYP- Fairly 13 NFT 135.6 20.3 40.9 8.2 123 22.6 64 19.1 1787 Lettuce 2.0 HYP- Fairly 13 DWC 92.6 23.9 30.2 9.5 79 29.4 53.5 15.7 1788 Lettuce 2.0 HYP- Fairly 13 DWC 90.6 24 25.7 7.3 69 16.8 40.5 7.9 1789 Lettuce 2.1 HYP- Fairly 43 Zip 55 17.97 43 15.5 41 16.87 1806 Lettuce Towers 38 DWC 68.4 29.9 48.8 22.2 62.5 31.5 36 NFT 112.1 27.06 68.2 24.5 91.4 27.64 2.1 HYP- Fairly 36 DWC 100.5 21.88 60.4 24.7 77.8 25.22 1809 Lettuce 36 100.8 23.41 52.7 21.4 82 23.76 Note, the first column indicates the lot of HYPERroots used. Plants grown on other substrates (e.g., Rockwool, Peat, Coir, or Ihort) did not include any horticultural hydrogel in the substrate.
TABLE-US-00002 TABLE 2 varieties of basil were grown on various substrates for 20 days, and their biomass was then taken. Average Wet Weight and Standard Deviation (g) Version Lot Species Days Watering HYPERroots Rockwool Jiffy Ihort 2.2 HCT-12 Basil- 28 NFT 18.6 1.64 10.6 5.95 8.8 7.94 10.1 3.09 Aroma 2 2.2 HCT-13 Basil- 35 NFT 7 1.06 2.8 0.35 1.8 1.8 3.8 0.95 Amethyst 2.2 HCT-14 Basil- 35 NFT 20.5 2.88 9.9 1.56 4.1 4.85 8.4 2.6 Emily 2.2 HCT-15 Basil- 35 NFT 19.3 6.88 9.2 1.29 10 7.93 7.3 1.67 Sweet Thai 2.2 HCT-16 Basil- 35 NFT 22.3 5.39 9.8 3.32 7.1 10.7 10.1 2.2 Genovese
[0096] Table 3 is data from lettuces and kales with DWC watering on various substrates.
TABLE-US-00003 Average Wet Weight and Standard Deviation (g) Version Lot Species Days Watering HYPERroots Rockwool Jiffy Ihort 2.2 HCT-8 Green 40 DWC 102.71 25.1 32.92 10.5 48.64 14 50.77 8.6 Oakleaf 2.2 HCT-9 Fairly 34 DWC 90.63 22.59 47 14.4 51.67 5.16 62.14 9.06 Lettuce 2.2 HCT-10 Red Butter 34 DWC 53.75 20.83 14 8.25 28.75 11.57 45 8.66 2.2 HCT-11 Chicarita 34 DWC 89.57 24.3 10.71 13.05 21.67 14.43 71.92 16.68 RZ 2.2 HCT-17 Red 34 DWC 150 48.18 16.36 8.39 20 30.55 75.63 18.41 Russian Kale 2.2 HCT-18 Lacinato 35 DWC 47.5 29.64 11.88 0.04 13.13 12.23 35 32.18 Kale 2.2 HCT-19 Scarlet 35 DWC 54.38 28.84 18.75 5.18 18.75 6.41 23.33 8.66 Kale 2.2 HCT-20 Toscano 35 DWC 60 17.73 11.67 7.53 38.13 17.1 46.88 13.35 Kale 2.2 HCT-21 Leaf 35 DWC 99.38 34.99 12.5 9.64 19.29 12.05 41.67 18.87 Broccoli
[0097] Table 4 shows data from a variety of basils and sweet pepper as outlined in Example
TABLE-US-00004 Average Wet Weight and Standard Deviation (g) Version Lot Species Days Watering HYPERroots Rockwool Soil Ihort 2.1 HYP-1824 King Arthur Bell 92 E&F 768 92.97 na na 574 73.8 na na Pepper 2.2 HCT-105 Genovese Basil 21 Hand 0.33 0.16 0.17 0.06 0.05 0.04 0.19 0.06 2.2 HCT-106 Sweet Thai Basil 21 Hand 0.2 0.08 0.18 0.05 0.27 0.09 0.14 0.05 2.2 HCT-107 Lemon Basil 21 Hand 0.61 0.29 0.33 0.1 0.48 0.15 0.28 0.08 2.2 HCT-108 Cinnamon Basil 21 Hand 0.38 0.22 0.28 0.09 0.07 0.08 0.27 0.09
[0098] Table 5 shows data from various leafy plants with watering conditions and varying substrates.
TABLE-US-00005 Average Wet Weight and Standard Deviation (g) Version Lot Species Days Watering HYPERroots HYPERroots LF Rockwool JIffy Ihort 2.2 HCT-90 Cedar 31 DWC 108 14 na na 100 15 112 17 90 16 2.2 HCT-90 Dunand 31 DWC 36 16 na na 31 13 31 13 32 8 2.2 HCT-90 Skyphos 31 DWC 50 6 na na 64 14 66 9 57 9 2.2 HCT-90 Bughatti 31 DWC 69 10 na na 55 12 73 10 58 11 2.2 HCT-87 Monte 26 DWC na na 28.8 8.2 30.6 5.2 22.4 5.3 28.4 6.5 Carlo Romaine 2.2 HCT-89 Rainbow 26 DWC na na 22 6.5 14.8 5.7 18.1 9.6 32.4 13.2 Chard 2.2 HCT-82-2 Five 27 DWC na na 26 4.7 23 6.5 15.9 3.4 29.6 6.5 Star Lettuce
Composition of the Disclosure
Examples
Example 1: Horticultural Hydrogels
Horticultural Hydrogels Supporting Increased Biomass
[0099] The following components were used to make a plurality of horticultural hydrogels:
TABLE-US-00006 RO RICO Carbon Water 8800 Black Fertilizer (Salt) 1687-1 1970 g 23 g 2 g 4 g M&S 1687-2 1970 g 23 g 2 g 4 g Miracle-Gro Water soluble Plant Food Vegetable & Herbs 1687-3 1970 g 23 g 2 g 4 g Haifa Ca(NO.sub.3).sub.2 + 1 mL/L FloraMicro 1687-4 1970 g 23 g 2 g 4 g Yara Ca(NO.sub.3).sub.2 + 1 mL/L FloraMicro 1687-5 1970 g 23 g 2 g 7 mL/L Clonex 1687-6 1970 g 23 g 2 g 1.3 mL/L Dyna-Gro
[0100] RO water was stirred at 500 rpm and solid ingredients were added. Liquid ingredients were then added. The mixture was heated to 85? C. and cooled to 60? C. before being poured into gel plug molds. The resulting hydrogels were tested for cohesiveness, hardness, and springiness.
TABLE-US-00007 Cohesiveness Hardness Springiness EC (%) (g/cm2) (%) pH (mS/cm) 1687-1 77.1 477.83 100 7.0 3.28 1687-2 84.52 221.24 100 7.8 4.88 1687-3 63.31 876.25 100 8.5 4.85 1687-4 62.99 883.48 100 8.7 4.57 1687-5 83.67 325.40 100 8.5 3.62 1687-6 85.83 231.09 100 8.1 3.56
[0101] Lettuce seeds were planted after the hydrogel had become solid and harvested at day 14. The total plant mass was then taken. Controls were plants grown in peat and coir under the same conditions.
TABLE-US-00008 Average Mass (g) Total Plant Mass (g) 1687-1 1.035245906 24.4381 1687-2 1.161994568 26.1991 1687-3 1.43010119 39.86597 1687-4 1.581263823 40.4764 1687-5 1.450607318 36.8462 1687-6 1.455981413 35.258
Example 2: Varying Carrageenan, Carbon, Fertilizer in the Hydrogel
[0102] JMP software was used to design a set of experiments to improve the formulation of Ricogel 81137 for plant growth, as 81137 has been shown to work more effectively than competitors in growing some leafy greens. JMP recommended 15 experiments that were run to optimize the 5 ingredients: water, carrageenan, carbon, calcium citrate, and M&S.
[0103] These are the amounts in grams required for ingredients in the 15 batches of gel, assuming that the total mass of each will be 2000 g:
TABLE-US-00009 Water Ricogel Carbon M&S Calcium Batch (g) (g) (g) (g) Citrate (g) Code 1962 20 2 8 8 HYP-1679-1 1960 34 2 4 0 HYP-1679-2 1960 20 8 4 8 HYP-1679-3 1964 20 8 8 0 HYP-1679-4 1962 20 2 8 8 HYP-1679-5 1974 20 2 4 0 HYP-1679-6 1960 22 2 8 8 HYP-1679-7 1960 20 8 4 8 HYP-1679-8 1960 24 8 8 0 HYP-1679-9 1960 34 2 4 0 HYP-1679-10 1974 20 2 4 0 HYP-1679-11 1974 20 2 4 0 HYP-1679-12 1960 20 8 4 8 HYP-1679-13 1964 20 8 8 0 HYP-1679-14 1960 34 2 4 0 HYP-1679-15 1979 18 1 2 0 HYP-1679-16 1979 18 1 2 0 HYP-1679-17 1979 18 1 2 0 HYP-1679-18 1971 24 3 2 0 HYP-1679-21
[0104] Each batch was made by the following process: charge water, initiate stirring, charge solid ingredients. Water and solid ingredients were mixed and heated to 85? C. then cooled to less than 70? C. and poured into gel plug molds. The Ricogel used was a uniform sample of 10 lots of 81137.
[0105] Samples were tested for cohesiveness (%), hardness (g), springiness (%). pH and EC (mS/cm).
The Results are Below:
[0106]
TABLE-US-00010 Name Cohesiveness (%) Hardness(g) Springiness (%) HYP-1661 73.38 755.29 100 HYP-1679-1 69.39 524.44 100 HYP-1679-2 76.79 897.54 100 HYP-1679-3 70.07 415.9 100 HYP-1679-4 68.81 507.11 100 HYP-1679-5 67.2 570.31 100 HYP-1679-6 75.86 317.74 100 HYP-1679-7 66.3 708.61 100 HYP-1679-8 71.88 485.94 100 HYP-1679-9 70.18 608.93 100 HYP-1679-10 75.05 1138.34 100 HYP-1679-11 74.39 398.4 100 HYP-1679-12 74.79 412.37 100 HYP-1679-13 69 478.8 100 HYP-1679-14 68.81 589.3 100 HYP-1679-15 76.59 783.83 100 HYP-1679-16 81.5 196.75 100 HYP-1679-17 Data not taken, Data not taken, Data not taken, too soft too soft too soft HYP-1679-18 82.99 184.2 100 HYP-1679-21 80.81 348.49 100
TABLE-US-00011 Name pH EC (mS/cm) HYP-1661 6.8 7.34 HYP-1679-1 6.4 6.15 HYP-1679-2 6.1 4.71 HYP-1679-3 6 4.09 HYP-1679-4 5.8 7.21 HYP-1679-5 6.2 7.27 HYP-1679-6 6.4 4.65 HYP-1679-7 6.5 6.85 HYP-1679-8 6.1 3.87 HYP-1679-9 5.8 6.38 HYP-1679-10 6.8 4.84 HYP-1679-11 6.6 3.99 HYP-1679-12 6.4 3.26 HYP-1679-13 6.1 5.22 HYP-1679-14 5.8 7.15 HYP-1679-15 6.3 5.11 HYP-1679-16 Data not taken Data not taken HYP-1679-17 7.5 Data not taken HYP-1679-18 7.2 2.29 HYP-1679-21 8.2 2.67
[0107] Samples were observed for dehydration seven (7) days after pouring by visualization and clear shrinkage of the plug where the hydrogel no longer fills the plug receptacle.
TABLE-US-00012 Total Total Total Edge Total Plugs Edge Plugs Name Plugs Dehydrated Plugs Dehydrated HYP-1661 50 43 26 24 HYP-1679-1 100 52 36 28 HYP-1679-2 100 65 36 33 HYP-1679-3 100 40 36 19 HYP-1679-4 100 24 36 18 HYP-1679-5 100 38 36 16 HYP-1679-6 100 9 36 3 HYP-1679-7 100 63 36 29 HYP-1679-8 100 23 36 15 HYP-1679-9 100 51 36 26 HYP-1679-10 100 78 36 35 HYP-1679-11 100 41 36 20 HYP-1679-12 100 20 36 12 HYP-1679-13 100 20 36 8 HYP-1679-14 100 81 36 33 HYP-1679-15 100 25 36 15 HYP-1679-16 100 Missed count 36 Missed count HYP-1679-17 100 Missed count 36 Missed count HYP-1679-18 100 42 36 Missed count HYP-1679-21 100 69 36 Missed count
Example 3: Germination and Biomass Measurements of the Hydrogel Recipe for 1689
[0108] 98 L of water was added to a 100 L glass jacketed reactor. The temperature of the jacket was adjusted to 50? C. Ricogel 8800 (1.15 kg) was charged to the reactor. Dialysis was initiated. This was continued for 72 hours. To this mixture was added M&S (200 g) and carbon black (400 g). The mixture was warmed to 85? C. The mixture was cooled to less than 70? C. The mixture was trayed and tested for plant growth. Various seeds were planted. Control groups of seeds planted in coir or peat were also used. When tested hydrogels had a hardness of 360.42, cohesiveness of 80.64, and springiness of 100.
[0109] Notably, after fourteen (14) days of plant growth there were no visible signs of dehydration (see below). The hydrogel plugs were easily transferable to a zip tower for further growth.
[0110] The following are results of the germination and growth of Butter Lettuce:
TABLE-US-00013 Confluence Graph Seeds Code Titles Planted Germination Successful % Germ % Healthy HYP-1689 Tray 1 40 39 38 97.50% 95.00% HYP-1689 Tray 2 40 40 40 100.00% 100.00% HYP-1689 Tray 3 40 40 39 100.00% 97.50% Coir Coir 40 39 21 97.50% 52.50% Peat Peat 20 16 16 80.00% 80.00%
[0111] The following table represents results for the growth of Kale
TABLE-US-00014 Confluence Graph Seeds Code Titles Planted Germination Successful % Germ % Healthy HYP-1689 Tray 1 40 34 30 85.00% 75.00% HYP-1689 Tray 2 40 33 32 82.50% 80.00% HYP-1689 Tray 3 40 29 28 72.50% 70.00% Coir Coir 30 11 9 36.67% 30.00% Peat Peat 20 17 15 85.00% 75.00% HYP-1689 HYP-1689 HYP-1689 Coir Peat Tray 1 Tray 2 Tray 3 Coir Peat Avg. Wet 0.5106 0.603314286 0.673285714 0.322018182 0.654205882 Weight STDEV 0.265696544 0.284583187 0.285486826 0.116675917 0.308565276 Total Weight 16.8498 21.116 18.852 3.5422 11.1215
Example 4: Horticultural Hydrogel Formulations in Spinach with Improved Germination Rates
[0112] The following ingredients were in all formulations:
TABLE-US-00015 Component Amount RO Water 1970 g RICO 8800 23 g Activated Carbon 2 g
[0113] The following formulations also contained: [0114] HYP-1687-1-(4 g) Standard M&S [0115] HYP-1687-2-(4 g) Miracle-Gro-Water soluble Plant Food Vegetable & Herbs HYP-1687-3-(4 g) Haifa Ca(NO.sub.3).sub.2+1 mL/L FloraMicro [0116] HYP-1687-4-(4 g) Yara brand Ca(NO.sub.3).sub.2+1 mL/L FloraMicro HYP-1687-5-Clonex 7 mL/L [0117] HYP-1687-6-Dyna-Gro 1.3 mL/L
[0118] The following procedure was used for each test. Added charged water into 5000 mL beaker. Initiated stirring at 500 rpm. Added the solid ingredients into a beaker and mixed together. Added solid ingredients to beaker. Added liquid ingredients into beaker, if applicable. Heated to 85? C. Cooled to 60? C. Poured into gel plug molds.
[0119] The formulations had the following properties:
TABLE-US-00016 Cohesiveness Hardness Springiness EC Formulation (%) (g) (%) pH (mS/cm) HYP-1687-1 77.91 477.83 100 7.0 3.28 HYP-1687-2 84.52 221.24 100 7.8 4.88 HYP-1687-3 63.31 876.25 100 8.5 4.85 HYP-1687-4 62.99 325.40 100 8.7 4.57 HYP-1687-5 83.67 325.40 100 8.5 3.62 HYP-1687-6 85.83 231.09 100 8.1 3.56
[0120] Germination rate exceeded 95% which is above the expected 80% in other substrate media.
Example 5: V 2.0 14 mL Plugs (HYP-1773)
Procedure
[0121] Charged water into 100 L glass, jacketed reactor. Initiated stirring at 100 rpm. Added the ingredients into a beaker and added to reactor. Increased agitation to 400 rpm. Waited until the mixture was homogeneous (2-5 minutes). Reduced agitation to 150 rpm. Heated to 85? C. Held at 85? C.+/?3 C for 30 minutes. Cooled to less than 70? C. Poured into 14 mL trays.
TABLE-US-00017 Component Lot Amount RO Water 24550 g Ricogel 8800 220515K 300 g Activation Carbon GCC-HH3401 75 g Haifa Ca(NO.sub.3).sub.2 435572396 62.5 g FloraMicro 12.5 g Cohesiveness Hardness Springiness EC Name (%) (g) (%) pH (mS/cm) HYP-1773 85.29 254.14 100 6.94 3.65
Example 6: V 2.1 100 L (HYP-1802)
Procedure
[0122] Charged water into 100 L reactor. Initiated stirring at 400 rpm. Added formulation ingredients. FloraPro was ground up with a mortar and pestle to ensure it was homogeneous. Reduced stirring to 200 rpm. Heated to 85? C. Held for 30 minutes. Cooled to 55? C. and poured into 14 mL gel molds.
TABLE-US-00018 Component Amount RO Water 98167 g Ricogel8800 1200 g Activated Carbon 300 g Haifa Ca(NO.sub.3).sub.2 250 g FloraPro 66 g Cohesiveness Hardness Springiness EC Name (%) (g) (%) pH (mS/cm) HYP-1803 77.36 260.69 100 6.54 6.61
Example 7: V 2.2 20 Tray Batch (HYP-1871)
Procedure
[0123] Changed water heater to Very hot an hour prior to beginning experiment. Charged water into 100 L glass, jacketed reactor. Set temperature to 125? C. Initiated stirring at 200 rpm. Added ingredients to reactor at 70? C. Decreased stirring to 100 RPM after 5-10 minutes. Turned jacket to 75? C. once 83? C. was reached to hold at 83? C.-85? C.+/?3 C for about 30 minutes. Cooled to 65? C. (+/?) 5? C. Poured into 14 mL trays.
TABLE-US-00019 Component Lot Amount RO Water 58900 g Ricogel8800 220507E 720 g Activation Carbon GCC-HH3401-1 180 g Haifa Ca(NO.sub.3).sub.2 435572396 150 g FloraPro 39 g Microcrystalline Cellulose 18 g Cohesiveness Hardness Springiness EC Name (%) (g) (%) pH (mS/cm) HYP-1871 79.17 238.03 100 6.98 5.73
Example 8: Horticultural Hydrogel Formulations
V2.2 Manufacturing for 100 L Batch
Ingredients
[0124]
TABLE-US-00020 Product Name Chemical Name Amount Ricogel8800 K-Carrageenan 1,200 g WDC Activated Carbon 300 g Haifa Cal GG Calcium Nitrate 250 g FloraPro Micronutrients 66 g Microcrystalline Cellulose 33 g RO Water 96.3 L
Procedure
[0125] Checked valves are closed, and hoses were properly connected on the USALabs 100 L reactor. In a beaker, added solid ingredients and mixed together. Checked that RO water tank light was on, then weighed water amount. Placed hose into RO water bucket and moved it into reactor via peristaltic pump in reverse. Initiated stirring at 400 RPM. Opened nitrogen tank valve and listened to the connected hose to ensure nitrogen was present and flowing. Removed the reactor's stopper with a hose and inserted funnel into the open neck. Added ingredients from beaker slowly via scooping or pouring. Once all ingredients were added, inserted the stopper with hose back into the open neck and glass lid. Closed/turned off nitrogen tank. Stirred at 400 RPM for 2-5 minutes. Powered on Heater/Chiller, selected Loop, Heat, and Cool. Set Heater/Chiller to 115? C.-135? C. Once mixture appeared homogenous, reduced stirring to 200 RPM. Closed jacket around reactor. At 82? C., adjusted Heater/Chiller to 85? C. Once 85? C. was reached, started timer for 30 minutes. After 30 minutes, decreased Heater/Chiller to 65? C. Once the mixture was 65? C. (+/?) 5?, opened the bottom valve and connected the dispensing hose to the connector. Placed hose nozzle to tray and turned pump on forward at the necessary speed to dispense. Squeegeed trays to smooth plugs. Added metal sheets or individual trays to the cold room for at least 30 minutes.
[0126] The horticultural hydrogels of this embodiment have the following specifications, two batches are provided, HYP-1881 and HYP-1891:
TABLE-US-00021 Specifica- HYP - HYP - Test Method tion 1881 1891 Appearance Inspection Black gel Black gel Black gel Hardness 10% compression ?150 g/cm.sup.2 261.93 282.06 TA Springiness 10% compression ?95.0% .sup.100% 96.58% TA Cohesive- 10% compression ?75.0% 82.91% 81.66% ness TA pH pH of gel SOP 6-8 6.42 6.64 EC EC of gel SOP 4-8 mS/cm 6.59 6.54
Example 9: HYP-1915 Cold Quench in Field Reactor V2.2 HYPERROOTS
Procedure
[0127] Set water heater to very hot for at least 30 minutes. Initiated stirring at 10. Added 134 kg heated, charged water to field reactor. Set temperature of jacket to 105? C. overnight and stirring at 30 rpm. Increased temperature to 165? C. the following morning to increase temperature of water from 74.5? C. up to 83? C.-85? C. Decreased temperature to 88? C. at 83? C. Added ingredients to reactor at 83? C. with stirring at 30 rpm. Increased stirring to 55-60 to remove clumps from behind baffles after about 30 minutes. Weighed 63 kg of room temperature water and dumped it in via water jugs. Cold quench dropped temperature from 83? C. to 65? C. Set jacket to 70? C. and decreased stirring to 30. Poured into: 200 cell?1.75, 288 cell, 1-inch deep trays, 50-cell, 10-200 cell, 6-288 cell, 50-cell, and a deep tray filled to an inch (for a thick mat) saved for Jonathan. Three trays placed in sealed plastic bag with nitrogen to test storing in wrapped condition.
TABLE-US-00022 Component Amount RO Water 197000 g Ricogel8800 2400 g Haifa Ca(NO.sub.3).sub.2 500 g Activation Carbon 600 g Microcrystalline Cellulose 60 g FloraPro 132 g Cohesiveness Hardness Springiness EC Name (%) (g) (%) pH (mS/cm) HYP-1915 85.09 249.07 97.26 6.79 6.67
Example 10: 50 L Batch of V2.2
Ingredients
[0128]
TABLE-US-00023 Component Lot # Amount RO Water 49,080 g Ricogel8800 220712F 600 g Activated Carbon GCC-HH3401-1 150 g Haifa 435572396 125 g FloraPro 33 g Microcrystalline Cellulose Fisher - A0443067 15 g
[0129] Changed water heater to Very hot 30 minutes to an hour prior to beginning experiment. Then charged water into 100 L glass, jacketed reactor. Set temperature to 125? C., and initiated stirring at 350 rpm. Added ingredients to reactor and decreased stirring to 200 RPM after 5-10 minutes. Turned jacket to 95? C. once 83? C. was reached to hold at 83? C. to 88? C.+/?3 C for about 30 minutes. Decreased temperature to 65? C. and stirring to 100 RPM. Poured into two 288-cell trays and the rest as standard once 65+/?5? C. was reached. Gels had a cohesiveness of 80.26%, hardness of 282.02 g, springiness of 96.03%, pH of 6.81, and electroconductivity of 6.94 mS/cm.
Example 11: 100 L Batch Loose Fill Horticultural Hydrogels
SOP: HYPERROOTS LF V1.0 Manufacturing for 100 L Batch
Ingredients
[0130]
TABLE-US-00024 Product Name Chemical Name Amount Manufacturer Ricogel8800 K-Carrageenan 2500 g W Hydrocolloids WDC Activated Carbon 600 g General Carbon Haifa Cal GG Calcium Nitrate 400 g Haifa Group FloraPro Micronutrients 100 g General Hydroponics Microcrystalline 20 g Thermo Scientific Cellulose RO Water 96.4 L In house
Procedure
[0131] Checked valves are closed, and hoses were properly connected on the USALabs 100 L reactor. In a beaker, added solid ingredients and mixed. Checked that RO water tank light was on, then weighed water amount. Placed the hose into the RO water bucket and moved it into the reactor via the peristaltic pump in reverse. Initiated stirring at 400 RPM. Opened nitrogen tank valve and listened to the connected hose to ensure nitrogen was present and flowing. Removed the reactor's stopper with a hose and inserted funnel into the open neck. Added ingredients from beaker slowly via scooping or pouring. Once all ingredients were added, inserted the stopper with hose back into the open neck in glass lid. Closed/turned off nitrogen tank. Stirred at 400 RPM for 2-5 minutes. Powered on Heater/Chiller, selected Loop, Heat, and Cool. Set Heater/Chiller to 115?-135? C. Once mixture appeared homogenous, reduced stirring to 200 RPM. If clumps persisted, pulsed 400 RPM stirring multiple times. Closed jacket around reactor. At 82?, adjusted Heater/Chiller to 89?. Once 83? C. is reached, started timer for 30 minutes. After 30 minutes, decreased Heater/Chiller to 65? C. Once the mixture is 65? C. (+/?) 5?, opened the bottom valve and connected the dispensing hose to the connector. Placed hose nozzle to tray and turned pump on forward at the necessary speed to begin dispensing. Squeegeed trays to smooth plugs. Added metal sheets or individual trays to the cold room for at least 30 minutes. Cut plugs into sizes appropriate for the loose-fill application.
Example 12: Increased in Biomass for Plants Grown in the Horticultural Hydrogel-Bell Peppers
[0132] Plants were allowed to grow naturally with no cultivation methods applied. This was done to see how vigorous the plants were without any other factors added in. Plants propagated in HYPERroots grew larger from the start, getting a week increase in flower formation, then leading to earlier harvest. No negative growth was noticed in plants propagation in HYPERroots. At end of trial plants propagated in HYPERroots produced more fruit and a week quicker than the control in same conditions.
TABLE-US-00025 HYPERroots Soil Total Weight of Fruit 2303.6 1720.7 Average Weight of Fruit 69.80606061 63.72962963 Number of Fruits 33 27 Fruits Per Plant 11 9 Weight of Fruit Per Plant 767.8666667 573.5666667 % Extra Total Weight of Fruit 34% % Extra Average Weight of Fruit 10% % Extra Number of Fruits 22% % Extra Fruits Per Plant 22%
Example 13: Hydrogels for Woody Plant Cultivation Ingredients
[0133]
TABLE-US-00026 Component Amount RO Water 97,385 Ricogel8800 (220507E) 2,000 g Activated Carbon 300 g Haifa Ca(NO.sub.3).sub.2 250 g FloraPro 66 g
Protocol
[0134] 100 L batch of 2% gel poured in 288-cell, sheets, and 200-cell trays that are to be frozen, thawed and used to test woody plant growth. Changed water heater to Very hot 30 minutes to an hour prior to beginning experiment. Charged water into 100 L glass, jacketed reactor. Set temperature to 125? C. Initiated stirring at 120 rpm. Added ingredients to reactor at 82? C. Increased stirring to 350 RPM after 10 minutes and had to pivot the baffle to release large clump around impeller. Decreased stirring to 150 RPM. Turned jacket to 87? C. once 85? C. was reached to hold at 83-85? C.+/?3 C for about 30 minutes. Turned stirring down to 100 RPM after heating and holding cycle. Cooled to 65? C. (+/?) 5? C. Poured into 288 cell trays, sheets, and 200-cell to be frozen, thawed and used as loose fill for woody plant growth studies.
[0135] The hydrogel pellets of this test had 84.93% cohesiveness, 583.75 g hardness, 100% springiness, pH of 6.71 and 8.07 mS/cm electroconductivity.
Example 14: Hydrogel Formulations for Mushroom Cultivation
[0136]
TABLE-US-00027 Component 1875-1 1875-2 1875-3 1875-4 1875-5 RO water 2921 g 2927 g 2912 g 2905 g 2902 g Ricogel 8800 60 g 60 g 75 g 75 g 75 g Micro- 10 g 10 g 10 g crystalline Cellulose Chitosan 3 g 3 g 3 g Haifa 7.5 g 7.5 g 7.5 g 7.5 g 7.5 g Ca(NO.sub.3).sub.2 FloraPro 2 g 2 g 2 g 2 g 2 g
Procedure
[0137] Charged water into 5 L reactor. Initiated stirring at 400 rpm. Added formulation ingredients. Reduced stirring to 200 rpm. Heated to 85? C. Held for 30 minutes. Cooled to 60? C.+/?5 and poured into 14 mL gel molds to be placed in the cold room. Place in pressure cooker for 30 minutes at 15 psi before inoculation.
Results
[0138]
TABLE-US-00028 Cohesive- Hardness Springiness EC Name ness (%) (g) (%) pH (mS/cm) HYP-1875-1 85.95 557.93 100 7.84 7.19 HYP-1875-2 86.32 535.78 100 8.18 7.65 HYP-1875-3 86.74 816.28 100 8.20 7.83 HYP-1875-4 87.19 738.85 100 8.47 7.85 HYP-1875-5 85.87 846.54 100 8.44 8.29
Example 15: Organic Horticultural Hydrogels
[0139] The following process was followed: Charged water into 5 L reactor, initiated stirring at 400 rpm, added formulation ingredients, reduced stirring to 200 rpm, heated to 85? C., held for 30 minutes, cooled to 55? C., and poured into 14 mL gel molds.
TABLE-US-00029 HYP-1798-1 HYP-1798-2 Component HYP-1775-1 HYP-1775-2 HYP-1775-7 (triplicate) (triplicate) RO Water 2946 g 2946 g 2906 g 2901 g 2910 g Ricogel8800 36 g 36 g 45 g 45 g 45 g Activated 9 g 9 g 9 g 18 g 18 g Carbon Acadian 9 g 9 g 6 g 6 g Root Rocket 9 g Cal-Mag 31 g 30 g 21 g
Properties
[0140]
TABLE-US-00030 Cohesive- Hardness Springiness EC Name ness (%) (g) (%) pH (mS/cm) HYP-1775-1 94.31 37.87 100 6.45 3.02 HYP-1775-2 93.49 42.90 100 7.15 3.00 HYP-1775-7 84.33 340.36 100 5.75 4.21 HYP-1798-1-1 89.12 200.89 100 5.21 5.60 HYP-1798-1-2 90.35 190.37 100 5.20 5.56 HYP-1798-1-3 89.85 191.82 100 5.20 5.93 HYP-1798-2-1 91.27 144.40 100 5.31 4.93 HYP-1798-2-2 91.61 156.08 100 5.30 4.96 HYP-1798-2-3 92.12 135.45 100 5.32 4.76
[0141] Other suitable organic formulations were made in large batches. The following process was followed.
Example 16: Liquid Formulations of the Horticultural Hydrogel
[0142] The following process was followed: ingredients added to a 5 L beaker, initiated stirring at 200 RPM, heated to 85? C., cooled to room temperature at 200 RPM, poured into labeled 1-gallon jug, and stored in refrigerator. The solutions were sprayed onto rock wool instead of a normal fertigation solution.
TABLE-US-00031 General Haifa FloraPro Carbon Cal Calcium + Microcrystaline RO Ricovis8870 WDC GG Micros Cellulose Name Water Mass Mass Mass Mass Mass HYP-1893-1 3987 4 4 20 .4 .4 HYP-1893-2 3932 4 20 4 4 4 HYP-1893-3 3987 4 4 4 .4 4 HYP-1893-4 3987 20 20 4 .4 4 HYP-1893-5 3960 10.95 12 10.86 2.2 2.2 HYP-1893-6 3960 10.95 12 10.86 2.2 2.2 HYP-1893-7 3932 4 4 20 .4 4 HYP-1893-8 3987 4 4 4 4 .4 HYP-1893-9 3987 20 4 4 4 4 HYP-1893-10 3987 4 20 20 4 .4 HYP-1893-11 3932 4 20 4 .4 .4 HYP-1893-12 3932 20 4 4 4 .4 HYP-1893-13 3987 10 4 20 4 4 HYP-1893-14 3987 20 20 10 .4 .4 HYP-1893-15 3932 20 4 10 .4 .4 HYP-1893-16 3932 10 20 20 4 4
Example 17: Specifications for K-Carrageenan
[0143]
TABLE-US-00032 Test Method Specification Appearance Inspection Creamy white powder to light tan Mesh Size, <80 mesh C of A >95.0% pH 1.5% aqueous at 7-10 60? C. Potassium gel strength 1.0% gel with 0.2% K >45 g/cm2 Total Plate Count ACTA labs method <50,000 CFU/g Yeast and Molds ACTA labs method <100 CFU/g Salmonella C of A Absent in 10 g E. coli C of A Absent in 5 g Coliform C of A <10 CFU/g L. monocytogenes C of A Absent in 25 g S. aureus C of A Absent in 25 g SEC HPLC ACTA labs method Peak at 1 RRT >50.0% Appearance of ACTA labs method Clear and colorless Solution
Compliant Products
[0144]
TABLE-US-00033 Vendor Product Part Number W Hydrocolloids K-carrageenan Ricogel 8800 W Hydrocolloids K-carrageenan Ricogel 81137 W Hydrocolloids K-carrageenan Ricogel 88128 Marcel K-carrageenan GU-9303
Example 18: Taking Hardness Measurements
[0145] Measurements were taken using a Stable Micro Systems TA.XT ExpressC Texture Analyzer (TA). The TA was powered on and calibrated with a 2000 g weight for weight and for height. The following measurements were measured: distance (mm), force (g), time (sec) and temperature (? F.). Pre-test speed was set to a compression value of 1.00 mm/sec, Test Speed was set to a compression value of 1.00 mm/sec, Post-test speed was set to a compression value of 2.00 mm/sec. Target mode Strain was set to 25.0% and a Count value of 2. Trigger Type of Force was set to a Trigger Force value of 5.0 g. Each hydrogel plug was placed directly underneath the TA probe and Start Test was selected. Up and Fast buttons were selected where the height needed to be adjusted to a higher setting to accommodate the plug. Three (3) plugs per recipe were tested. Results for absolute positive force, absolute positive distance, peak force, and positive area were collected. These parameters then can result in cohesiveness measurements (the hydrogel's ability to return to original height after compression), hardness (the maximum force of the gel), and springiness (tested twice with compressive force, Force2/Force1?100%).
[0146] The following Table shows the results for the HYP-1689 batch
TABLE-US-00034 Abs. Abs. Abs. Abs. (+) (+) (+) (+) Peak Peak (+) (+) Test Force Force Dist. Dist. Force Force Area Area Cohesiveness Springiness ID (Cycle: 1) (Cycle: 2) (Cycle: 1) (Cycle: 2) (Cycle: 1) (Cycle: 2) (Cycle: 1) (Cycle: 2) s (%) s (%) 363.4 348.5 363.4 348.5 1238. 993.4 1 31 41 12.86 12.86 31 41 541 25 360.9 346.4 12.81 12.81 360.9 346.4 1206. 990.7 2 24 26 5 5 24 26 967 01 362.6 348.5 12.78 12.78 362.6 348.5 1227. 991.4 3 81 04 5 5 81 04 357 02 354.2 338.2 12.83 12.83 354.2 338.2 1195. 961.1 4 42 74 3 3 42 74 327 67 360.8 344.4 12.78 12.78 360.8 344.4 1225. 976.9 5 24 55 5 5 24 55 045 3 HYP - 80.64 100.0 1689 % 0% 360.4 345.2 12.81 12.81 360.4 345.2 1218. 982.7 Avg: 21 4 6 6 21 4 647 25 17.26 13.70 S.D. 3.632 4.246 0.032 0.032 3.632 4.246 8 9 Coef. of Variation 1.008 1.23 0.251 0.251 1.008 1.23 1.417 1.395
Example 19: Taking PH and Electroconductivity (EC) Measurements
Taking the Electrical Conductivity (EC) and pH of a Gel Plug
[0147] pH was calibrated with known standards (4.01 and 7.00) in separate beakers. A temperature and pH probe were added to the one beaker and stirred gently until the pH meter was reached and leveled. The meter was thoroughly rinsed with RO water and repeated with the other standard in the other beaker.
[0148] The hydrogels were measured by pressing and mashing 5-6 hydrogel plugs in a bag. The temperature and pH probe were inserted into the bags containing the mashed plugs and were gently stirred until the indication sound on the pH meter was activated. pH was recorded and the meter was rinsed with RO water.
[0149] EC was measured using the same mashed plugs (5-6 hydrogel plug) by opening the EC probe program, adding the EC probe to the mashed plugs and ensuring gel was surrounding the electrodes and recording the measurement once leveled. The EC probe was then rinsed with RO water.
Example 20: Taking HS-GC Measurements
[0150] Headspace gas chromatography to confirm the absence of residual solvents in the starting kappa-carrageenan. Samples were tested using headspace GC and found that none of the samples contained any residual solvents. The total amount of volatiles was very low in the samples. Sometimes, hydrocarbons and siloxanes were observed. These could be classified as greases, probably from the machines used to press the carrageenan.
[0151] More particularly, polysaccharide samples were submitted as powders in plastic vials. The objective of the testing was to evaluate the samples for residual solvents. Direct Injection (DI)-Gass Chromatography/Mass Spectroscopy (GC/MS) were done.
[0152] The sample was placed into a tared 20 mL headspace vial and weighed. The vial was immediately sealed and placed onto an Agilent Technologies 7697A Headspace Sampler to outgas where the gasses within the headspace vial were analyzed using a Hewlett Packard 6890 Gas Chromatograph/5973 Mass Selective Detector.
[0153] A blank was analyzed prior to the sample analysis to ensure that the system did not contain any compounds of interest, which it did not.
[0154] An external standard (0.05 pL of isopropyl alcohol) was analyzed in duplicate following the sample analysis. The average response from the external standard injections was used to quantify the individual compounds identified in each sample.
[0155] The outgas temperature and time were 92? C. and one (1) hour with approximately 0.1 gram.
[0156] None of the samples exhibited any evidence of the presence of any kind of solvents. The total outgassing was really low and showed the presence of hydrocarbons and sometimes siloxanes. The complete results are listed in Table 1 included with this report. The compounds identified in each sample were quantified based on the average response of the two external standard (mixture) injections performed following the sample analysis.
[0157] The compounds seen in the blank are listed above the results. Those compounds that were seen in the blank are shown in bold in the sample table. Those compounds which had a response less than or equal to what was seen in the blank were denoted with an asterisk (*) and were NOT included in the totals.
[0158] The relative percent of each compound is listed along with the retention time, response, and match quality. The relative percent is computed by dividing the individual compound response by the total outgassing response for the sample and the resultant multiplied by one hundred (100).
[0159] A match quality was assigned to each compound identified in Table 1. The match quality indicates how well the unknown spectra match that of a reference library. Values in the 90's indicate a very reliable match, 80's and 70's can be considered a fair match while anything below that should be used more as a guide as to what type of compound the unknown is.
[0160] Upon further investigation of the mass spectra at each retention time it was noticed that some retention times appeared to contain two co-eluting compounds. Co-eluting compounds were italicized as mixtures in the sample table and if they contained a compound of interest the response for the mixture was included in totals for that category.
[0161] The search of the mass spectrum at some of the retention times resulted in no good matches. These compounds were identified as <unknown> in the table.
Sample Characterization
[0162]
TABLE-US-00035 Lot Type Jira # SRF-IS-22-3722-01 #1 Ricogel 81137 HYP-1677-2 SRF-IS-22-3722-01 #2 Ricogel 81137 HYP-1677-3 SRF-IS-22-3722-01 #3 Ricogel 81137 HYP-1677-4 SRF-IS-22-3722-01 #4 Ricogel 81137 HYP-1677-5 SRF-IS-22-3722-01 #5 Ricogel 81137 HYP-1677-6 SRF-IS-22-3722-01 #6 Ricogel 81137 HYP-1677-7 SRF-IS-22-3722-01 #7 Ricogel 81137 HYP-1677-8 SRF-IS-22-3722-01 #8 Ricogel 81137 HYP-1677-9 SRF-IS-22-3722-01 #9 Ricogel 81137 HYP-1677-10 SRF-IS-22-3722-01 #10 Ricogel 81137 HYP-1677-11 211012C Ricogel 8800 HYP-1677-1
Example 21: Karl Fisher Testing
Water Content of Starting Kappa Carrageenan
[0163] Karl Fischer Method of Moisture Determination for moisture in liquids, or small amounts of moisture in prepared solids.
[0164] The Water Determination Test (Karl Fischer Method) is designed to determine the moisture content in substances, utilizing the quantitative reaction of water with iodine and sulfur dioxide, in the presence of a lower alcohol such as methanol, and an organic base such as pyridine.
[0165] There are two different determination methods in the iodine-providing principle: the volumetric titration method and the coulometric titration method.
[0166] In the volumetric titration method, the iodine required for a reaction with water, is previously dissolved in water, and the moisture content in the sample is determined by measuring the amount of iodine consumed as a result of a reaction with water in the sample.
[0167] The apparatus for volumetric titrations, consists of an automatic burette, a back titration flask, a stirrer, and equipment for amperometric titration at constant voltage, or potentiometric titration at constant current.
[0168] The apparatus for coulometric titration is comprised of an electrolytic cell for iodine production, a stirrer, a titration flask, and a potentiometric titration system at constant current. The iodine production device is composed of an anode and a cathode, separated by a diaphragm. The anode is immersed in the analyte solution, and the cathode is immersed in the catholyte solution. Both electrodes are usually made of platinum-mesh. This volumetric technique involves dissolving the sample in a suitable solvent and adding measured quantities of a reagent.
[0169] In the coulometric titration method, first, iodine is produced by electrolysis of a reagent containing the iodide ion, and then, the moisture content in the sample is determined by measuring the quantity of electricity which is required for the electrolysis (i.e., for the production of iodine), based on the quantitative reaction of the generated iodine with water.
[0170] It will be understood that various details of the presently disclosed subject matter may be changed without departing from the scope of the presently disclosed subject matter. Furthermore, the foregoing description is for the purpose of illustration only, and not for the purpose of limitation.
[0171] All publications, patents, and patent applications cited in this specification are incorporated herein by reference for the teaching to which such citation is used.
[0172] Tested embodiments described herein represent exemplary embodiments.
[0173] The specific responses observed may vary according to and depending on the particular hydrogel formulation, as well as the type of formulation and mode of administration employed, and such expected variations or differences in the results are contemplated in accordance with practice of the present disclosure.
[0174] Although specific embodiments of the present disclosure are herein illustrated and described in detail, the disclosure is not limited thereto. The above detailed descriptions are provided as exemplary of the present disclosure and should not be construed as constituting any limitation of the disclosure. Modifications will be obvious to those skilled in the art, and all modifications that do not depart from the spirit of the disclosure are intended to be included with the scope of the appended claims.