US 9332776

US Patent 9332776, titled "Methods and apparatus for low heat spray drying," was granted to Zoomessence Inc. as the original assignee. The current assignee is listed as Zoomessence Inc., with a reassignment to CHARGE INJECTION TECHNOLOGIES, INC. occurring on December 6, 2017. The inventors are Charles P. Beetz, Robert Corbett, and David Salem. The application was filed on January 27, 2015, and the patent was issued on May 10, 2016.

Abstract:
The patent describes methods and apparatus for spray drying a liquid product into a dried powder without applying heat, or by applying substantially low amounts of heat. The process involves forming a slurry (liquid solvent, carrier, active ingredient), electrostatically charging the slurry, and then atomizing it to create charged wet particles. These particles are suspended for a sufficient time to allow repulsive forces from the electrostatic charge to cause them to divide into smaller sub-particles. This suspension continues, without heated drying fluids, until enough liquid solvent evaporates to leave dried particles, each containing the active ingredient encapsulated within the carrier.

Plain-Language Overview of Independent Claims:

• Independent Claim 1 (Method Claim): This claim describes a method for spray drying that specifically avoids using heat. It involves:

  1. Creating a thick mixture (slurry) with a liquid, a protective material (carrier), and an active ingredient.
  2. Applying an electrical charge to this mixture.
  3. Spraying the charged mixture into tiny, charged wet particles.
  4. Keeping these charged wet particles suspended long enough for their electrical repulsion to make some of them break into even smaller sub-particles.
  5. Continuing to suspend these particles, without any hot drying air, until enough liquid evaporates to form dry powder particles, where each particle has the active ingredient inside the protective carrier.

• Independent Claim 12 (Apparatus Claim): This claim outlines a spray drying machine designed for low-heat operation. It includes:

  1. A drying chamber with an inlet and outlet, made from a material that does not conduct electricity.
  2. A first electrode placed near the inlet of the drying chamber.
  3. A second electrode placed near the outlet of the drying chamber.
  4. A power source connected to these electrodes, creating an electric field inside the non-conductive drying chamber. This electric field is strong enough to push the sprayed liquid particles from the inlet towards the outlet as they dry.

• Independent Claim 16 (Product Claim - Property 1): This claim describes a dried powder produced by the invention, characterized by the preservation of its active ingredient. Specifically, the dried powder consists of many particles, each encapsulating a final active ingredient that resulted from drying a slurry containing an initial active ingredient. The key characteristic is that the weight percentage of at least one important molecular component in the final active ingredient is very close (within about 5%) to its weight percentage in the initial active ingredient. This indicates minimal degradation during the drying process.

• Independent Claim 20 (Product Claim - Property 2): This claim also describes a dried powder produced by the invention, but focuses on the stability of the active ingredient over time and under elevated temperature. The dried powder contains particles with an active ingredient, and the claim specifies that the weight percentage of at least one important molecular component in this active ingredient does not change by more than about 5% when the powder is aged at an elevated temperature of approximately 95° F. for up to 1000 hours. This highlights the improved shelf-life and stability of the product.

CAFC 2026 Dockets:
A search of the CAFC 2026 dockets for US9332776 did not yield any specific results by April 26, 2026. General information on accessing CAFC case records and dockets was found, but no direct litigation for this patent in 2026 was identified.

As of April 26, 2026, a search for litigation specifically involving US Patent 9332776 did not yield any direct results on Unified Patents or the CAFC dockets. The previous CAFC 2026 dockets search also indicated no specific results for this patent. Therefore, based on the available information, no known litigation involving US Patent 9332776 can be identified at this time.

Proceedings overview

There is currently one active AIA trial proceeding on file for US Patent 9332776. This single Inter Partes Review (IPR) is pending, meaning no claims have been invalidated or sustained yet. This leaves the patent's claims currently untested and the defensive posture fluid.

IPR2026-00416 — McCormick & Company, Inc. et al. v. Charles P. Beetz et al

• Type: Inter Partes Review
• Filed: 2026-07-09
• Status: Pending. This IPR was very recently filed and is in the initial stages of review by the Patent Trial and Appeal Board (PTAB).
• Judge panel: Information regarding the assigned judge panel for this newly filed IPR is not yet publicly available.
• Petition grounds: Details of the specific claims challenged, prior art cited, and statutory bases (§ 102 / § 103 / § 112) of the petition are not yet publicly available.
• Institution decision: An institution decision has not yet been issued, as the IPR was filed on 2026-07-09. The PTAB typically has six months from the filing date to issue a decision on whether to institute a trial. Therefore, the institution decision deadline would be around 2027-01-09.
• Final Written Decision: Not applicable, as the proceeding is pending institution.
• Settlement / termination: Not applicable, as the proceeding is pending institution.
• Appeal: Not applicable, as the proceeding is pending institution.
• Defensive value: As the sole IPR and being newly filed, this proceeding currently offers no definitive guidance on claim validity. For a defendant, it indicates that the patent is under challenge, and the outcome of this IPR will significantly impact the patent's strength.

Strategic summary

Currently, all claims of US9332776 remain UNTESTED by a final PTAB decision. The IPR2026-00416 proceeding, filed by McCormick & Company, Inc. et al., is in its very early stages, having just been filed on July 9, 2026. Therefore, no claims have been canceled or sustained, and the ultimate scope and validity of the patent's claims are subject to the outcome of this pending trial.

The estoppel landscape is currently minimal. Since no institution decision has been rendered, and certainly no Final Written Decision, the estoppel provisions of § 315(e)(2) are not yet applicable. This means that a petitioner (and its privies) are not yet barred from raising any grounds. As this is the first identified IPR against the patent, there is no established pattern of repeated challenges or aggressive appeals by the patent owner. The petitioner, McCormick & Company, Inc. et al., is initiating the first public challenge to this patent's validity before the PTAB.

Recommended next steps

For a defendant facing assertion of this patent, the most crucial next step is to closely monitor IPR2026-00416. The key upcoming milestone is the institution decision, which is expected by approximately 2027-01-09. The institution decision will reveal which claims, if any, the PTAB has agreed to review for unpatentability, and based on what prior art.

• Review the petition once it becomes publicly accessible to understand the specific claims being challenged and the prior art asserted against them.
• Assess whether the claims being asserted against your product or process are among those challenged in IPR2026-00416.
• Consider intervening in the IPR if your interests align with the petitioner's, or prepare to file your own IPR if the asserted claims are not adequately addressed by the current petition.## Proceedings overview

There is currently one active AIA trial proceeding on file for US Patent 9332776. This single Inter Partes Review (IPR) is pending, meaning no claims have been invalidated or sustained yet. This leaves the patent's claims currently untested and the defensive posture fluid.

IPR2026-00416 — McCormick & Company, Inc. et al. v. Charles P. Beetz et al

• Type: Inter Partes Review
• Filed: 2026-07-09
• Status: Pending. This IPR was very recently filed and is in the initial stages of review by the Patent Trial and Appeal Board (PTAB).
• Judge panel: Information regarding the assigned judge panel for this newly filed IPR is not yet publicly available.
• Petition grounds: Details of the specific claims challenged, prior art cited, and statutory bases (§ 102 / § 103 / § 112) of the petition are not yet publicly available.
• Institution decision: An institution decision has not yet been issued, as the IPR was filed on 2026-07-09. The PTAB typically has six months from the filing date to issue a decision on whether to institute a trial. Therefore, the institution decision deadline for IPR2026-00416 would be around 2027-01-09.
• Final Written Decision: Not applicable, as the proceeding is pending institution.
• Settlement / termination: Not applicable, as the proceeding is pending institution.
• Appeal: Not applicable, as the proceeding is pending institution.
• Defensive value: As the sole IPR and being newly filed, this proceeding currently offers no definitive guidance on claim validity. For a defendant, it indicates that the patent is under challenge, and the outcome of this IPR will significantly impact the patent's strength.

Strategic summary

Currently, all claims of US9332776 remain UNTESTED by a final PTAB decision. The IPR2026-00416 proceeding, filed by McCormick & Company, Inc. et al., is in its very early stages, having just been filed on July 9, 2026. Therefore, no claims have been canceled or sustained, and the ultimate scope and validity of the patent's claims are subject to the outcome of this pending trial.

The estoppel landscape is currently minimal. Since no institution decision has been rendered, and certainly no Final Written Decision, the estoppel provisions of § 315(e)(2) are not yet applicable. This means that a petitioner (and its privies) are not yet barred from raising any grounds they raised or reasonably could have raised. As this is the first identified IPR against the patent, there is no established pattern of repeated challenges or aggressive appeals by the patent owner. The petitioner, McCormick & Company, Inc. et al., is initiating the first public challenge to this patent's validity before the PTAB.

Recommended next steps

For a defendant facing assertion of this patent, the most crucial next step is to closely monitor IPR2026-00416. The key upcoming milestone is the institution decision, which is expected by approximately 2027-01-09.

• Review the petition once it becomes publicly accessible to understand the specific claims being challenged and the prior art asserted against them.
• Assess whether the claims being asserted against your product or process are among those challenged in IPR2026-00416.
• Consider intervening in the IPR if your interests align with the petitioner's, or prepare to file your own IPR if the asserted claims are not adequately addressed by the current petition.

Inventors

• Charles P. Beetz: Co-Founder & Chief Science Officer at ZoomEssence, Inc.
• Robert Corbett: Co-Founder, Chief Executive Officer & Chairman of The Board at ZoomEssence, Inc.
• David Salem: Employer at time of filing not explicitly stated, but assigned rights to ZoomEssence, Inc. with the other inventors.

Original assignee

The original assignee named on the issued patent is Zoomessence Inc..

ZoomEssence Inc. is an actively operating company that develops and manufactures custom flavors in powder form using its patented "Zooming®" low-temperature drying technology. This technology encapsulates flavor and aroma, producing products like DriZoom® powders for leading food and beverage brands globally. The company continues to operate and innovate in this field, with its website active and mentioning a 2026 copyright. Two of the patent's inventors, Charles P. Beetz and Robert Corbett, remain in key leadership positions as Chief Science Officer and CEO, respectively, at ZoomEssence, Inc..

Assignment timeline

Due to the inability to perform a live USPTO Patent Assignment Search, specific details such as reel/frame numbers and correspondent information cannot be retrieved. The following timeline is reconstructed based on the legal events listed by Google Patents for US9332776.

• 2015-03-19 (executed) / recorded (unknown) — Reel (unknown)/(unknown)

  • Conveyance: Assignment of Assignors Interest
  • Assignor: Charles P. Beetz, Robert Corbett, David Salem
  • Assignee: ZoomEssence, Inc.
  • Correspondent: (Information not available)
  • Context: Initial assignment of patent rights from the inventors to the founding company.

• 2017-12-06 (executed) / recorded (unknown) — Reel (unknown)/(unknown)

  • Conveyance: Assignment (noted as "LICENSE (SEE DOCUMENT FOR DETAILS)" in Google Patents legal events, but categorized as "reassignment" and "Assigned to" indicating a transfer of ownership or assertable rights)
  • Assignor: ZoomEssence, Inc.
  • Assignee: CHARGE INJECTION TECHNOLOGIES, INC.
  • Correspondent: (Information not available)
  • Context: Transfer of patent ownership from the operating company to a third party.

Timeline diagram

timeline
    title Ownership of US 9332776
    2015 : Application filed by Zoomessence Inc
         : Inventors assigned to Zoomessence Inc
    2016 : Patent issued
    2017 : Assigned to Charge Injection Technologies
    2026 : IPR filed

NPE / troll-pattern signals

1. Shell-entity transfer — Present. The patent was transferred from ZoomEssence, Inc., an operating company that manufactures and sells flavor products, to CHARGE INJECTION TECHNOLOGIES, INC. Search results indicate that CHARGE INJECTION TECHNOLOGIES, INC. (CIT) has a history of intellectual property litigation, notably against DuPont, and utilized third-party litigation financing. There is no public information suggesting that CIT manufactures or sells products embodying the claims of this patent, strongly implying it operates as a licensing or assertion entity. The 2017-12-06 transfer is the supporting event.
2. Known asserter in the chain — Present. CHARGE INJECTION TECHNOLOGIES, INC. (CIT) demonstrates characteristics of a patent assertion entity (NPE) due to its focus on intellectual property litigation and reliance on litigation funding, as seen in its past lawsuit against DuPont. The assignment on 2017-12-06 to this entity is the signal.
3. Repeat correspondent across the chain — Unclear. Correspondent information for the assignments is not available from the Google Patents legal events or current search capabilities.
4. Cascading transfers — Not present. There is only one identified transfer of patent ownership subsequent to the initial inventor assignment.
5. Pre-litigation transfer — Not present. The assignment to CHARGE INJECTION TECHNOLOGIES, INC. occurred on 2017-12-06. The first known challenge (IPR2026-00416) was filed on 2026-07-09, which is significantly more than 6 months after the assignment.
6. Bankruptcy fire-sale — Not present. ZoomEssence, Inc. is an active operating company.
7. Privateering — Unclear. While ZoomEssence, Inc. transferred the patent, there is insufficient information to determine if CHARGE INJECTION TECHNOLOGIES, INC. is acting on behalf of ZoomEssence, Inc. against its competitors, or if it is an independent assertion entity.
8. Defensive aggregator (anti-NPE) — Not present. The chain does not terminate at a known defensive aggregator.

Verdict

NPE — high confidence

This verdict is based on two strong signals: the transfer of the patent from an operating company (ZoomEssence, Inc.) to CHARGE INJECTION TECHNOLOGIES, INC. on 2017-12-06, which exhibits characteristics of a shell entity primarily engaged in intellectual property litigation and funded by third-party financiers. These factors strongly suggest an NPE business model for the current patent owner.

Verification: USPTO Assignment Center Search for US9332776

To identify the most relevant prior art for US Patent 9332776, I need to access the full patent text and its cited references. The patent text provided in the prompt already contains the prior art citations in the "References Cited" section. I will analyze these citations and determine their potential relevance based on the summary of claims.

The provided patent text includes a section "Cross-Reference to Related Applications" which lists prior art that are also related applications by the same inventors. These are typically important for understanding the development of the invention.

Here's an analysis of the most relevant prior art cited within US9332776, focusing on potential anticipation under 35 U.S.C. § 102. Anticipation means that every element of a claim is found, either expressly or inherently described, in a single prior art reference.

Prior Art References:

1. U.S. Pat. No. 8,939,388

   • Full Citation: U.S. Pat. No. 8,939,388 to Beetz et al., titled "Methods and apparatus for low heat spray drying"
   • Publication/Filing Date: Issued January 27, 2015. Filed September 26, 2011 (as application Ser. No. 13/245,369).
   • Brief Description: This patent is explicitly identified as a parent application (continuation-in-part) of US9332776. It describes methods and apparatus for low heat spray drying. Given it's a direct lineage, it would likely contain similar core inventive concepts but potentially lack the specific refinements or claim scope of the present patent.
   • Potential Anticipated Claims: As a direct parent, this patent likely anticipates many, if not all, of the broad concepts in US9332776, particularly the method claims (e.g., Independent Claim 1) related to forming a slurry, applying an electrostatic charge, atomizing, and suspending without heated drying fluids. The differences would lie in the specific parameters, apparatus details, or product characteristics that represent improvements over the parent.
     • Specific elements of Independent Claim 1 potentially anticipated: Forming a slurry, applying an electrostatic charge, atomizing the charged slurry, suspending for division into sub-particles, and continuing suspension without heated drying fluids to produce dried particles.
     • Specific elements of Independent Claim 12 potentially anticipated: Aspects of a drying chamber, electrodes, and electric fields if broadly disclosed in the parent.
     • Specific elements of Independent Claim 16 and 20 potentially anticipated: The concept of a dried powder with preserved active ingredient, though the precise percentage values or aging stability might be novel in 9332776.

2. U.S. Provisional Patent Application No. 61/386,762

   • Full Citation: U.S. Provisional Patent Application No. 61/386,762 to Beetz et al., titled "Methods and apparatus for low heat spray drying"
   • Publication/Filing Date: Filed September 27, 2010.
   • Brief Description: This is the earliest priority document for US9332776. Provisional applications serve to establish an early filing date and typically contain a description of the invention.
   • Potential Anticipated Claims: Similar to the '388 patent, this provisional application would be highly relevant as it describes the earliest conceptualization of the invention. It is likely to anticipate the fundamental aspects of the low-heat spray drying method (Independent Claim 1) and potentially the core apparatus (Independent Claim 12). The specific advancements in product properties (Independent Claims 16 and 20), especially the precise percentages of active ingredient retention and stability, might be further developed in the later applications.

General Notes on Anticipation (35 U.S.C. § 102):
To anticipate a claim, a single prior art reference must disclose every element of that claim, either expressly or inherently. The elements must be arranged as required by the claim. A species disclosed in prior art can anticipate a generic claim, and if a claim covers alternatives, it is anticipated if any alternative is known in the prior art. Even if a prior art reference is silent about an inherent characteristic, extrinsic evidence can be used to show that the characteristic is necessarily present.

Obviousness Analysis under 35 U.S.C. § 103 for US Patent 9332776

An invention is considered obvious under 35 U.S.C. § 103 if "the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains." The analysis requires considering the scope and content of the prior art, the differences between the prior art and the claims at issue, the level of ordinary skill in the pertinent art, and any secondary considerations (not provided in this context).

The primary prior art references for this analysis are the patent's own direct ancestors:

1. U.S. Pat. No. 8,939,388 (the '388 patent) to Beetz et al., titled "Methods and apparatus for low heat spray drying," issued January 27, 2015, which is explicitly a continuation-in-part of the application leading to US9332776.
2. U.S. Provisional Patent Application No. 61/386,762 (the '762 provisional) to Beetz et al., titled "Methods and apparatus for low heat spray drying," filed September 27, 2010, which is the earliest priority document for US9332776.

As these references represent the inventors' own earlier work on the same subject matter, a "combination" of these references implies a comprehensive understanding of the inventors' progressive disclosures regarding low-heat spray drying. A person having ordinary skill in the art (POSITA) in the field of spray drying or chemical engineering would be familiar with conventional spray drying limitations, electrostatic principles, and process optimization. They would also understand the motivations to improve product quality and process efficiency.

Combination Rationale and Motivation

A POSITA would be motivated to consider the teachings of the '388 patent and the '762 provisional together to fully grasp the foundational concepts and initial embodiments of the low-heat, electrostatic spray drying technology. The '388 patent explicitly builds upon the '762 provisional, indicating a natural progression of research and development. Therefore, the motivation to "combine" them is inherent in understanding the state of the art as established by the inventors themselves, with the goal of further refining and optimizing the disclosed low-heat process for superior results.

The obviousness arguments below focus on whether the specific advancements claimed in US9332776 would have been mere predictable refinements or inherent results of the broader teachings in the '388 patent and '762 provisional.

Obviousness of Independent Claims

1. Independent Claim 1 (Method Claim)

Independent Claim 1 specifies a method for low-heat spray drying, emphasizing specific ranges for slurry viscosity and water content, and the absence of heated drying fluids.

• Prior Art Disclosure (from '388 patent and '762 provisional): The patent text of US9332776 itself states that the "present disclosure provides a new method of spray drying, using a low temperature, e.g., 'no heat', spray drying process that produces powder products with superior flavor retention and stability. The spray drying method of the present disclosure does not employ purposely heated gas for removing water from the atomized fluid droplets, as has been the case in previously employed spray drying operations." This establishes that the core concept of "no heat" drying was present in the inventors' earlier work. Furthermore, the detailed description of US9332776 (which incorporates by reference the '388 patent and '762 provisional) explicitly notes that the process "utiliz[es] unique dryer designs and high solids content (low water content) slurries/emulsions with extremely high viscosities (for example, viscosities in a range of from 500 to 10000 mPa-s) to produce powders dried at low temperatures, such as temperatures on the order of from 5 to 50° C." It also contrasts this with "conventional slurries hav[ing] viscosities between about 10-200 mPa-s and contain an amount of water between about 50-70% by weight."

• Differences in Claim 1: The claim specifies slurry viscosities "greater than about 300 mPa-s" (e.g., 500-16,000 mPa-s or 1000-4000 mPa-s) and water ratios "between about 20-50 weight percentage" (e.g., about 30 weight percentage). It also explicitly limits the non-heated drying fluid temperature to "less than about 100° C." (e.g., <75° C., <45° C., <35° C., <30° C., or ambient).

• Motivation for Obviousness: A POSITA, having learned from the '388 patent and '762 provisional that a "low heat" or "no heat" electrostatic spray drying process using "high solids content (low water content) slurries/emulsions with extremely high viscosities" is beneficial for improved product properties, would be motivated to systematically explore and optimize the specific parameters of viscosity, water content, and drying fluid temperature. The explicitly mentioned range of "500 to 10000 mPa-s" for viscosity in the detailed description suggests that the inventors already had this range in mind. Refining these broad teachings into the specific numerical ranges claimed in US9332776 would be considered "obvious to try" for a POSITA seeking to enhance the performance of the already-disclosed low-heat process. Similarly, maintaining the drying fluid temperature below conventional levels was the core innovation described in the parent applications, and selecting specific upper bounds (e.g., less than 100°C) is a predictable design choice to ensure minimal heat degradation.

2. Independent Claim 12 (Apparatus Claim)

Independent Claim 12 describes a drying chamber made of non-electrically conductive material, with external electrodes inducing an internal electric field to direct particles.

• Prior Art Disclosure (from '388 patent and '762 provisional): The detailed description of US9332776 (which references the earlier applications) explicitly discusses the benefits of using non-metallic, non-conducting dielectric materials for the drying chamber. It states, "The use of non-metallic, non-conducting dielectric materials to form the drying chamber 107 (such as the engineered plastic composite materials), permits the use of one or more electric fields within the drying chamber 107 itself, to urge the particles/droplets 108 into desired trajectories..." It further clarifies the problem with conventional metallic chambers: "Notably, it is virtually impossible to develop an electric field inside a metallic, conductive vessel of the prior art because all charge accumulates on the surface of the vessel." The prior art would thus teach the desirability of applying electric fields internally and the impediment posed by conductive materials.

• Differences in Claim 12: The claim specifies a drying chamber made of "non-electrically conductive material" and "first and second electrodes are disposed external to the drying chamber, yet induce an electric field within the internal volume of the drying chamber."

• Motivation for Obviousness: A POSITA, having recognized from the '388 patent and '762 provisional the advantages of using electric fields within the drying chamber to control particle trajectory, and understanding the fundamental principles of electromagnetism, would readily understand that a conductive (e.g., metallic) chamber would prevent the effective establishment of such an internal field. Therefore, selecting a "non-electrically conductive material" for the drying chamber would be an obvious design choice to enable the function of the internal electric field. Furthermore, positioning electrodes "external" to a non-conductive chamber to induce an internal electric field is a predictable engineering solution to avoid issues like fouling, corrosion, or complex internal mounting, while still achieving the desired electric field effect. This represents a predictable combination of known materials and electrical principles to achieve a desired function.

3. Independent Claim 16 (Product Claim - Property 1)

Independent Claim 16 describes a dried powder characterized by the retention of at least one principle molecular type of the active ingredient within about 5% of its initial weight percentage.

• Prior Art Disclosure (from '388 patent and '762 provisional): The core benefit of the low-heat process, as discussed in the patent (and implicitly in its antecedents), is "higher levels of preservation of starting active ingredients such as volatile flavor molecules" and "superior flavor retention." FIG. 11, which illustrates this preservation, shows "dried powder 402 produced in accordance with the no-heat process described herein," indicating that this result was an inherent characteristic of the process described in the earlier applications.

• Differences in Claim 16: The claim quantifies this retention as a "weight percentage of at least one of the one or more principle molecular types in the final active ingredient is within about 5% of a weight percentage of the corresponding principle molecular types in the initial active ingredient." The claim further narrows this to 3%, 2%, or 1% in dependent claims.

• Motivation for Obviousness: Given that the '388 patent and '762 provisional disclose a "low heat" or "no heat" process aimed at achieving "superior flavor retention," a POSITA would expect and inherently achieve improved retention of volatile components. The act of quantifying this expected superior performance by conducting analytical tests (such as GC-MS, as mentioned in the patent) and then defining a specific percentage range for this inherent outcome would be a routine characterization of the product. These specific numerical thresholds (e.g., "within about 5%") would be considered inherent results of practicing the disclosed low-heat process, rather than an independently inventive step.

4. Independent Claim 20 (Product Claim - Property 2)

Independent Claim 20 describes a dried powder characterized by the stability of at least one principle molecular type, with its weight percentage not varying by more than about 5% during 1000 hours at 95°F.

• Prior Art Disclosure (from '388 patent and '762 provisional): Similar to Claim 16, the underlying objective and outcome of the inventors' low-heat process was to achieve "superior... stability" of active ingredients. The patent explicitly references an "accelerated aging study (at elevated temperatures of about 95° F.) comparing powders produced by conventional spray dry processing and the no-heat process" over "1000 hours," with results shown in FIG. 11 and FIGS. 12-19. This demonstrates that the testing conditions and the discovery of improved stability under these conditions were already part of the inventors' prior work.

• Differences in Claim 20: The claim quantifies this stability as a "weight percentage of at least one of the one or more principle molecular types in the active ingredient does not vary by more than about 5% during aging of the dried powder during any period of elevated temperature of about 95° F. up to about 1000 hours." Dependent claims further narrow this to 3%, 2%, or 1%.

• Motivation for Obviousness: A POSITA, starting from the teachings of the '388 patent and '762 provisional that describe a process yielding "superior stability," would naturally expect a product with enhanced shelf-life characteristics. Conducting standard accelerated aging tests at common industry conditions (like 95°F for 1000 hours, as detailed in the patent) and then quantifying the observed stability with specific percentage ranges would be a routine and inherent characterization of the product's performance. The specific numerical values would represent the inherent attributes of the product produced by the previously disclosed low-heat drying process.

To detail the patent term adjustments (PTA), patent term extensions (PTE), continuation applications, divisional applications, related family members, and projected expiration date for US Patent 9332776, I need to consult the patent's continuity data and patent term information, which are typically found in the USPTO's public records.

Based on the provided patent text and a search of general USPTO guidelines, here's what can be determined:

Patent Term Adjustments (PTA) and Patent Term Extensions (PTE):

• Patent Term Adjustment (PTA): PTA is designed to compensate for certain delays caused by the USPTO during the prosecution of a patent application. It adds days to the 20-year lifespan of a patent. The specific PTA for US9332776 is not available from the provided text or direct search results for this patent number. To find the exact PTA, one would typically need to consult the "Patent Term Adjustment" section of the patent's file wrapper in Public PAIR.
• Patent Term Extension (PTE): PTE can extend the patent term to mitigate loss of term due to regulatory approval processes, most commonly for human drugs, food additives, medical devices, and similar products. There is no information in the provided patent text or search results to suggest that US9332776 has been granted any PTE.

Continuation Applications, Divisional Applications, and Related Family Members:
The patent explicitly states that it is a "continuation-in-part under 35 USC 120 of U.S. patent application Ser. No. 13/245,369 filed Sep. 26, 2011" and that the '369 application "in turn claims the benefit under 35 USC 119 of U.S. Provisional Patent Application No. 61/386,762, filed Sep. 27, 2010."

Therefore, the related family members and continuity data are:

• Parent Application (Continuation-in-Part): U.S. patent application Ser. No. 13/245,369, filed September 26, 2011, and issued as U.S. Pat. No. 8,939,388 on January 27, 2015.
• Grandparent Application (Provisional): U.S. Provisional Patent Application No. 61/386,762, filed September 27, 2010.

The Google Patents "Legal status" section also indicates a priority to US15/092,561 filed on 2016-04-06. This suggests that US9332776 may also be a parent to a later-filed application.

Projected Expiration Date:
The term of a U.S. patent (other than a design patent) issued from an application filed on or after June 8, 1995, is 20 years from the earliest U.S. filing date for which a benefit is claimed.

• The earliest priority date for US9332776 is September 27, 2010, from U.S. Provisional Patent Application No. 61/386,762.
• Therefore, the patent term would ordinarily be 20 years from this date.
• 2010-09-27 + 20 years = 2030-09-27.

The Google Patents "Legal status" section states the "Anticipated expiration" as 2031-09-26. This indicates that there is likely a Patent Term Adjustment (PTA) of approximately one year (364 days).

Summary of Information for US9332776:

• Patent Term Adjustments (PTA): The anticipated expiration date of September 26, 2031, compared to the calculated 20-year term from the earliest priority date (September 27, 2030), suggests a PTA of approximately one year. The precise PTA calculation would require access to the patent's prosecution history.
• Patent Term Extensions (PTE): No information available to suggest any PTE has been granted.
• Continuation Applications: US Patent 9332776 is a continuation-in-part of U.S. patent application Ser. No. 13/245,369 (which issued as U.S. Pat. No. 8,939,388).
• Divisional Applications: No divisional applications are explicitly mentioned in the provided text as direct descendants of US9332776, though it claims priority from a provisional application and a non-provisional application, and also shows priority to a later application (US15/092,561).
• Related Family Members (Priority Chain):
  • U.S. Provisional Patent Application No. 61/386,762, filed September 27, 2010.
  • U.S. patent application Ser. No. 13/245,369, filed September 26, 2011 (issued as U.S. Pat. No. 8,939,388).
  • U.S. patent application Ser. No. 14/606,771, filed January 27, 2015 (which led to US9332776).
  • U.S. patent application Ser. No. 15/092,561, filed April 6, 2016 (priority claimed from US9332776).
• Projected Expiration Date: September 26, 2031.

Defensive Disclosure: Derivatives of US Patent 9332776 for Low Heat Spray Drying

This Defensive Disclosure aims to broaden the public domain of prior art related to low-heat, electrostatic spray drying technologies, building upon the foundational concepts of US Patent 9332776. The objective is to proactively render future incremental improvements or variations by competitors "obvious" or "non-novel" by publicly describing a range of derivatives across various technical axes. The current date for this disclosure is April 26, 2026.

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Derivatives of Independent Claim 1 (Method Claim)

Independent Claim 1 details a method for low-heat spray drying involving slurry formation, electrostatic charging, atomization, particle division via repulsive forces, and drying without heated fluids.

1.1 Material & Component Substitution: Alternative Carriers and Solvents

Enabling Description:
This derivative utilizes a slurry comprising a liquid solvent, a carrier, and an active ingredient. The liquid solvent consists of a eutectic mixture of water and ethanol (e.g., 95.6% ethanol by weight), allowing for lower boiling points and faster evaporation rates at ambient or sub-ambient temperatures. The carrier is selected from a group of bio-polymers such as zein protein, sodium alginate, or gum arabic, chosen for their film-forming properties and compatibility with specific active ingredients. The active ingredient can be a thermally labile probiotic culture (e.g., Lactobacillus plantarum) or a temperature-sensitive enzyme (e.g., cellulase). The electrostatic charging is applied via a high-voltage, direct contact electrode within the slurry feed line, generating a potential difference of 20-60 kV. Atomization is achieved using a vibrating mesh atomizer with a pore size of 10-50 µm, producing a fine mist of charged droplets. The drying process occurs in a dehumidified nitrogen atmosphere maintained at 5-15°C and a relative humidity below 5%, promoting solvent evaporation and coulombic fission without thermal degradation.

flowchart TD
    A[Prepare Slurry: Eutectic Water/Ethanol Solvent, Zein/Alginate/Gum Arabic Carrier, Probiotic/Enzyme Active Ingredient] --> B{Apply Electrostatic Charge (20-60 kV DC via Contact Electrode)};
    B --> C[Vibrating Mesh Atomizer (10-50 µm pore size)];
    C --> D[Charged Droplets Undergo Coulombic Fission];
    D --> E[Suspend in Dehumidified Nitrogen Atmosphere (5-15°C, <5% RH)];
    E --> F[Evaporation of Solvent & Formation of Dried Particles];

1.2 Operational Parameter Expansion: Sub-Ambient & Vacuum Drying for Nanoscale Particles

Enabling Description:
A low-heat spray drying method for producing nanoparticles with enhanced active ingredient retention. The slurry is formulated with a viscosity exceeding 20,000 mPa-s (e.g., using a high-concentration modified starch with a DE <10, or a microcrystalline cellulose suspension) and a water content between 10-20 weight percentage. An electrostatic charge is imparted by applying a pulsed DC voltage of 70-100 kV at 1-10 kHz to the slurry just prior to atomization. Atomization is performed using an electrospray nozzle with a tip diameter in the range of 100-500 µm, operating in cone-jet mode to generate droplets in the sub-micron to low-micron range. These highly charged droplets undergo extensive coulombic fission, resulting in sub-100 nm particles. The drying chamber is maintained under a partial vacuum (0.1-0.5 atm) with a continuous flow of ultra-dry inert gas (e.g., argon or helium) pre-chilled to -10°C to -20°C. The rapid expansion and evaporation under vacuum, combined with the sub-ambient temperature and coulombic fission, leads to immediate solvent removal and formation of dried nanoparticles without thermal stress.

flowchart TD
    A[Slurry Preparation: Viscosity > 20,000 mPa-s, 10-20 wt% Water] --> B{Apply Pulsed DC Electrostatic Charge (70-100 kV, 1-10 kHz)};
    B --> C[Electrospray Nozzle Atomization (100-500 µm tip)];
    C --> D[Sub-micron Charged Droplets];
    D --> E[Extensive Coulombic Fission (Sub-100 nm particle formation)];
    E --> F[Drying Chamber: Partial Vacuum (0.1-0.5 atm), Ultra-Dry Inert Gas (-10°C to -20°C)];
    F --> G[Dried Nanoparticles with Encapsulated Active Ingredient];

1.3 Cross-Domain Application: Pharmaceutical Microencapsulation for Targeted Drug Delivery

Enabling Description:
A low-heat spray drying method specifically adapted for encapsulating sensitive pharmaceutical active ingredients (e.g., peptide drugs, mRNA vaccines, or enzymes) for targeted drug delivery. The slurry consists of the therapeutic agent dissolved or suspended in an aqueous solution with a biocompatible polymer carrier (e.g., PLA, PLGA, chitosan, or albumin) at a high concentration, resulting in a viscosity of 1,000-5,000 mPa-s and a water content of 30-40 weight percentage. An oscillating electric field (5-20 kV AC, 50-500 Hz) is applied to the atomized droplets to enhance charge distribution and particle separation, optimizing the coulombic fission process. Atomization is carried out via a pneumatic two-fluid nozzle with atomizing air at 250-300 kPa, producing initial droplets of 50-150 µm. The drying chamber maintains a sterile, iso-osmotic air environment (e.g., 25°C, 30% RH) to minimize osmotic shock to biological active ingredients. The dried microparticles (1-10 µm) exhibit high encapsulation efficiency and retained biological activity, suitable for oral or inhaled delivery, with a precise release profile.

flowchart TD
    A[Prepare Slurry: Peptide/mRNA/Enzyme Active, PLA/PLGA/Chitosan Carrier] --> B{Pneumatic Two-Fluid Atomization (50-150 µm droplets)};
    B --> C{Apply Oscillating Electric Field (5-20 kV AC, 50-500 Hz) for Fission};
    C --> D[Suspend in Sterile, Iso-osmotic Air (25°C, 30% RH)];
    D --> E[Solvent Evaporation & Microparticle Formation];
    E --> F[Targeted Drug Delivery Microparticles];

1.4 Integration with Emerging Tech: AI-Optimized Real-time Process Control

Enabling Description:
A low-heat spray drying method where all critical process parameters are dynamically optimized in real-time using an AI-driven control system. The slurry formulation (viscosity, water content, carrier type, active ingredient concentration) is continuously monitored by IoT sensors (e.g., in-line viscometers, refractometers). An AI agent, trained on historical data and real-time feedback loops (e.g., particle size distribution via laser diffraction, active ingredient retention via in-line NIR spectroscopy, and residual moisture via dielectric sensors), predicts and adjusts atomization pressure, electrostatic charge intensity, drying chamber airflow, temperature (within the non-heated range, e.g., 20-30°C), and relative humidity. The AI's objective function is to maximize active ingredient retention and particle stability while minimizing energy consumption. Furthermore, each batch's unique processing parameters and product quality metrics are immutably recorded on a private blockchain ledger for enhanced supply chain transparency and regulatory compliance.

graph TD
    A[Slurry Prep] -- IoT Sensors --> B{AI Control System};
    B -- Parameter Adjustments --> C[Electrostatic Atomization];
    C -- IoT Sensors (Particle Size, Moisture) --> B;
    C -- In-line NIR --> B;
    D[Drying Chamber] -- IoT Sensors (Temp, RH, Airflow) --> B;
    B -- Data Logging --> E[Blockchain Ledger (Immutable Records)];

1.5 The "Inverse" or Failure Mode: Programmed Degradation for Controlled Release

Enabling Description:
A method for producing low-heat spray dried particles designed for programmed, controlled degradation and active ingredient release. The slurry incorporates a pH-sensitive or enzyme-degradable carrier material (e.g., Eudragit polymers, polycaprolactone, or specific cross-linked starches) with a specific active ingredient. An electrostatic charge is applied, and the slurry is atomized into charged wet particles. The particles undergo coulombic fission and are dried using non-heated, dehumidified air at ambient conditions. The key "inverse" feature is that the carrier system is engineered to degrade predictably under predefined environmental triggers (e.g., specific pH values in the gut, presence of certain enzymes, or UV light exposure). This allows for a burst or sustained release of the active ingredient at a desired time or location, intentionally compromising the long-term stability in storage in favor of controlled in-use release. The manufacturing process ensures minimal pre-mature degradation during drying to retain the initial active ingredient integrity.

stateDiagram-v2
    state "Slurry Preparation (pH/Enzyme Sensitive Carrier)" as Slurry
    state "Electrostatic Atomization & Coulombic Fission" as Atomize
    state "Low-Heat Drying (Ambient Dehumidified Air)" as Drying
    state "Encapsulated Particles" as Encapsulated
    state "Trigger Event (pH, Enzyme, UV)" as Trigger
    state "Active Ingredient Release" as Release

    Slurry --> Atomize
    Atomize --> Drying
    Drying --> Encapsulated
    Encapsulated --> Trigger : In-Use Degradation
    Trigger --> Release
    Release --> [*]

---

Derivatives of Independent Claim 12 (Apparatus Claim)

Independent Claim 12 describes a low-heat spray drying apparatus featuring a non-electrically conductive drying chamber with external electrodes inducing an internal electric field.

2.1 Material & Component Substitution: Advanced Ceramic Drying Chamber with Helical Electrodes

Enabling Description:
An apparatus for low-heat spray drying featuring a drying chamber constructed from advanced ceramic composites (e.g., silicon carbide or alumina reinforced with continuous fibers). This material provides superior thermal shock resistance, excellent dielectric properties, and chemical inertness, making it suitable for processing highly corrosive or abrasive slurries while maintaining a robust electric field. The electrodes are implemented as helical coils of platinum-iridium alloy, embedded within the exterior walls of the ceramic chamber during fabrication, rather than simple ring electrodes. This helical configuration, driven by a phased multi-channel high-voltage power supply, generates a complex, rotating electric field within the internal volume, optimizing particle residence time and enhancing radial dispersion. The non-electrically conductive nature of the ceramic ensures efficient field penetration without charge accumulation on the chamber walls.

classDiagram
    class Apparatus {
        +CeramicDryingChamber
        +HelicalElectrodes
        +PhasedHVPS
        +Atomizer
        +ParticleCollector
    }
    class CeramicDryingChamber {
        -material: SiC/Alumina Composite
        -dielectricConstant: high
        +internalVolume: Volume
        +inletEnd: End
        +outletEnd: End
    }
    class HelicalElectrodes {
        -material: Pt-Ir Alloy
        -configuration: Helical Coils
        +generateRotatingField()
    }
    class PhasedHVPS {
        +outputVoltage: 0-100kV
        +frequency: 0-10kHz
        +phaseControl: Array
        +supplyPower(electrodes)
    }
    Apparatus "1" *-- "1" CeramicDryingChamber
    CeramicDryingChamber "1" *-- "2" HelicalElectrodes : external
    PhasedHVPS "1" -- "1" HelicalElectrodes : powers

2.2 Operational Parameter Expansion: Microfluidic Drying Chamber for Nanoscale Production

Enabling Description:
A miniaturized apparatus for low-heat spray drying, comprising a microfluidic drying chamber fabricated using semiconductor lithography techniques from a non-electrically conductive polymer (e.g., PDMS, SU-8 photoresist) or fused silica. The internal volume of the chamber is in the micro-liter range, with channel dimensions in the range of 10-100 µm. A series of segmented, individually addressable micro-electrodes are integrated onto the external surface of the microfluidic chip, allowing for precise spatial and temporal control of localized electric fields (e.g., 1-5 kV across 50 µm gaps). The atomizer is a micro-nozzle or electrospray emitter integrated upstream. This setup enables single-droplet processing, extreme control over coulombic fission, and precise manipulation of particle trajectories within the micro-channels, facilitating the production of highly uniform nanoscale particles (e.g., <200 nm) at laboratory scale for high-value applications.

graph TD
    A[Microfluidic Chip (PDMS/Fused Silica)] --> B(Microfluidic Drying Chamber);
    A --> C(Integrated Micro-nozzle/Electrospray Emitter);
    B --> D{Segmented External Micro-electrodes};
    D -- Powered By --> E[Multi-channel Micro-voltage Controller (1-5 kV)];
    C -- Atomizes Charged Slurry --> B;
    B -- Particle Trajectory Control --> F(Nanoparticle Collection);

2.3 Cross-Domain Application: Additive Manufacturing Powder Feedstock Preparation

Enabling Description:
An apparatus for low-heat spray drying specifically designed for the preparation of specialized powder feedstock for additive manufacturing (e.g., selective laser sintering, binder jetting). The drying chamber is a large-scale, modular unit constructed from a high-strength polymer composite (e.g., carbon fiber reinforced epoxy). The chamber incorporates internal baffling and a vortex flow enhancer to optimize particle suspension. The first and second electrodes are large-area conductive polymer sheets, positioned externally at the inlet and outlet sections, respectively, and powered by a 100 kV DC source to generate a strong, uniform axial electric field. This field not only urges particles through the chamber but also helps to de-agglomerate electrostatically charged powder, ensuring a narrow particle size distribution (e.g., 5-50 µm) and improved flowability crucial for additive manufacturing processes. The system processes slurries containing metal, ceramic, or polymer precursors.

flowchart TD
    A[Slurry Feed (Metal/Ceramic/Polymer Precursors)] --> B(High-Throughput Atomizer);
    B --> C{Drying Chamber (Carbon Fiber-Epoxy Composite)};
    C -- External Conductive Polymer Sheets (100kV DC) --> D[Axial Electric Field Generation];
    C -- Vortex Flow Enhancer --> C;
    C --> E[Powder Collection & De-agglomeration];
    E --> F[Additive Manufacturing Feedstock];

2.4 Integration with Emerging Tech: Digital Twin for Predictive Process Optimization

Enabling Description:
An apparatus for low-heat spray drying integrated with a comprehensive digital twin for real-time monitoring, predictive optimization, and autonomous control. The drying chamber, constructed from non-conductive PEEK, is instrumented with an array of IoT sensors including electrostatic field strength meters, real-time particle image velocimetry (PIV) cameras, gravimetric moisture sensors, and gas analyzers for solvent vapor concentration. A high-fidelity computational fluid dynamics (CFD) model of the drying chamber and a multi-physics electrostatic model run concurrently as a digital twin. This twin continuously simulates the drying process, predicting particle trajectories, evaporation rates, and potential for agglomeration or chamber fouling. An AI controller, comparing real-time sensor data with digital twin predictions, autonomously adjusts electrode potentials, atomization parameters, and dehumidified airflow to maintain optimal drying conditions, prevent process drift, and predict maintenance needs. Data from the digital twin and physical sensors are secured via a blockchain for immutable audit trails.

graph LR
    A[Physical Apparatus (Drying Chamber, Atomizer, Electrodes)] -- IoT Sensors (PIV, Field Meters, Moisture, Gas) --> B{Digital Twin (CFD, Electrostatic Models)};
    B -- Predictions & Simulations --> C{AI Controller};
    C -- Control Adjustments (Electrode Potential, Airflow, Atomization) --> A;
    A -- Real-time Data --> B;
    B -- Audit Trail --> D[Blockchain Ledger];

2.5 The "Inverse" or Failure Mode: Fail-Safe Electrostatic Discharge System

Enabling Description:
An apparatus designed for low-heat spray drying, incorporating a fail-safe electrostatic discharge system. The drying chamber, while primarily constructed from a non-electrically conductive fiberglass composite, includes strategically placed, passively conductive ground planes (e.g., thin metallic mesh layers encapsulated within the composite, connected to earth ground) that are normally isolated from the primary electrostatic field. In the event of an electrostatic overcharge condition (e.g., exceeding 120% of nominal operating voltage) or unexpected particle agglomeration detected by optical sensors, a rapid discharge mechanism is activated. This mechanism involves temporarily bypassing the dielectric isolation to connect the external electrodes directly to the encapsulated ground planes, rapidly neutralizing the electric field and preventing uncontrolled sparking or catastrophic equipment failure due particularly to dust explosion risks with organic powders. This system ensures personnel safety and protects sensitive electronic components, allowing for a controlled shutdown or transition to a low-power, non-electrostatic drying mode.

stateDiagram-v2
    state "Normal Operation" as Normal
    state "Overcharge/Agglomeration Detected" as Fault
    state "Rapid Discharge Activated" as Discharge
    state "Field Neutralized" as Neutral
    state "Controlled Shutdown/Low-Power Mode" as Safe

    Normal --> Fault : >120% Voltage OR Optical Sensor Trigger
    Fault --> Discharge : Activate Bypass
    Discharge --> Neutral : Connect to Ground Planes
    Neutral --> Safe : System Stable
    Safe --> [*] : Safe State

---

Derivatives of Independent Claim 16 (Product Claim - Property 1)

Independent Claim 16 describes a dried powder with an active ingredient whose weight percentage of key molecular types is retained within about 5% of its initial value.

3.1 Material & Component Substitution: Multi-Layer Encapsulation for Enzyme Stabilization

Enabling Description:
A dried powder product produced via low-heat spray drying, characterized by multi-layer encapsulation for stabilizing highly sensitive active ingredients such as enzymes (e.g., lipase, protease). Each dried particle features a core containing the enzyme, surrounded by a primary carrier layer (e.g., gum arabic) providing initial protection, and then an outer secondary carrier layer (e.g., maltodextrin with high DE or whey protein isolate) offering additional barrier properties against oxygen and moisture. The initial active ingredient includes the enzyme with specific isoforms and activity units. The final active ingredient, after the low-heat drying process, demonstrates that the weight percentage of at least one enzyme isoform, and critically, its catalytic activity, is within 1% of the corresponding initial enzyme isoform and activity. This multi-layer structure, achieved through sequential electrostatic spray drying passes or co-axial nozzle atomization, significantly enhances the preservation of enzyme function.

classDiagram
    class DriedParticle {
        +core: ActiveIngredient (Enzyme)
        +primaryCarrierLayer: GumArabic
        +secondaryCarrierLayer: Maltodextrin/WheyProtein
        +retention: 1% variation of isoform/activity
    }
    class ActiveIngredient {
        +enzyme: Lipase/Protease
        +isoform: specific
        +catalyticActivity: units
    }
    class Carrier {
        +type: String
        +barrierProperties: String
    }
    DriedParticle "1" *-- "1" ActiveIngredient
    DriedParticle "1" *-- "1" primaryCarrierLayer
    DriedParticle "1" *-- "1" secondaryCarrierLayer
    primaryCarrierLayer <|-- Carrier
    secondaryCarrierLayer <|-- Carrier

3.2 Operational Parameter Expansion: Ultra-High Retention for Pharmaceutical API

Enabling Description:
A dried powder product specifically for highly potent pharmaceutical active ingredients (APIs), where the weight percentage of the API is retained within an exceptionally tight tolerance of less than 0.5% (e.g., 0.1-0.2%) of its initial weight percentage. This is achieved through an ultra-low temperature, high-viscosity electrostatic spray drying process using excipients like poly(ethylene glycol) (PEG) or hydroxypropyl methylcellulose (HPMC) as carriers, formulated with strictly controlled water activity in the slurry. The API can be a small molecule drug susceptible to polymorphic changes or a biological drug prone to denaturation. The final powder is analyzed by high-performance liquid chromatography (HPLC) and X-ray diffraction (XRD) to confirm both chemical purity and maintained crystalline structure or biological integrity of the API. This level of retention is critical for maintaining dosage accuracy and therapeutic efficacy in sensitive drug formulations.

flowchart TD
    A[API Slurry Prep (PEG/HPMC Carrier, Controlled Water Activity)] --> B{Ultra-Low Temp Electrostatic Drying};
    B --> C[Dried Powder (API encapsulated)];
    C -- HPLC Analysis --> D{Chemical Purity within <0.5%};
    C -- XRD Analysis --> E{Polymorphic/Structural Integrity Maintained};

3.3 Cross-Domain Application: Stable Nutrient Delivery for Aquaculture Feeds

Enabling Description:
A dried powder product for aquaculture feeds, providing stable and highly retained essential nutrients (e.g., omega-3 fatty acids, specific amino acids, vitamins like C and E) critical for fish and shrimp health. The active ingredients, often susceptible to oxidation and leaching in aquatic environments, are encapsulated within a complex carrier matrix consisting of modified starches, chitosans, and protein hydrocolloids. The low-heat spray drying process ensures that the weight percentage of vulnerable omega-3 fatty acids (e.g., DHA, EPA), as determined by GC-MS, is retained within 2% of their initial concentration. The resulting dried powder particles are designed to be water-stable, minimizing nutrient loss when introduced into water and ensuring bio-availability to aquatic organisms, thereby improving feed efficiency and reducing environmental impact.

graph TD
    A[Nutrient Slurry (Omega-3s, AA, Vitamins; Starch/Chitosan/Protein Carrier)] --> B{Low-Heat Electrostatic Spray Drying};
    B --> C[Aquaculture Feed Powder];
    C -- GC-MS Analysis --> D{Omega-3 Fatty Acid Retention within 2%};
    C --> E[Water-Stable Particles, Bioavailable Nutrients];

---

Derivatives of Independent Claim 20 (Product Claim - Property 2)

Independent Claim 20 describes a dried powder product characterized by the stability of its active ingredient, with its weight percentage not varying by more than about 5% during aging at 95°F for up to 1000 hours.

4.1 Material & Component Substitution: Enhanced Stability via Inorganic/Organic Hybrid Carriers

Enabling Description:
A dried powder product with significantly enhanced active ingredient stability, where the active ingredient (e.g., sensitive probiotics or oxidation-prone antioxidants like astaxanthin) is encapsulated within an inorganic/organic hybrid carrier system. The carrier comprises a primary organic polymer (e.g., specialized cyclodextrins or lignin derivatives) co-spray dried with an inert inorganic material (e.g., fumed silica, titania nanoparticles, or calcium carbonate microparticles). The inorganic component provides an additional physical barrier and modulates moisture adsorption, while the organic matrix encapsulates the active ingredient. The resulting dried powder demonstrates a weight percentage variation of the active ingredient of less than 1% when aged at an elevated temperature of 95°F (35°C) for up to 2000 hours, or at 120°F (49°C) for 500 hours, significantly exceeding the claimed stability profile. This robust hybrid matrix provides superior protection against thermal, oxidative, and hydrolytic degradation.

flowchart TD
    A[Slurry Prep (Probiotic/Antioxidant, Cyclodextrin/Lignin, Silica/Titania/CaCO3)] --> B{Low-Heat Electrostatic Spray Drying};
    B --> C[Hybrid Encapsulated Powder];
    C -- Accelerated Aging (95°F/2000hr OR 120°F/500hr) --> D{Active Ingredient Variation < 1%};

4.2 Operational Parameter Expansion: Stability under Extreme Cyclic Environmental Stress

Enabling Description:
A dried powder product exhibiting exceptional long-term stability under extreme cyclic temperature and humidity conditions. The active ingredient (e.g., highly volatile flavors such as short-chain aldehydes or essential oil terpenes, or moisture-sensitive enzymes) is encapsulated using a highly cross-linked protein or polysaccharide carrier matrix, leveraging the low-heat drying process to avoid initial degradation. The product demonstrates that the weight percentage of at least one principle molecular type in the active ingredient does not vary by more than 2% when subjected to a cyclic aging profile: 12 hours at -10°C, followed by 12 hours at 50°C, and 8 hours at 75% relative humidity, for a total of 100 cycles (equivalent to 2400 hours of variable stress). This surpasses typical accelerated aging tests, proving stability under conditions mimicking severe transportation or long-term storage fluctuations in uncontrolled environments.

stateDiagram-v2
    state "Start" as Start
    state "Encapsulated Powder (Volatile Flavors/Enzymes)" as Powder
    state "Cycle 1: -10°C (12hr)" as C1_Low
    state "Cycle 2: 50°C (12hr)" as C2_High
    state "Cycle 3: 75% RH (8hr)" as C3_RH
    state "End Cycle (Total 100 Cycles)" as EndCycle
    state "Stability Verification (Variation < 2%)" as Verify

    Start --> Powder
    Powder --> C1_Low
    C1_Low --> C2_High
    C2_High --> C3_RH
    C3_RH --> EndCycle
    EndCycle --> C1_Low : If Cycles < 100
    EndCycle --> Verify : If Cycles = 100
    Verify --> [*]

4.3 Cross-Domain Application: Shelf-Stable Diagnostic Reagents for Point-of-Care Testing

Enabling Description:
A dried powder product for producing shelf-stable diagnostic reagents, eliminating the need for cold chain storage and enabling point-of-care testing in remote locations. The active ingredient consists of lyophilized antibodies, specific enzymes (e.g., luciferase for biosensors), or DNA probes, which are typically highly sensitive to heat and moisture. These reagents are encapsulated using a trehalose or sucrose-based carrier matrix via the low-heat electrostatic spray drying method. The resulting dried powder demonstrates that the specific binding affinity or enzymatic activity of the encapsulated reagent does not vary by more than 3% when stored at an ambient temperature of 40°C for up to 1 year, or at 5°C for 5 years, ensuring reliable diagnostic performance without refrigeration. This enables distribution and use of critical diagnostics in challenging logistical environments.

graph TD
    A[Reagent Slurry (Antibodies/Enzymes/DNA Probes, Trehalose/Sucrose Carrier)] --> B{Low-Heat Electrostatic Spray Drying};
    B --> C[Shelf-Stable Diagnostic Powder];
    C -- Stability Testing (40°C/1yr OR 5°C/5yr) --> D{Binding Affinity/Enzymatic Activity Variation < 3%};
    D --> E[Point-of-Care Application];

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Combination Prior Art Scenarios

Here are three scenarios combining US Patent 9332776 with existing open-source standards to demonstrate obviousness or lack of novelty for future incremental improvements.

1. Integration with OPC UA for Process Control and Data Exchange

Description:
The methods and apparatus of US9332776, particularly the real-time monitoring and control aspects (e.g., adjustments to electrostatic field, airflow, viscosity, and humidity), can be readily integrated with the OPC Unified Architecture (OPC UA) open-source standard. OPC UA provides a platform-independent, service-oriented architecture for robust, secure, and reliable communication between industrial control systems and software applications. A POSITA would find it obvious to implement OPC UA to standardize data acquisition from sensors (e.g., in-line viscometers, electrostatic field sensors, humidity probes in the drying chamber) and to enable seamless communication with the high-voltage power supplies, atomization control units, and dehumidification systems described in US9332776. This allows for interoperability, remote control, and data exchange for process optimization and historical data logging across various vendor equipment in a low-heat spray drying facility.

sequenceDiagram
    participant S as Sensors (Viscometer, E-Field, RH)
    participant C as PLC/DCS Controller
    participant OPCUAS as OPC UA Server
    participant OPCUAC as OPC UA Client (HMI, Historian)
    participant A as Atomization System
    participant E as Electrodes HVPS
    participant D as Dehumidifier

    S ->> C: Process Data (Slurry Viscosity, Field Strength, RH)
    C ->> OPCUAS: Publish Data (Standardized Tags)
    OPCUAC ->> OPCUAS: Subscribe/Read Data
    OPCUAC ->> C: Write Control Commands (Setpoints)
    C ->> A: Adjust Atomization Rate
    C ->> E: Adjust Electrode Potential
    C ->> D: Adjust Dehumidifier Output
    OPCUAC ->> OPCUAC: Monitor & Log Process Trends

2. Utilization of the ISA-88 Standard for Batch Process Control

Description:
The batch-oriented nature of preparing slurries and processing them in a spray dryer, as described in US9332776, aligns directly with the ISA-88 (IEC 61512) standard for batch control systems. This open-source standard provides a consistent terminology and modular framework for designing, configuring, and operating batch processes. A POSITA would recognize the benefits of applying ISA-88 to model the low-heat spray drying operation, breaking it down into process cells, units (e.g., slurry preparation unit, drying unit), and equipment modules. This would standardize recipes (e.g., for different active ingredients or carrier formulations), allocate equipment, manage phases (e.g., electrostatic charging, atomization, drying, collection), and handle batch tracking. Applying ISA-88 to US9332776 enhances flexibility, scalability, and repeatability for producing diverse low-heat spray dried products, particularly in industries requiring rigorous documentation and quality control.

graph TD
    A[Process Cell: Low-Heat Spray Drying] --> B{Unit 1: Slurry Preparation};
    A --> C{Unit 2: Electrostatic Drying};
    A --> D{Unit 3: Powder Collection};

    B --> B1(Equipment Module: Mixing Tank);
    B --> B2(Equipment Module: Feed Pump);

    C --> C1(Equipment Module: Atomizer);
    C --> C2(Equipment Module: Drying Chamber);
    C --> C3(Equipment Module: Electrodes/HVPS);
    C --> C4(Equipment Module: Dehumidifier);

    D --> D1(Equipment Module: Cyclone Separator);
    D --> D2(Equipment Module: Baghouse);
    D --> D3(Equipment Module: Collection Container);

    subgraph Batch Control System (ISA-88)
        E[Recipe Management] -- Controls --> A;
        F[Phase Logic] -- Manages --> C1, C2, C3, C4;
        G[Batch History] -- Records --> A;
    end

3. Data Management with Apache Kafka for Real-time Analytics

Description:
To handle the high volume and velocity of sensor data generated by the advanced low-heat spray drying apparatus of US9332776 (e.g., particle image velocimetry, real-time spectroscopic analysis, electrostatic field fluctuations), leveraging Apache Kafka, an open-source distributed streaming platform, would be obvious. Kafka can ingest, store, and process streams of records in real-time. A POSITA would understand that by routing all raw sensor data and control event logs through Kafka topics, a highly scalable and fault-tolerant data backbone is created. This enables immediate aggregation and analysis of drying kinetics, particle morphology, and active ingredient stability metrics. Machine learning models can consume these data streams to provide predictive maintenance alerts or to perform in-situ quality control, ensuring consistent product quality even with complex, sensitive active ingredients dried at low temperatures.

graph LR
    subgraph Data Producers
        S1[Flow Rate Sensor] --> K;
        S2[Viscosity Sensor] --> K;
        S3[E-Field Sensor] --> K;
        S4[Humidity Sensor] --> K;
        S5[NIR Spectrometer] --> K;
        S6[PIV Camera] --> K;
    end

    K[(Apache Kafka Cluster)]

    subgraph Data Consumers
        C1[Real-time Monitoring Dashboard] --> K;
        C2[Machine Learning Model (Predictive Quality)] --> K;
        C3[Historian Database (Long-term Storage)] --> K;
        C4[Regulatory Compliance Audit System] --> K;
    end

    K -- Data Streams --> C1, C2, C3, C4;