Cleaning performance verification for fast in-place and off-site cleaning
By contacting a solution containing alkali metal hydroxides and oxidizing compounds with the substrate, the cleaning effectiveness of CIP and COP systems is tested, solving the problem of incomplete cleaning in existing technologies. This enables rapid and visualized cleaning verification, ensuring the cleanliness and safety of the equipment.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-07-24
- Publication Date
- 2026-03-24
AI Technical Summary
Existing CIP and COP cleaning systems are difficult to detect when cleaning is incomplete or uneven, which may lead to equipment contamination and cross-contamination, especially when it is difficult to verify the cleaning effect on thermally degraded contaminants.
The solution contains alkali metal hydroxides and oxidizing compounds (such as sodium hypochlorite, sodium persulfate, sodium dichromate, etc.) and comes into contact with the substrate. Organic or non-organic contaminants are detected by colorimetric reaction to ensure cleaning effectiveness.
This provides a rapid, visual method to effectively detect and verify the cleaning effectiveness of CIP and COP systems, ensuring that there are no residual contaminants on equipment surfaces and improving the safety and regulatory compliance of cleaning systems.
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Figure CN121729615A_ABST
Abstract
Description
BACKGROUND
[0001] Clean-in-place (CIP) and clean-out-of-place (COP) are two common methods used in the food, beverage, and pharmaceutical industries for cleaning and sanitizing processing equipment. CIP systems are designed to clean equipment without disassembly, allowing for a quick and efficient cleaning process. In a CIP system, a cleaning solution is circulated through the equipment to remove any contaminants, and then the solution is drained from the system. CIP systems are often automated and can be programmed to run at specific intervals, reducing the need for manual cleaning and minimizing the risk of human error. CIP systems are commonly used in industries such as dairy, brewing, food, beverage, pharmaceutical, nutraceutical, and cosmetic production, which must frequently sanitize equipment.
[0002] COP systems, on the other hand, are disassembled for cleaning. This process can be time-consuming and labor-intensive, but is often necessary for equipment that is not suitable for cleaning using a CIP method. COP systems are commonly used in the pharmaceutical industry, which must thoroughly clean and sanitize equipment to avoid cross-contamination. The disassembled equipment is then cleaned manually or using a specialized cleaning system before being reassembled and returned to use.
[0003] While CIP and COP cleaning procedures are effective, they are not without challenges. For example, CIP systems rely on the flow of cleaning solution to effectively clean. Areas with low flow or insufficient contact with the cleaning solution can not be cleaned and can subsequently become a source of contamination or biofilm. If a plant is running a CIP procedure, the plant can not be aware of this source of contamination because of the nature of CIP procedures, which make it difficult to visually observe the interior of the equipment. COP equipment relies on the thoroughness of personnel to clean. If the cleaning is not thorough, missed spots can also become a source of contamination.
[0004] It is against this background that the present disclosure arises. SUMMARY
[0005] Various additional inventive aspects will be set forth in the description that follows. The aspects of the application can relate to individual features and to combinations of features. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the broad inventive concepts upon which the embodiments disclosed herein are based.
[0006] A method of testing a surface for organic matter or non-organic contaminants includes wiping the surface with a substrate; contacting the substrate with a solution comprising: an alkali hydroxide; one or more oxidizing compounds comprising sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or a monopersulfate salt; and one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, and combinations thereof; and detecting a colorimetric reaction on the substrate or in the solution.
[0007] Another embodiment is a method of testing water for organic matter or non-organic contaminants, the method comprising: obtaining a sample of a water source; mixing the sample with a solution comprising: an alkali hydroxide; one or more oxidizing compounds comprising sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or a monopersulfate salt; and one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, and combinations thereof; and detecting a colorimetric reaction in the solution.
[0008] Another embodiment is a kit for testing organic matter or non-organic contaminants, the kit comprising: a swab, a sponge, a wipe, or a test paper; a solution for detecting the presence of organic matter or non-organic contaminants, the solution comprising: an alkali hydroxide; one or more oxidizing compounds comprising sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or a monopersulfate salt; and one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, and sodium dichromate; and a test container configured to hold the solution, wherein the swab, sponge, wipe, or test paper contacts the solution. BRIEF DESCRIPTION OF DRAWINGS
[0009] The accompanying drawings, which are incorporated in and form a part of the description, illustrate several aspects of the present disclosure. A brief description of the drawings is as follows:
[0010] Figure 1 is a schematic method of testing a surface for organic matter or non-organic contaminants according to examples of the present disclosure.
[0011] Figure 2 is a schematic method of testing a liquid source for organic matter or non-organic contaminants according to examples of the present disclosure.
[0012] Figure 3A illustrates a color change produced by a solution comprising tea powder according to examples of the present disclosure.
[0013] Figure 3BColor changes resulting from solutions of milk having varying concentrations according to examples of the present disclosure are illustrated.
[0014] Figure 4A Graphical representation of the results of Example 2.
[0015] Figure 4B Graphical representation of the results of Example 2.
[0016] Figure 4C Graphical representation of the results of Example 2.
[0017] Figure 4D Graphical representation of the results of Example 2.
[0018] Figure 5A Graphical representation of the results of Example 3.
[0019] Figure 5B Graphical representation of the results of Example 3.
[0020] Figure 5C Graphical representation of the results of Example 3. DETAILED DESCRIPTION
[0021] As used herein, weight percent (wt.%), "percent by weight," "percent weight," and the like are synonymous with the term "concentration," refer to the concentration of a substance as the weight of that substance divided by the total weight of the composition and multiplied by 100.
[0022] As used herein, the term "about" to modify the amount of an ingredient in the compositions of the present application or used in the methods of the present application refers to variation in the numerical quantity due to experimental error, e.g., by typical measurement and liquid handling procedures used in preparing the solutions for use in the real world; by errors in these procedures due to inadvertience; by differences in the manufacturing, sourcing, or purity of the ingredients used to prepare the compositions or carry out the methods; and the like. The term about also encompasses amounts that differ due to different equilibration conditions for the compositions resulting from the particular starting mixture. Whether modified by the term "about" or not, the claims include equivalent values.
[0023] It should be noted that, as used in this specification and the appended claims, the singular forms "a," "an," and "the" include plural referents unless the content clearly dictates otherwise. Thus, for example, reference to a composition containing "a compound" includes a mixture of two or more compounds. It should also be noted that the term "or" is generally employed in its sense including "and / or" unless the content clearly dictates otherwise.
[0024] For the purpose of simplicity and clarity, any range of values recited in the specification is intended to encompass all values within the range, and is to be interpreted as supporting a requirement that any sub-range of values falling within the specified range is expressly disclosed. By way of illustration, a range of 1 to 5 as disclosed in the specification is to be interpreted to support a requirement that the claims cover any sub-range of values within the range of 1-5; 1-4; 1-3; 1-2; 2-5; 2-4; 2-3; 3-5; 3-4; and 4-5.
[0025] As used herein, "cleaning" refers to the removal of organic or inorganic soils. In some examples, "cleaning" can refer to any process that aids in the removal of soils, including bleaching, microbial population reduction, wiping, spraying, soaking, disinfecting, sterilizing, treatment with UV sterilization, oxidation, absorption, use of biochemical treatments, dilution, filtration, membrane filtration, treatment, application of antimicrobial agents, and combinations thereof.
[0026] As used herein, the term "consisting essentially of means the recited components, and excludes additional components that would affect the test of color change or cleaning ability of the cleaning agent disclosed herein, if present. The term "consisting essentially of can also refer to the components of a solution. For example, a solution can consist essentially of dichromate and would not include any other ingredients that would positively or negatively affect the solution's ability to change color, such as permanganate. As used herein, the term "consisting essentially of with respect to a method refers to the recited steps and excludes additional steps (or components, if the composition is included in the method), if present, that would affect the test of the surface or sample of the liquid.
[0027] Described herein are compositions and methods for rapidly verifying cleaning efficacy in CIP systems and COP systems. The compositions and methods of the present disclosure can be particularly suitable for systems where cleanliness of CIP systems and COP systems is important for safety and regulatory compliance, such as surfaces in food and beverage manufacturing, laboratory and pharmaceutical equipment, and high-traffic areas.
[0028] Many processes that clean using CIP methods and COP methods have difficult to remove soils, especially where the soils have been thermally degraded. The term "thermally degraded" is used to refer to materials that have been exposed to heat and thus have undergone a change in the chemical structure of the material, such as denaturation and cross-linking reactions of proteins, carbohydrates, fats, and oils. This is common in systems that heat materials during cooking, such as pasteurization of beverages. Other common soils that are cleaned with CIP methods and COP methods include organic substances, non-organic substances, proteins, fats, carbohydrates, starches, sugars, minerals, bacteria, viruses, biofilms, and complex soils that contain more than one type of soil. The term "organic substances" refers to carbon-containing compounds from living organisms and includes compounds from plants and animals. In particular, organic substances can refer to carbon-containing compounds used or produced in food and beverage production. Such organic substances can cause fouling, where the substances deposit on surfaces during food and beverage production.
[0029] While CIP systems and COP systems are designed to completely clean processing equipment, such as in the food, beverage, and pharmaceutical industries, the equipment is not always completely cleaned. This can occur if the solution in the CIP system or COP system does not contact the surface to be cleaned at all or for a long enough time, there is not enough mechanical action due to turbulence of the solution or impact from the spray, or if the solution does not have the cleaning performance required to completely clean the system. Cleaning solutions, especially in CIP systems, are often reused multiple times and thus over time, the solution loses its cleaning efficacy.
[0030] It can be desirable to test whether equipment and surfaces cleaned using CIP methods and COP methods have been sufficiently cleaned. Figure 1 An illustrative method 100 of verifying cleaning performance is shown. A surface is cleaned at step 110 using a CIP method or COP method known in the art. The cleaned surface is then wiped at step 112 with a substrate that will pick up any organic substances or non-organic soils on the surface. The substrate can be a wipe, a swab, an absorbent ball, a test paper, or any other suitable substrate. In some examples, the substrate is a single-use disposable substrate.
[0031] After wiping the surface, the substrate is contacted with a solution at step 114, which can be a concentrated solution or a diluted concentration solution. The solution can include an alkali hydroxide, such as sodium hydroxide, potassium hydroxide, and lithium hydroxide. In some examples, the solution includes a combination of alkali hydroxides. In some examples, the solution includes a single alkali hydroxide, such as sodium hydroxide or potassium hydroxide. The hydroxide-containing compound can provide alkalinity to the solution to allow for dissolution of the soil and a color change when the solution contacts the soil, which will be discussed in more detail below.
[0032] The solution can also include one or more oxidizing compounds including sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, monopersulfate, or combinations thereof.
[0033] The solution can also include one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, and sodium dichromate. The permanganate and dichromate containing compounds can act as oxidizing agents that produce color. For example, the permanganate can produce a purple, green, yellow, or other color depending on the level of organic matter or non-organic soils.
[0034] In some examples, the solution also includes potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphate salts, or combinations thereof. The tripolyphosphate salts act as water hardness scale inhibitors and chelating agents that prevent or minimize mineral deposits on surfaces due to dissolved minerals such as calcium and magnesium. Additionally, metal ions can be chelated to prevent deposition on surfaces.
[0035] In some examples, the solution further comprises up to 100% by weight of water. In some examples, the solution comprises from about 0.16% to about 99.9% by weight of water. In some examples, the solution comprises from about 0.16% to about 99% by weight of water, from about 0.16% to about 95% by weight of water, from about 0.16% to about 90% by weight of water, from about 0.16% to about 85% by weight of water, from about 0.16% to about 80% by weight of water, from about 0.16% to about 75% by weight of water, from about 0.16% to about 70% by weight of water, from about 0.16% to about 65% by weight of water, from about 0.16% to about 60% by weight of water, from about 0.16% to about 55% by weight of water, from about 0.16% to about 50% by weight of water, from about 0.16% to about 45% by weight of water, from about 0.16% to about 40% by weight of water, from about 0.16% to about 35% by weight of water, from about 0.16% to about 30% by weight of water, from about 0.16% to about 25% by weight of water, from about 0.16% to about 20% by weight of water, from about 0.16% to about 15% by weight of water, from about 0.16% to about 10% by weight of water, from about 0.16% to about 5% by weight of water, from about 0.16% to about 2.5% by weight of water, from about 0.16% to about 1% by weight of water, from about 0.16% to about 0.5% by weight of water, from about 0.5% to about 99.9% by weight of water, from about 1% to about 99.9% by weight of water, from about 2.5% to about 99.9% by weight of water, from about 5% to about 99.9% by weight of water, from about 10% to about 99.9% by weight of water, from about 15% to about 99.9% by weight of water, from about 20% to about 99.9% by weight of water, from about 25% to about 99.9% by weight of water, from about 30% to about 99.9% by weight of water, from about 35% to about 99.9% by weight of water, from about 40% to about 99.9% by weight of water, from about 45% to about 99.9% by weight of water, from about 50% to about 99.9% by weight of water, from about 55% to about 99.9% by weight of water, from about 60% to about 99.9% by weight of water, from about 65% to about 99.9% by weight of water, from about 70% to about 99.9% by weight of water, from about 75% to about 99.9% by weight of water, from about 80% to about 99.9% by weight of water, from about 85% to about 99.9% by weight of water, from about 90% to about 99.9% by weight of water, or from about 95% to about 99.9% by weight of water.
[0036] After the substrate has come into contact with the solution, at step 116, the presence or absence of a colorimetric reaction is detected on the substrate or in the solution. For example, a swab may be immersed in the solution, and the solution may have a colorimetric reaction that changes the color of the solution. In other examples, the substrate may be a test strip immersed in the solution, or the substrate may be placed on a test strip, and either the test strip or the substrate may produce a colorimetric reaction. A colorimetric reaction indicates the presence of organic or non-organic contaminants on the surface being tested. The absence of a colorimetric reaction indicates the absence of organic or non-organic contaminants on the surface being tested. The colorimetric reaction is discussed in more detail below.
[0037] If organic matter, non-organic contaminants, or biofilm are present on the surface, the surface can then be cleaned again at step 118 by repeating the CIP or COP method, or by other means such as wiping, spraying, soaking, UV sterilization, or a combination thereof. This method can be repeated until no color reaction is detected, indicating that the organic matter or non-organic contaminants have been successfully removed. In some examples, "cleaning" may mean cleaning the surface until the resulting color reaction and / or the absorbance reading obtained from the sample is below an acceptable contaminant threshold level. In some examples, "cleaning" may include applying an antimicrobial agent to the surface. In some examples, "cleaning" may include cleaning with an alkali. In some examples, "cleaning" may include cleaning with an acid. In some examples, "cleaning" may include switching from an alkaline or neutral composition to an acidic composition, or vice versa. Standard operating procedures may indicate specific absorbance readings or the number of RLUs acting as thresholds, where values above the threshold indicate unacceptable contaminant levels, and values below the threshold indicate acceptable contaminant levels.
[0038] The cleaning described herein can be performed using any suitable cleaning agent known in the art. Some non-limiting examples include peracids, peracetic acids, peroxyacetic acids, carboxylic acids, peroxycarboxylic acids, citric acid, lactic acid, peroxyoctanoic acid, methanesulfonic acid, organic acids (including monocarboxylic acids, dicarboxylic acids, and tricarboxylic acids, such as formic acid, butyric acid, valeric acid, hexanoic acid, itaconic acid, trichloroacetic acid, oxalic acid, terephthalic acid, citric acid, acetic acid, lactic acid, malonic acid, maleic acid, succinic acid, hydroxysuccinic acid, adipic acid, caprylic acid, fumaric acid, methacrylic acid, methylaminosulfonic acid, propionic acid, gluconic acid, glutamic acid, glutaric acid, benzoic acid, etc. Acids (tartaric acid, glycolic acid, and salicylic acid), inorganic acids (such as phosphoric acid, nitric acid, sulfuric acid, and aminosulfonic acid), quaternary ammonium compounds and their salts, sodium chlorite, alcohols (such as isopropanol and ethanol), hydrogen peroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, surfactants, sodium hypochlorite, calcium hypochlorite, chlorine dioxide, enzymes (such as proteases, lipases, cellulases, xylanases, and pectinsases), rinsing agents, combinations thereof, and any other suitable cleaning agents known in the art.
[0039] The solution can be prepared as a concentrate and diluted to a use solution. The concentrate contains varying amounts of each component. In some examples, the alkali metal hydroxide is present in the concentrate at approximately 0.1% to approximately 45% by weight. Alkali metal hydroxides may be present in concentrated solutions in amounts of about 0.1 wt% to about 40 wt%, about 0.1 wt% to about 35 wt%, about 0.1 wt% to about 30 wt%, about 0.1 wt% to about 25 wt%, about 0.1 wt% to about 20 wt%, about 0.1 wt% to about 15 wt%, about 0.1 wt% to about 10 wt%, about 0.1 wt% to about 5 wt%, about 0.1 wt% to about 2 wt%, about 0.1 wt% to about 1 wt%, about 0.5 wt% to about 45 wt%, about 1 wt% to about 45 wt%, about 2 wt% to about 45 wt%, about 5 wt% to about 45 wt%, about 10 wt% to about 45 wt%, about 15 wt% to about 45 wt%, about 20 wt% to about 45 wt%, about 25 wt% to about 45 wt%, about 30 wt% to about 45 wt%, about 35 wt% to about 45 wt%, or about 40 wt% to about 45 wt%.
[0040] In some examples, one or more oxidizing compounds are present in the concentrated solution at about 0.1 wt% to about 40 wt%. One or more oxidizing compounds may be present in the concentrated solution at about 0.1 wt% to about 35 wt%, about 0.1 wt% to about 30 wt%, about 0.1 wt% to about 25 wt%, about 0.1 wt% to about 20 wt%, about 0.1 wt% to about 15 wt%, about 0.1 wt% to about 10 wt%, about 0.1 wt% to about 5 wt%, about 0.1 wt% to about 2 wt%, about 0.1 wt% to about 1 wt%, about 0.5 wt% to about 40 wt%, about 1 wt% to about 40 wt%, about 2 wt% to about 40 wt%, about 5 wt% to about 40 wt%, about 10 wt% to about 40 wt%, about 15 wt% to about 40 wt%, about 20 wt% to about 40 wt%, about 25 wt% to about 40 wt%, about 30 wt% to about 40 wt%, or about 35 wt% to about 40 wt%.
[0041] In some examples, one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, and sodium dichromate are present in the concentrated solution at about 0.001 wt% to about 5 wt%. One or more compounds may be present at about 0.001 wt% to about 4.5 wt%, about 0.001 wt% to about 4 wt%, about 0.001 wt% to about 3.5 wt%, about 0.001 wt% to about 3 wt%, about 0.001 wt% to about 2.5 wt%, about 0.001 wt% to about 2 wt%, about 0.001 wt% to about 1.5 wt%, about 0.001 wt% to about 1 wt%, about 0.001 wt% to about 0.5 wt%, or about 0.001 wt% to about 0. It exists in the concentrated solution at 1 wt%, about 0.001 wt%, about 0.01 wt%, about 0.01 wt%, about 5 wt%, about 0.1 wt%, about 5 wt%, about 0.5 wt%, about 1 wt%, about 5 wt%, about 1.5 wt%, about 2 wt%, about 2.5 wt%, about 3 wt%, about 3.5 wt%, about 4 wt%, or about 4.5 wt% to about 5 wt%.
[0042] In some examples, potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof are present in the concentrated solution at about 0.01 wt% to about 6 wt%. Potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof may be present at about 0.01 wt% to about 5.5 wt%, about 0.01 wt% to about 5 wt%, about 0.01 wt% to about 4.5 wt%, about 0.01 wt% to about 4 wt%, about 0.01 wt% to about 3.5 wt%, about 0.01 wt% to about 3 wt%, about 0.01 wt% to about 2.5 wt%, about 0.01 wt% to about 2 wt%, about 0.01 wt% to about 1.5 wt%, about 0.01 wt% to about 1 wt%, about 0.01 wt% to about 1 wt%. It exists in the concentrated solution in amounts of about 0.5 wt%, about 0.01 wt%, about 0.1 wt%, about 0.1 wt%, about 0.5 wt%, about 6 wt%, about 1 wt%, about 6 wt%, about 1.5 wt%, about 6 wt%, about 2 wt%, about 2.5 wt%, about 6 wt%, about 3 wt%, about 3.5 wt%, about 6 wt%, about 4 wt%, about 4.5 wt%, about 6 wt%, about 5 wt%, or about 5.5 wt% to about 6 wt%.
[0043] The concentrated solution can be prepared by combining the amounts of components described above into a concentrated solution. In some examples, the concentrated solution is used as a test solution to perform the method without dilution. In other examples, the concentrated solution is diluted to approximately 1% to approximately 20% of the working solution. In some examples, the concentrated solution is diluted to approximately 4% of the working solution.
[0044] If the concentrated solution is diluted, the amount of each component in the solution will also be diluted. For example, as described above, the concentrated solution may contain about 0.1 wt% to about 45 wt% of an alkali metal hydroxide. If the concentrated solution is diluted to a 4% working solution, the amount of alkali metal hydroxide in the diluted working solution will be about 0.004 wt% to about 1.8 wt%. Therefore, if the concentrated solution is diluted to a 4% working solution, the amount of one or more oxidizing compounds will be about 0.004 wt% to about 1.6 wt%. If the concentrated solution is diluted to a 4% working solution, the amount of one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, and sodium dichromate will be about 0.00004 wt% to about 0.2 wt%. If the concentrated solution is diluted to a 4% working solution, the amount of potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof will be about 0.0004 wt% to about 0.24 wt%. This disclosure contemplates every integer value within these ranges.
[0045] The concentrated solution can be diluted to a working solution of approximately 1% to approximately 20%. The diluted solution within this dilution range may contain about 0.001 wt% to about 9 wt%, about 0.001 wt% to about 8 wt%, about 0.001 wt% to about 7 wt%, about 0.001 wt% to about 6 wt%, about 0.001 wt% to about 5 wt%, about 0.001 wt% to about 4 wt%, about 0.001 wt% to about 3 wt%, about 0.001 wt% to about 2 wt%, about 0.001 wt% to about 1 wt%, about 0.001 wt% to about 0.5 wt%, about 0.001 wt% to about 0.1 wt%, about 0.1 wt% to about 9 wt%, about 0.5 wt% to about 9 wt%, about 1 wt% to about 9 wt%, about 2 wt% to about 9 wt%, about 3 wt% to about 9 wt%, about 4 wt% to about 9 wt%, about 5 wt% to about 9 wt%, about 6 wt% to about 9 wt%, about 7 wt% to about 9 wt%, or about 8 wt% to about 9 wt% of alkali metal hydroxide.
[0046] The diluted working solution in the dilution range of about 1% to about 20% may contain one or more oxidizing compounds in the following proportions: about 0.001 wt% to about 8 wt%, about 0.001 wt% to about 7 wt%, about 0.001 wt% to about 6 wt%, about 0.001 wt% to about 5 wt%, about 0.001 wt% to about 4 wt%, about 0.001 wt% to about 3 wt%, about 0.001 wt% to about 2 wt%, about 0.001 wt% to about 1 wt%, about 0.001 wt% to about 0.5 wt%, about 0.001 wt% to about 0.1 wt%, about 0.1 wt% to about 8 wt%, about 0.5 wt% to about 8 wt%, about 1 wt% to about 8 wt%, about 2 wt% to about 8 wt%, about 3 wt% to about 8 wt%, about 4 wt% to about 8 wt%, about 5 wt% to about 8 wt%, about 6 wt% to about 8 wt%, or about 7 wt% to about 8 wt%.
[0047] The diluted solution for use, within a dilution range of about 1% to about 20%, may contain about 0.00001 wt% to about 1 wt%, about 0.00001 wt% to about 0.5 wt%, about 0.00001 wt% to about 0.1 wt%, about 0.00001 wt% to about 0.01 wt%, about 0.00001 wt% to about 0.005 wt%, about 0.00001 wt% to about 0.001 wt%, about 0.00001 wt% to about 0.0005 wt%, and about 0.00001 wt% to about 0.0001 wt%. The percentage by weight, from about 0.00001% by weight to about 0.00005% by weight, from about 0.00005% by weight to about 1% by weight, from about 0.0001% by weight to about 1% by weight, from about 0.0005% by weight to about 1% by weight, from about 0.001% by weight to about 1% by weight, from about 0.005% by weight to about 1% by weight, from about 0.01% by weight to about 1% by weight, from about 0.1% by weight to about 1% by weight, or some from about 0.5% by weight to about 1% by weight of one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate and sodium dichromate.
[0048] The diluted solution for use in the dilution range of about 1% to about 20% may contain about 0.0001 wt% to about 1.2 wt%, about 0.0001 wt% to about 1 wt%, about 0.0001 wt% to about 0.5 wt%, about 0.0001 wt% to about 0.1 wt%, about 0.0001 wt% to about 0.05 wt%, about 0.0001 wt% to about 0.01 wt%, about 0.0001 wt% to about 0.005 wt%, about 0.0001 wt% to about 0.001 wt%, about 0.0001 wt% to about 0.0005 wt%, about 0.0005 wt% to about 1.2 wt%, about 0.001 wt% to about 1.2 wt%, about 0.005 wt% to about 1.2 wt%, about 0.01 wt% to about 1.2 wt%, about 0.05 wt% to about 1.2 wt%, about 0.1 wt% to about 1.2 wt%, about 0.5 wt% to about 1.2 wt%, or some about 1 wt% to about 1.2 wt% of potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof.
[0049] In some examples, the concentrated solution or the working solution may have a pH of about 9.5 to about 13.5. In some examples, the concentrated solution or the working solution may have a pH of about 9.5 to about 13, about 9.5 to about 12, about 9.5 to about 11, about 9.5 to about 10, about 10 to about 13.5, about 11 to about 13.5, or about 12 to about 13.5.
[0050] As used herein, unless otherwise indicated, "solution" may refer to a concentrated solution, a diluted working solution, or both. When a solution comes into contact with a substrate, a color reaction occurs if organic matter or non-organic contaminants are present. The color change resulting from the color reaction will depend on the components contained in the solution. For example, if the solution contains potassium permanganate, sodium permanganate, or another permanganate compound, the solution may be purple before contacting a substrate containing organic matter or non-organic contaminants. If a permanganate-containing solution comes into contact with a substrate containing organic matter or non-organic contaminants, a color reaction occurs, changing the purple color to green, yellow, or light purple. In other examples, if the solution contains a dichromate compound, the solution will be orange before contacting the substrate. If a dichromate-containing solution comes into contact with a substrate containing organic matter or non-organic contaminants, a color reaction occurs, changing the orange solution to green.
[0051] In some examples, the color reaction occurs in less than 30 minutes, less than 20 minutes, less than 10 minutes, less than 5 minutes, less than 1 minute, less than 30 seconds, or less than 10 seconds. Figure 3A Examples of colorimetric reactions after 10 minutes are shown. In some examples, colorimetric reactions are observed at temperatures ranging from approximately 10°C to approximately 60°C. In some examples, colorimetric reactions are observed at temperatures ranging from approximately 10°C to approximately 55°C, approximately 10°C to approximately 50°C, approximately 10°C to approximately 45°C, approximately 10°C to approximately 40°C, approximately 10°C to approximately 35°C, approximately 10°C to approximately 30°C, approximately 10°C to approximately 25°C, approximately 10°C to approximately 20°C, approximately 10°C to approximately 15°C, approximately 15°C to approximately 60°C, approximately 20°C to approximately 60°C, approximately 25°C to approximately 60°C, approximately 30°C to approximately 60°C, approximately 35°C to approximately 60°C, approximately 40°C to approximately 60°C, approximately 45°C to approximately 60°C, approximately 50°C to approximately 60°C, or approximately 55°C to approximately 60°C. In some examples, colorimetric reactions are observed at room temperature, which is approximately 15°C to approximately 25°C.
[0052] In some examples, the colorimetric reaction is observed visually with the eye. In other examples, instruments such as color comparators, colorimeters, or spectrometers can be used to observe the colorimetric reaction. A color comparator or colorimeter measures the color change by evaluating the wavelength of light produced by the colorimetric reaction in the visible spectrum. In some examples, the colorimetric reaction is measured between approximately 400 nm and approximately 700 nm. A color comparator or colorimeter, or any other instrument suitable for reading absorbance wavelengths, can detect the colorimetric reaction and measure the absorbance of the color after the colorimetric reaction. In some examples, a control sample without a colorimetric reaction can be measured by the instrument and compared to the solution or substrate after the colorimetric reaction. The absorbance after coloring and / or color change can be evaluated using digital imaging or graphical analysis. In some examples, software or computer programs associated with the instrument can measure the change in absorbance before and after the colorimetric reaction. In some examples, the instrument can be a portable instrument that can be used by ordinary users, such as cleaners or technicians.
[0053] In some examples, "color change" refers to a color change visible to the human eye. In other examples, "color change" refers to a color change that can be measured by an instrument. Color change can be quantified in units of absorbance (AU) or in nanometers (nm) of wavelength change. In some examples, color change can be quantified by an instrument in ppm and then converted to units of absorbance.
[0054] In some examples, a color change occurs if there is a wavelength change of 5 nm or greater, 10 nm or greater, 15 nm or greater, 20 nm or greater, 25 nm or greater, 40 nm or greater, 50 nm or greater, or 100 nm or greater. In some examples, a color change occurs if there is a change in the absorbance unit of the sample measured by the instrument. This color change can be 0.1 absorbance units or more, 0.2 absorbance units or more, 0.3 absorbance units or more, 0.4 absorbance units or more, 0.5 absorbance units or more, 0.7 absorbance units or more, or 1 absorbance unit or more.
[0055] The method described above can be used with CIP (Clean-In-Place) or COP (Clean-Out-of-Place) systems. In some examples, CIP systems are located in food factories, beverage factories, or pharmaceutical factories. In some examples, the method is used to test surfaces in food factories, beverage factories, pharmaceutical factories, hospitals, kitchens, hotels, laboratories, or offices. This method can be used to verify cleaning effectiveness on any surface that may have organic or non-organic contaminants.
[0056] In some examples, the solution used to test the surface does not contact the surface. For example, a sterile substrate such as a swab can be used to wipe the surface to be tested, and the swab can be immersed in the solution to produce a colorimetric reaction. In such examples, the solution does not contact the surface, and rinsing the surface is not required after the test. In other examples, the solution can contact the substrate, and then the substrate contacts the surface to be tested. For example, the solution can be preloaded onto a swab and then wiped onto the surface to be tested. In such examples, a colorimetric reaction can occur on the swab, which can be observed visually or with instruments. The solution does not contain organic matter, and therefore even if the solution contacts the surface, it does not need to be rinsed off the surface after the test.
[0057] In some examples, method 100 for verifying cleaning performance uses a solution substantially composed of an alkali metal hydroxide, one or more oxidizing compounds, and one or more other compounds, wherein the one or more oxidizing compounds include sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, and combinations thereof. In some examples, the solution substantially composed of an alkali metal hydroxide, one or more oxidizing compounds, and one or more other compounds, wherein the one or more oxidizing compounds include sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, selected from the group consisting of potassium permanganate, sodium permanganate, and combinations thereof. In some examples, the solution substantially composed of an alkali metal hydroxide, one or more oxidizing compounds, and one or more other compounds, wherein the one or more oxidizing compounds include sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, selected from the group consisting of potassium dichromate, sodium dichromate, and combinations thereof.
[0058] This article also discloses a method 200 for testing organic or non-organic contaminants from liquid sources, such as... Figure 2 As shown. The liquid may include water, saline solution, beverage, sterile liquid, or any other liquid containing organic or non-organic contaminants to be tested. At step 210, a sample of the liquid is obtained from the liquid source, and at step 212, the sample is mixed with a solution for testing the organic or non-organic contaminants of the liquid source. The solution may contain alkali metal hydroxides, such as sodium hydroxide, potassium hydroxide, and lithium hydroxide. In some examples, the solution contains a combination of alkali metal hydroxides. In some examples, the solution contains a single alkali metal hydroxide, such as sodium hydroxide or potassium hydroxide.
[0059] The solution may also contain one or more oxidizing compounds, including sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, monopersulfate, or combinations thereof. The solution may also contain one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, and sodium dichromate. In some examples, the solution also contains potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof. In some examples, the solution also contains up to 100% by weight water.
[0060] After the sample and solution are mixed, a colorimetric reaction is detected at step 214 to determine the presence or absence of a colorimetric reaction in the solution. A colorimetric reaction indicates the presence of organic or non-organic contaminants in the tested liquid sample. The absence of a colorimetric reaction indicates the absence of organic or non-organic contaminants in the liquid sample. If organic or non-organic contaminants are present in the liquid sample, at step 216, the liquid source may be cleaned or replaced to remove the organic or non-organic contaminants. Cleaning may include removing organic or non-organic contaminants by oxidation, absorption, use of biochemical treatment, dilution, filtration, membrane filtration, treatment, UV sterilization, application of antimicrobial agents, combinations thereof, or any other suitable cleaning method known in the art. In some examples, it may be necessary to replace the liquid source instead of cleaning to remove organic or non-organic contaminants. This method may be repeated until no colorimetric reaction is detected after cleaning the liquid source, indicating that the organic or non-organic contaminants have been successfully removed. In some examples, this method is repeated until the level of organic or non-organic contaminants is below an acceptable contaminant threshold.
[0061] The cleaning described herein can be performed using any suitable cleaning agent known in the art. Some non-limiting examples include peracids, peracetic acids, peroxyacetic acids, carboxylic acids, peroxycarboxylic acids, citric acid, lactic acid, peroxyoctanoic acid, methanesulfonic acid, organic acids (including monocarboxylic acids, dicarboxylic acids, and tricarboxylic acids, such as formic acid, butyric acid, valeric acid, hexanoic acid, itaconic acid, trichloroacetic acid, oxalic acid, terephthalic acid, citric acid, acetic acid, lactic acid, malonic acid, maleic acid, succinic acid, hydroxysuccinic acid, adipic acid, caprylic acid, fumaric acid, methacrylic acid, methylaminosulfonic acid, propionic acid, gluconic acid, glutamic acid, glutaric acid, benzoic acid, etc. Acids (tartaric acid, glycolic acid, and salicylic acid), inorganic acids (such as phosphoric acid, nitric acid, sulfuric acid, and aminosulfonic acid), quaternary ammonium compounds and their salts, sodium chlorite, alcohols (such as isopropanol and ethanol), hydrogen peroxide, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, surfactants, sodium hypochlorite, calcium hypochlorite, chlorine dioxide, enzymes (such as proteases, lipases, cellulases, xylanases, and pectinsases), rinsing agents, combinations thereof, and any other suitable cleaning agents known in the art.
[0062] In some examples, the solution used for testing is not added directly to the liquid source. Instead, a sample is removed from the liquid source and mixed with the solution used for testing, preventing contamination of the liquid source. This can be beneficial for large volumes of liquids, such as large containers of deionized water, where small samples can be removed for testing without adding anything to the entire liquid source.
[0063] The solution contains varying amounts of each component. In some examples, alkali metal hydroxides are present in the solution at approximately 0.1% to approximately 45% by weight. Alkali metal hydroxides may be present in solution in amounts of about 0.1 wt% to about 40 wt%, about 0.1 wt% to about 35 wt%, about 0.1 wt% to about 30 wt%, about 0.1 wt% to about 25 wt%, about 0.1 wt% to about 20 wt%, about 0.1 wt% to about 15 wt%, about 0.1 wt% to about 10 wt%, about 0.1 wt% to about 5 wt%, about 0.1 wt% to about 2 wt%, about 0.1 wt% to about 1 wt%, about 0.5 wt% to about 45 wt%, about 1 wt% to about 45 wt%, about 2 wt% to about 45 wt%, about 5 wt% to about 45 wt%, about 10 wt% to about 45 wt%, about 15 wt% to about 45 wt%, about 20 wt% to about 45 wt%, about 25 wt% to about 45 wt%, about 30 wt% to about 45 wt%, about 35 wt% to about 45 wt%, or about 40 wt% to about 45 wt%.
[0064] In some examples, one or more oxidizing compounds are present in solution at about 0.1 wt% to about 40 wt%. One or more oxidizing compounds may be present in solution at about 0.1 wt% to about 35 wt%, about 0.1 wt% to about 30 wt%, about 0.1 wt% to about 25 wt%, about 0.1 wt% to about 20 wt%, about 0.1 wt% to about 15 wt%, about 0.1 wt% to about 10 wt%, about 0.1 wt% to about 5 wt%, about 0.1 wt% to about 2 wt%, about 0.1 wt% to about 1 wt%, about 0.5 wt% to about 40 wt%, about 1 wt% to about 40 wt%, about 2 wt% to about 40 wt%, about 5 wt% to about 40 wt%, about 10 wt% to about 40 wt%, about 15 wt% to about 40 wt%, about 20 wt% to about 40 wt%, about 25 wt% to about 40 wt%, about 30 wt% to about 40 wt%, or about 35 wt% to about 40 wt%.
[0065] In some examples, one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, and sodium dichromate are present in solution at about 0.001 wt% to about 5 wt%. One or more compounds may be present at about 0.001 wt% to about 4.5 wt%, about 0.001 wt% to about 4 wt%, about 0.001 wt% to about 3.5 wt%, about 0.001 wt% to about 3 wt%, about 0.001 wt% to about 2.5 wt%, about 0.001 wt% to about 2 wt%, about 0.001 wt% to about 1.5 wt%, about 0.001 wt% to about 1 wt%, about 0.001 wt% to about 0.5 wt%, about 0.001 wt% to about 0. It exists in solution in the form of 0.1% by weight, about 0.001% by weight to about 0.01% by weight, about 0.01% by weight to about 5% by weight, about 0.1% by weight to about 5% by weight, about 0.5% by weight to about 5% by weight, about 1% by weight to about 5% by weight, about 1.5% by weight to about 5% by weight, about 2% by weight to about 5% by weight, about 2.5% by weight to about 5% by weight, about 3% by weight to about 5% by weight, about 3.5% by weight to about 5% by weight, about 4% by weight to about 5% by weight, or about 4.5% by weight to about 5% by weight.
[0066] In some examples, potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof are present in solution at about 0.01 wt% to about 6 wt%. Potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof may be present at about 0.01 wt% to about 5.5 wt%, about 0.01 wt% to about 5 wt%, about 0.01 wt% to about 4.5 wt%, about 0.01 wt% to about 4 wt%, about 0.01 wt% to about 3.5 wt%, about 0.01 wt% to about 3 wt%, about 0.01 wt% to about 2.5 wt%, about 0.01 wt% to about 2 wt%, about 0.01 wt% to about 1.5 wt%, about 0.01 wt% to about 1 wt%, about 0.01 wt%. It exists in solution in the form of about 0.5 wt%, about 0.01 wt%, about 0.1 wt%, about 0.1 wt%, about 6 wt%, about 0.5 wt%, about 6 wt%, about 1 wt%, about 6 wt%, about 1.5 wt%, about 6 wt%, about 2 wt%, about 2.5 wt%, about 6 wt%, about 3 wt%, about 3.5 wt%, about 6 wt%, about 4 wt%, about 4.5 wt%, about 6 wt%, about 5 wt%, or about 5.5 wt% to about 6 wt%.
[0067] The solution can be prepared by combining the components into a concentrated solution. In some examples, the concentrated solution is used as a test solution to perform the method without dilution. In other examples, the concentrated solution is diluted to approximately 1% to approximately 20% of the working solution. In some examples, the concentrated solution is diluted to approximately 4% of the working solution.
[0068] If the concentrated solution is diluted, the amount of each component in the solution will also be diluted. For example, as described above, the concentrated solution may contain about 0.1 wt% to about 45 wt% of an alkali metal hydroxide. If the concentrated solution is diluted to a 4% working solution, the amount of alkali metal hydroxide in the diluted working solution will be about 0.004 wt% to about 1.8 wt%. Therefore, if the concentrated solution is diluted to a 4% working solution, the amount of one or more oxidizing compounds will be about 0.004 wt% to about 1.6 wt%. If the concentrated solution is diluted to a 4% working solution, the amount of one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, and sodium dichromate will be about 0.00004 wt% to about 0.2 wt%. If the concentrated solution is diluted to a 4% working solution, the amount of potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof will be about 0.0004 wt% to about 0.24 wt%. This disclosure contemplates every integer value within these ranges.
[0069] The concentrated solution can be diluted to a working solution of approximately 1% to approximately 20%. The diluted solution within this dilution range may contain about 0.001 wt% to about 9 wt%, about 0.001 wt% to about 8 wt%, about 0.001 wt% to about 7 wt%, about 0.001 wt% to about 6 wt%, about 0.001 wt% to about 5 wt%, about 0.001 wt% to about 4 wt%, about 0.001 wt% to about 3 wt%, about 0.001 wt% to about 2 wt%, about 0.001 wt% to about 1 wt%, about 0.001 wt% to about 0.5 wt%, about 0.001 wt% to about 0.1 wt%, about 0.1 wt% to about 9 wt%, about 0.5 wt% to about 9 wt%, about 1 wt% to about 9 wt%, about 2 wt% to about 9 wt%, about 3 wt% to about 9 wt%, about 4 wt% to about 9 wt%, about 5 wt% to about 9 wt%, about 6 wt% to about 9 wt%, about 7 wt% to about 9 wt%, or about 8 wt% to about 9 wt% of alkali metal hydroxide.
[0070] The diluted working solution in the dilution range of about 1% to about 20% may contain one or more oxidizing compounds in the following proportions: about 0.001 wt% to about 8 wt%, about 0.001 wt% to about 7 wt%, about 0.001 wt% to about 6 wt%, about 0.001 wt% to about 5 wt%, about 0.001 wt% to about 4 wt%, about 0.001 wt% to about 3 wt%, about 0.001 wt% to about 2 wt%, about 0.001 wt% to about 1 wt%, about 0.001 wt% to about 0.5 wt%, about 0.001 wt% to about 0.1 wt%, about 0.1 wt% to about 8 wt%, about 0.5 wt% to about 8 wt%, about 1 wt% to about 8 wt%, about 2 wt% to about 8 wt%, about 3 wt% to about 8 wt%, about 4 wt% to about 8 wt%, about 5 wt% to about 8 wt%, about 6 wt% to about 8 wt%, or about 7 wt% to about 8 wt%.
[0071] The diluted solution for use, within a dilution range of about 1% to about 20%, may contain about 0.00001 wt% to about 1 wt%, about 0.00001 wt% to about 0.5 wt%, about 0.00001 wt% to about 0.1 wt%, about 0.00001 wt% to about 0.01 wt%, about 0.00001 wt% to about 0.005 wt%, about 0.00001 wt% to about 0.001 wt%, about 0.00001 wt% to about 0.0005 wt%, and about 0.00001 wt% to about 0.0001 wt%. The percentage by weight, from about 0.00001% by weight to about 0.00005% by weight, from about 0.00005% by weight to about 1% by weight, from about 0.0001% by weight to about 1% by weight, from about 0.0005% by weight to about 1% by weight, from about 0.001% by weight to about 1% by weight, from about 0.005% by weight to about 1% by weight, from about 0.01% by weight to about 1% by weight, from about 0.1% by weight to about 1% by weight, or some from about 0.5% by weight to about 1% by weight of one or more compounds selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate and sodium dichromate.
[0072] The diluted solution for use in the dilution range of about 1% to about 20% may contain about 0.0001 wt% to about 1.2 wt%, about 0.0001 wt% to about 1 wt%, about 0.0001 wt% to about 0.5 wt%, about 0.0001 wt% to about 0.1 wt%, about 0.0001 wt% to about 0.05 wt%, about 0.0001 wt% to about 0.01 wt%, about 0.0001 wt% to about 0.005 wt%, about 0.0001 wt% to about 0.001 wt%, about 0.0001 wt% to about 0.0005 wt%, about 0.0005 wt% to about 1.2 wt%, about 0.001 wt% to about 1.2 wt%, about 0.005 wt% to about 1.2 wt%, about 0.01 wt% to about 1.2 wt%, about 0.05 wt% to about 1.2 wt%, about 0.1 wt% to about 1.2 wt%, about 0.5 wt% to about 1.2 wt%, or some about 1 wt% to about 1.2 wt% of potassium tripolyphosphate, sodium tripolyphosphate, other tripolyphosphates, or combinations thereof.
[0073] In some examples, the solution may have a pH of about 9.5 to about 13.5. In some examples, the solution may have a pH of about 9.5 to about 13, about 9.5 to about 12, about 9.5 to about 11, about 9.5 to about 10, about 10 to about 13.5, about 11 to about 13.5, or about 12 to about 13.5.
[0074] When a solution and a liquid sample are mixed, a color reaction occurs if organic matter or non-organic contaminants are present. This color reaction will depend on the components contained in the solution. For example, if the solution contains potassium permanganate, sodium permanganate, or another permanganate compound, the solution may be purple before contacting it with a liquid sample containing organic matter or non-organic contaminants. If the permanganate-containing solution is contacted with a liquid sample containing organic matter or non-organic contaminants, a color reaction occurs, changing the purple color to green or yellow. In other examples, if the solution contains dichromate, the solution will be orange before contacting the liquid sample. If the dichromate-containing solution is contacted with a liquid sample containing organic matter or non-organic contaminants, a color reaction occurs, changing the orange solution to green.
[0075] In some examples, the colorimetric reaction occurs within less than 30 minutes, less than 20 minutes, less than 10 minutes, less than 5 minutes, less than 1 minute, or less than 30 seconds. In some examples, the colorimetric reaction is observed at temperatures from about 10°C to about 60°C. In some examples, the colorimetric reaction is observed at temperatures from about 10°C to about 55°C, from about 10°C to about 50°C, from about 10°C to about 45°C, from about 10°C to about 40°C, from about 10°C to about 35°C, from about 10°C to about 30°C, from about 10°C to about 25°C, from about 10°C to about 20°C, from about 10°C to about 15°C, from about 15°C to about 60°C, from about 20°C to about 60°C, from about 25°C to about 60°C, from about 30°C to about 60°C, from about 35°C to about 60°C, from about 40°C to about 60°C, from about 45°C to about 60°C, from about 50°C to about 60°C, or from about 55°C to about 60°C. In some examples, a colorimetric reaction was observed at room temperature, which is approximately 15°C to approximately 25°C.
[0076] In some examples, the colorimetric reaction is observed visually with the eye. In other examples, instruments such as color comparators or colorimeters can be used to observe the colorimetric reaction. A color comparator or colorimeter measures the color change by evaluating the wavelength of light produced in the visible spectrum. In some examples, the colorimetric reaction is measured between approximately 400 nm and approximately 700 nm. A color comparator or colorimeter, or any other instrument suitable for reading absorbance wavelengths, can detect the colorimetric reaction and measure the absorbance of the color after the colorimetric reaction. In some examples, a control sample of the solution can be measured by the instrument and compared with the solution after the colorimetric reaction. The absorbance after coloring and / or color change can be evaluated using digital imaging or graphical analysis. In some examples, software or computer programs associated with the instrument can measure the change in absorbance before and after the colorimetric reaction. In some examples, the instrument can be a portable instrument that can be used by ordinary users, such as cleaners or technicians.
[0077] In some examples, "color change" refers to a color change visible to the human eye. In other examples, "color change" refers to a color change that can be measured by an instrument. Color change can be quantified in units of absorbance (AU) or in nanometers (nm) of wavelength change. In some examples, color change can be quantified by an instrument in ppm and then converted to units of absorbance.
[0078] In some examples, a color change occurs if there is a wavelength change of 5 nm or greater, 10 nm or greater, 15 nm or greater, 20 nm or greater, 25 nm or greater, 40 nm or greater, 50 nm or greater, or 100 nm or greater. In some examples, a color change occurs if there is a change in the absorbance unit of the sample measured by the instrument. This color change can be 0.1 absorbance units or more, 0.2 absorbance units or more, 0.3 absorbance units or more, 0.4 absorbance units or more, 0.5 absorbance units or more, 0.7 absorbance units or more, or 1 absorbance unit or more.
[0079] In some examples, method 200 for testing organic or non-organic contaminants in a liquid uses a solution substantially composed of an alkali metal hydroxide, one or more oxidizing compounds, and one or more other compounds, including sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, and combinations thereof. In some examples, the solution substantially composed of an alkali metal hydroxide, one or more oxidizing compounds, and one or more other compounds, including sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, selected from the group consisting of potassium permanganate, sodium permanganate, and combinations thereof. In some examples, the solution substantially composed of an alkali metal hydroxide, one or more oxidizing compounds, and one or more other compounds, including sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, selected from the group consisting of potassium dichromate, sodium dichromate, and combinations thereof.
[0080] The methods described above can be used with CIP or COP systems, or any setup described above. In some examples, the method is specifically used to test the liquid source for organic or non-organic contaminants before the liquid is used in a sterile environment. For example, the liquid source could be deionized water intended for laboratory testing, which must be free of any organic or non-organic contaminants or other pollutants. In some examples, the liquid source is water or saline solution intended for use in a hospital or clinical setting. In some examples, the liquid source is water or saline solution intended for use in pharmaceutical preparation or medical procedures. In some examples, the liquid source is beverages, such as dairy or brewed products, that are susceptible to contamination, bacterial growth, or other contaminants that could lead to foodborne illnesses.
[0081] The methods described above can be used in CIP or COP cleaning settings to quickly verify that surfaces have been adequately cleaned to remove organic or inorganic contaminants. This method can be used with instruments that measure the absorbance of the colorimetric reaction produced using the solutions described herein. Users of this method can adapt it to a specific industry and set thresholds for acceptable absorbance readings associated with the presence of organic or inorganic contaminants. For example, a user in the beverage industry might determine that a certain level of organic or inorganic contaminants is acceptable in their CIP or COP system and calibrate the instrument to measure absorbance exceeding a specific value and alert the user that the amount of organic matter exceeds the acceptable threshold. In another example, a user in the pharmaceutical industry or a user producing brine might determine that any organic or inorganic contaminants are unacceptable in their CIP or COP system and calibrate the instrument to a sensitivity that measures absorbance and detects any increase in absorbance exceeding a baseline level. The methods and kits described herein are intended for setting permissible thresholds for organic or inorganic contaminants based on industry and user needs.
[0082] In some examples, the threshold for acceptable absorbance readings may correspond to contamination levels of up to 0 ppm, up to 10 ppm, up to 50 ppm, up to 100 ppm, up to 500 ppm, up to 1,000 ppm, or up to 10,000 ppm. These thresholds indicate that if the contamination level is at or below the threshold level, the surface or solution being tested is considered clean. If the contamination exceeds the threshold, the surface or solution is considered unclean. For example, a pharmaceutical plant might set the acceptable contamination threshold to 0 ppm to maintain sterile conditions for its drugs, while a food and beverage plant might have a threshold level of 1,000 ppm, or perhaps no contamination at all. In some examples, the threshold may also refer to a visual inspection, comparing a swab taken from a clean surface with one taken from the surface being tested to see if there are any visual changes on the swab.
[0083] This document also describes kits comprising the components described above to perform the methods disclosed herein. In some examples, the kit includes a substrate, such as a swab, absorbent bulb, swab, test strip, or other suitable substrate. The kit may also include a solution for detecting the presence of organic or non-organic contaminants. In some examples, the solution is the same as described above for the methods described herein. The kit may also include a test container configured to contain the solution, such as a beaker, aliquot tubes, sample cards, or any other suitable container. The container is configured to contain the solution, wherein a substrate such as an absorbent bulb, swab, or test strip is in contact with the solution. The colorimetric reaction may occur in the solution in the test container or on the substrate. The details of the methods described above apply to kits for testing organic or non-organic contaminants. The kit is intended for use in performing the methods described above.
[0084] The following non-limiting embodiments are provided as exemplary implementations of the invention. Although the numerical ranges and parameters illustrating the broad scope of the invention are approximate, the values described in the specific embodiments are reported as precisely as possible. However, any numerical value inherently contains some error, which is necessarily caused by the standard deviation found in its corresponding test measurement. These embodiments are illustrative and may only show a limited number of the components described above. For the sake of brevity, only a few embodiments are shown, but the full range of quantities of the components described above is contemplated.
[0085] Example
[0086] Example 1 : Preparation of the solution
[0087] The rapid cleaning validation method described herein is used to test for the presence of organic or non-organic contaminants in a CIP or COP system. In this embodiment, a solution is prepared by combining the components described in Table 1 below. The solutions in Table 1 are prepared to form a concentrated solution. The concentrated solution is diluted to a 4% working solution before use.
[0088] Table 1 : Preparation of the test solution .
[0089]
[0090] Example 2: Testing of milk samples
[0091] Ten 500 mL beakers were filled with 100 mL of the working solution from Example 1. One beaker was left untreated as a blank sample for comparison with the other samples. The remaining nine beakers each contained whole milk added in increasing amounts of 10 ppm, 20 ppm, 30 ppm, 40 ppm, 50 ppm, 100 ppm, 500 ppm, 1000 ppm, and 10,000 ppm. The control beaker and the nine test beakers were arranged in ascending order of concentration from right to left, and photographs were taken for visual observation of the colorimetric reaction after 20 minutes. A schematic diagram of the results in the beakers with concentrations of 10 ppm, 20 ppm, 30 ppm, 40 ppm, 50 ppm, 100 ppm, 1000 ppm, and 10,000 ppm is shown below. Figure 3B The control sample retained its initial purple color, while the milk at concentrations of 10 ppm to 100 ppm showed minimal change in purple hue upon visual observation. Beakers containing milk at 1000 ppm and 10,000 ppm showed a colorimetric reaction from the initial purple of the solution to a greenish hue. The beakers were observed again after 60 minutes to assess further color changes in the colorimetric reaction.
[0092] 10 mL of each solution was transferred to 10 mL vials, and the absorbance of each solution was read using a HACH DR 890 portable colorimeter instrument according to procedure #41. This procedure is used to detect dissolved manganese in the solution and provides absorbance readings compared to a control sample with 0 ppm milk. Table 2 shows the absorbance readings using the HACH DR 890 for each of the ten vials after 20 minutes and 60 minutes. For milk concentrations greater than 100 ppm, a color change is visually observable, and a colorimeter is not required to observe the presence of milk. At concentrations of 100 ppm or lower, a colorimeter is advantageous for measuring the presence of milk that is not visually observable. Using a colorimeter, a change in absorbance reading relative to the control sample indicates the presence of milk. Colorimeter readings can be affected by milk turbidity at concentrations above 100 ppm, so visual observation may be preferred in some cases.
[0093] Table 2: HACH DR 890 absorbance readings
[0094]
[0095] The samples were also measured using a benchtop Shimadzu UV-3101PC UV-VIS-NIR spectrophotometer. Color was measured at various wavelengths from 400 nm to 700 nm after 20 minutes and after 60 minutes. Figure 4AThe absorbance of all nine samples of milk with values ranging from 0 ppm to 10,000 ppm is shown, measured at wavelengths between 280 nm and 700 nm at 20 minutes and 60 minutes. Figure 4B The graph shows the absorbance of milk samples with concentrations of 0 ppm, 10 ppm, and 50 ppm, measured at wavelengths from 400 nm to 700 nm after 20 minutes. When the milk concentration was below 100 ppm, the absorbance decreased in the range of 480 nm to 570 nm, but when the milk concentration increased to above 100 ppm, an increase in absorbance was measured in both the 480 nm to 570 nm and 580 nm to 700 nm ranges.
[0096] Figure 4C The absorbance at 528 nm and 620 nm is shown for milk concentrations from 0 ppm to 1000 ppm. The graph illustrates a linear relationship between absorbance and milk concentration below 100 ppm. This is useful because concentrations of milk or other organic or non-organic contaminants below 100 ppm typically do not produce visually observable results.
[0097] Figure 4D The absorbance measurements of a sample containing 50 ppm emulsion at 400 nm to 700 nm, taken at 20 and 60 minutes, are shown. The absorbance in a single sample varies with various wavelengths and over time. At almost all absorbance values, the absorbance of the sample after 20 minutes differs from that measured after 60 minutes. Therefore, for all samples tested, including blank controls for comparison, absorbance readings should be taken at the same elapsed time intervals.
[0098] Example 3: Testing of tea samples
[0099] Using the solution described in Example 1 and the method described in Example 2, the colorimetric reactions of various concentrations of black tea powder were tested using the methods and solutions described herein. Nine 500 mL beakers were filled with 100 mL of the working solution and contained the following amounts of black tea powder: 0 ppm, 10 ppm, 20 ppm, 30 ppm, 40 ppm, 50 ppm, 100 ppm, 500 ppm, and 1000 ppm. The absorbance of each sample was measured using a Shimadzu UV-3101PC UV-VIS-NIR spectrophotometer at 20 minutes from the start of the colorimetric reaction (i.e., when the black tea powder was added to the working solution), and at 60 minutes for wavelengths from 400 nm to 700 nm at 10 ppm, 20 ppm, 30 ppm, 40 ppm, and 50 ppm, as shown in the figure. Figure 5A . Figure 5BThe absorbance of samples with 0 ppm, 10 ppm, 50 ppm and 100 ppm, measured at 400 nm to 700 nm after 20 minutes, is shown. Figure 5C The absorbance at 528 nm and 620 nm is shown for black tea concentrations from 0 ppm to 100 ppm. The results show that the preferred measurement conditions are in the wavelength ranges of 470 nm to 520 nm and 570 nm to 650 nm, after 20 minutes and at room temperature.
[0100] Example 4: Field swab testing
[0101] Following the CIP cleaning procedure, equipment from the tea processing facility was disassembled. The equipment was wiped down to test for the presence of organic and non-organic contaminants. The swabs were evaluated using the compositions, solutions, and methods described herein. Simultaneously, the ATP test was used to evaluate identical swab samples removed from the equipment. The results of each test are shown in Table 3.
[0102] Table 3: Comparison of described compositions and methods to ATP testing
[0103]
[0104] Comparative results show that the compositions, solutions, and methods described herein provide 1) observable color changes and 2) changes in absorbance, which can be measured to detect and identify the presence of organic matter and / or non-organic contaminants.
[0105] Additionally, in the ATP test, a swab is applied to a surface to sample for contamination, and after 20 minutes, the swab reads 0 RLU. A 0 RLU measurement indicates the absence of contamination on the surface, as no RLU is detected. However, swabs applied to the same surface under the same conditions using the compositions, solutions, and methods described herein produce readings measured by a HACH DR890 that differ from the blank control readings, indicating the presence of contamination on the surface. Therefore, the compositions, solutions, and methods described herein detect the presence of contamination not detected by the ATP test.
[0106] Additionally, the reactions produced by the compositions, solutions, and methods described herein can be used to calculate a threshold percentage, where the absorbance reading of the sample is divided by the absorbance reading of a blank control sample. This is helpful if low concentrations of contaminants are present, and thus produces minimal or no visible color change, as the threshold percentage provides an objective value for comparison with the sample. For example, end users in the field can set a threshold for the acceptable amount of contaminants in CIP equipment used in food and beverage processing facilities. The absorbance of a sample removed from the CIP equipment can be measured and compared to the threshold to determine the presence of contaminants, and if present, whether the amount of contaminants is below the threshold. The threshold can vary for different industries, where the varying contaminant levels can be acceptable or unacceptable.
[0107] Preferred aspects and embodiments of this disclosure have been described, and modifications and equivalents of the disclosed concepts will readily occur to those skilled in the art. However, it is intended that such modifications and equivalents be included within the scope of the appended claims.
Claims
1. A method for testing organic or non-organic contaminants on a surface, the method comprising: (a) Wipe the surface with a substrate; (b) Contacting the substrate with a solution, the solution comprising: (i) Alkali metal hydroxides, (ii) one or more oxidizing compounds, said one or more oxidizing compounds comprising sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, and (iii) one or more compounds, said one or more compounds being selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, and combinations thereof; and (c) Detect the colorimetric reaction on the substrate or in the solution.
2. The method according to claim 1, wherein the solution further comprises potassium tripolyphosphate or sodium tripolyphosphate.
3. The method according to claim 1 or 2, wherein the detection of a colorimetric reaction indicates the presence of organic matter or non-organic contaminants on the surface.
4. The method according to any one of claims 1 to 3, further comprising: Step (d) Clean the surface to remove the organic matter or non-organic contaminants.
5. The method of claim 4, wherein cleaning the surface comprises: Wipe, spray, soak, UV sterilize, or a combination thereof.
6. The method according to any one of claims 4 to 5, further comprising: Repeat steps (a) through (d) until no color reaction is detected.
7. The method according to any one of claims 1 to 6, wherein the solution comprises: (a) 0.1% to 45% by weight of alkali metal hydroxides, (b) 0.1% to 40% by weight of the one or more of the aforementioned oxidized compounds, and (c) 0.001% by weight to 5% by weight of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, or combinations thereof.
8. The method according to any one of claims 1 to 7, wherein the solution comprises about 0.01% by weight to about 6% by weight of sodium tripolyphosphate or potassium tripolyphosphate.
9. The method according to any one of claims 1 to 8, wherein the solution further comprises up to 100% by weight water.
10. The method according to any one of claims 1 to 9, wherein the colorimetric reaction is visually detected.
11. The method according to any one of claims 1 to 9, wherein the colorimetric reaction is measured by a color comparator or a colorimeter.
12. The method according to any one of claims 1 to 11, wherein the solution is diluted to about 1% to about 20% of the working solution before the solution contacts the substrate.
13. The method according to any one of claims 1 to 12, wherein the solution does not contact the surface and does not need to be rinsed off after the test.
14. The method according to any one of claims 1 to 13, wherein the surface is part of a Clean In-Site (CIP) system or a Clean Off-Site (COP) system.
15. The method of claim 14, wherein the CIP system is located in a food factory, beverage factory, or pharmaceutical factory.
16. The method according to any one of claims 1 to 15, wherein the surface is located in a hospital, kitchen, hotel, laboratory, or office.
17. The method according to any one of claims 1 to 16, wherein the pH of the solution is about 9.5 to about 13.
5.
18. The method according to any one of claims 1 to 17, wherein the colorimetric reaction produces a color change in the presence of organic matter or non-organic contaminants.
19. The method of claim 18, wherein the color change is a change of 0.1 or a larger unit of absorbance.
20. The method according to any one of claims 1 to 19, wherein the colorimetric reaction occurs in less than 30 minutes.
21. The method according to any one of claims 1 to 20, wherein the colorimetric reaction occurs in less than 20 minutes.
22. The method according to any one of claims 1 to 21, wherein the colorimetric reaction is observed at room temperature.
23. The method according to any one of claims 1 to 22, wherein the colorimetric reaction is observed at about 10°C to about 60°C.
24. The method according to any one of claims 1 to 23, wherein the color comparator measures the colorimetric response at a range of 400 nm to 700 nm.
25. A method for testing organic or non-organic contaminants in a liquid, the method comprising: (a) Obtaining a sample from the liquid source; (b) Mixing the sample and the solution, wherein the solution comprises: (i) Alkali metal hydroxides, (ii) one or more oxidizing compounds, said one or more oxidizing compounds comprising sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, and (iii) one or more compounds, said one or more compounds being selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, and combinations thereof; and (c) Detect the colorimetric reaction in the solution.
26. The method of claim 25, wherein the solution further comprises potassium tripolyphosphate or sodium tripolyphosphate.
27. The method according to any one of claims 25 to 26, wherein the detection of a colorimetric reaction indicates the presence of organic matter or non-organic pollutants in the water source.
28. The method according to any one of claims 25 to 27, further comprising: Step (d) cleans the liquid source to remove the organic or non-organic contaminants.
29. The method of claim 28, wherein cleaning the liquid source comprises: Oxidation, absorption, biochemical treatment, dilution, filtration, membrane filtration, treatment, UV sterilization, or a combination thereof.
30. The method according to any one of claims 28 to 29, further comprising: Repeat steps (a) through (d) until no color reaction is detected.
31. The method according to any one of claims 25 to 30, wherein the solution comprises: (a) 0.1% to 45% by weight of alkali metal hydroxides, (b) 0.1% to 40% by weight of the one or more of the aforementioned oxidized compounds, and (c) 0.001% by weight to 5% by weight of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, or combinations thereof.
32. The method according to any one of claims 25 to 31, wherein the solution comprises about 0.01% by weight to about 0.01% by weight of sodium tripolyphosphate or potassium tripolyphosphate.
33. The method according to any one of claims 25 to 32, wherein the solution further comprises up to 100% by weight water.
34. The method according to any one of claims 25 to 33, wherein the colorimetric reaction is visually detected.
35. The method according to any one of claims 25 to 33, wherein the colorimetric reaction is measured by a color comparator or a colorimeter.
36. The method according to any one of claims 25 to 35, wherein the solution is diluted to about 1% to about 20% of the working solution before the solution comes into contact with the sample.
37. The method according to any one of claims 25 to 36, wherein the pH of the solution is about 9.5 to about 13.
5.
38. The method according to any one of claims 25 to 37, wherein the solution is not added to the liquid source.
39. The method according to any one of claims 25 to 38, wherein the liquid is water used for saline, pharmaceuticals, laboratory reagents, medical procedures, food or beverage preparation, or for cleaning or rinsing.
40. The method according to any one of claims 25 to 39, wherein the colorimetric reaction occurs in less than 30 minutes.
41. The method according to any one of claims 25 to 40, wherein the colorimetric reaction occurs in less than 20 minutes.
42. The method according to any one of claims 25 to 41, wherein the colorimetric reaction is observed at room temperature.
43. The method according to any one of claims 25 to 42, wherein the colorimetric reaction is observed at about 10°C to about 60°C.
44. The method according to any one of claims 25 to 43, wherein the colorimetric reaction produces a color change in the presence of organic matter or non-organic contaminants.
45. The method of claim 44, wherein the color change is a change in absorbance units of 0.1 or greater.
46. The method of claim 36, wherein the color comparator or the colorimeter measures the colorimetric response at a range of 400 nm to 700 nm.
47. A kit for testing organic or non-organic pollutants, the kit comprising: Swabs, absorbent balls, swabs, or test strips; A solution for detecting the presence of organic matter or non-organic pollutants, the solution comprising: Alkali metal hydroxides One or more oxidizing compounds, said one or more oxidizing compounds including sodium hypochlorite, potassium hypochlorite, sodium persulfate, potassium persulfate, or monopersulfate, and One or more compounds, wherein the one or more compounds are selected from the group consisting of potassium permanganate, sodium permanganate, potassium dichromate and sodium dichromate; and A test container configured to contain the solution, wherein the swab, the absorbent ball, the swab, or the test strip is in contact with the solution.
48. The kit of claim 47, wherein the swab, the absorbent ball, the swab, or the test strip is in contact with the surface or source of the liquid containing the organic or non-organic contaminant to be tested before contacting the solution.
49. The kit according to any one of claims 47 to 48, wherein a colorimetric reaction will occur in the solution in the presence of organic matter or non-organic contaminants.
50. The kit according to any one of claims 47 to 49, wherein the solution further comprises up to 100% by weight water.
51. The kit according to any one of claims 47 to 50, wherein the solution comprises: (a) 0.1% to 45% by weight of alkali metal hydroxides, (b) 0.1% to 40% by weight of the one or more of the aforementioned oxidized compounds, and (c) 0.001% by weight to 5% by weight of potassium permanganate, sodium permanganate, potassium dichromate, sodium dichromate, or combinations thereof.
52. The kit according to any one of claims 47 to 51, wherein the colorimetric reaction of the solution is visually observed after the swab, the absorbent ball, the swab, or the test paper is immersed in or soaked in the solution.
53. The kit according to any one of claims 47 to 51, wherein the colorimetric reaction of the solution is measured in the instrument after the swab, the absorbent ball, the swab, or the test paper is immersed in or soaked in the solution.
54. The kit according to any one of claims 47 to 53, wherein the pH of the solution is from about 9.5 to about 13.
5.
55. The kit according to any one of claims 47 to 54, wherein the kit is used on the surface of a Clean In-Place (CIP) system or a Clean Off-Site (COP) system.
56. The kit according to claim 55, wherein the CIP system is located in a food factory, beverage factory, or pharmaceutical factory.
57. The kit according to any one of claims 47 to 55, wherein the kit is intended for use in hospitals, kitchens, hotels, laboratories, or offices.
58. The kit according to any one of claims 47 to 57, wherein the colorimetric reaction occurs in less than 30 minutes.
59. The kit according to any one of claims 47 to 58, wherein the colorimetric reaction occurs in less than 20 minutes.
60. The kit according to any one of claims 47 to 59, wherein the colorimetric reaction is observed at room temperature.
61. The kit according to any one of claims 47 to 60, wherein the colorimetric reaction is observed at about 10°C to about 60°C.
62. The kit according to any one of claims 47 to 61, wherein the kit is used for testing liquid sources.
63. The kit according to claim 62, wherein the liquid is water used for saline, pharmaceuticals, laboratory reagents, medical procedures, food or beverage preparation, or for cleaning or rinsing.
64. The kit according to any one of claims 47 to 63, wherein the colorimetric reaction produces a color change in the presence of organic matter or non-organic contaminants.
65. The kit according to claim 64, wherein the color change is a change of 0.1 or greater absorbance units.
66. The kit according to any one of claims 47 to 65, wherein the colorimetric reaction is visually detected.
67. The kit according to any one of claims 47 to 65, wherein the colorimetric reaction is measured by a color comparator or a colorimeter.
68. The kit according to any one of claims 47 to 67, wherein the solution is diluted to about 1% to about 20% of the working solution before the solution comes into contact with the swab, the absorbent ball, the swab, or the test strip.
69. The kit according to claim 67, wherein the instrument is a color comparator or colorimeter that measures the colorimetric reaction at 400 nm to 700 nm.