DESC:FIELD OF THE INVENTION:
The present invention relates to Cleaning-in-place process and cleaning composition thereof. More particularly, this invention is directed to cleaning process for removing food soils that are adhere to the internal metal surfaces or joints of food processing equipment’s and lines following preparation.
BACKGROUND AND PRIOR ART:
The ready-to-drink/serve beverages like tea or coffee category has experienced rapid growth over recent years, as it combines the benefits of tea as a healthier beverage with the portable convenience of a prepared beverage that is ready to consume. During the manufacturing of such beverages, a heat is applied to the leaves or beans to release volatile compounds. Also, many food and beverage products are concentrated or created as a result of evaporation. Industrially processed ready-to-drink beverages may include a variety of different additives, including flavors, sweeteners, Carbohydrates, Vegetable Oil, Mineral salts, Food additives, Proteins or milk products. When a coffee or tea beverage is processed in industry, milk solids is heated, it generally results in formation and deposition of organic and inorganic soil on internal wall of processing equipment’s including pipes and transfer lines, and such burnt soil become tenacious on metal surfaces. It is very important task to clean and remove the deposited soil before taking new line of production or even before changeover.
The primary source of soil is from the food product being handled. Majority of the drinks contains more of the simple flavonoids called Catechins, while the processing and oxidization that the leaves undergo to make tea converts these simple flavonoids to the more complex varieties, called Theaflavins and Thearubigins. It turns out that complex varieties, e.g. Theaflavins and Thearubigins, strongly adhere to metal surfaces, e.g. internal wall of processing equipment’s, and that soil or stain, can be extremely difficult to completely remove without costly, energy demanding and time-consuming cleaning processes. Microbiological biofilms also contribute to the soil buildup on surfaces.
As known in the art, Cleaning-in-place (CIP) is industrially accepted process to clean and disinfect interior surfaces of tanks and pipelines of liquid food/beverages manufacturing equipment by passing cleaning solution through the system without dismantling the equipment.
Often, CIP protocol involves five important steps, Pre-rinse, detergent cleaning (acid/ alkali), rinse, detergent cleaning (acid/alkali), and final rinse. Sanitization is done separately after CIP. Cleaning composition used in cleaning cycle is one of the important considerations in evaluating cleaning effectiveness of CIP. It has been found that conventional CIP process uses an alkaline detergent or caustic treatment along with oxidizing agents such as Hydrogen peroxide.
EP 1,725,645 discloses the use of peroxides, preferably hydrogen peroxide, for the cleaning of equipment for producing or processing dairy products. The lactoperoxidase and thiocyanate(s) is added to the cleaning solution containing the hydrogen peroxide. The supplementary addition is performed in order to increase even more the effectiveness of cleaning with respect to the soiled and/or contaminated equipment.
WO 2007/050291 A1 discloses the pre-treatment composition followed by conventional CIP process. It directed to a method that includes treating the soiled surfaces with a strong acidic solution, preferably acidic peroxide solution. This pre-treatment is additional process that needs to perform in addition to actual CIP process
It has been noted that, in most of the conventional practice, the cleaning solution is made up as an aqueous solution of a caustic alkali, along with some oxidizing agents, such as Hydrogen peroxide, sodium persulphate, sodium perborate, sodium percarbonate, potassium permanganate as effective compositions.

The known methods are associated with the problems, such as once the cleaning cycle is over the cleaning solution is discharged to the drains due to formation of precipitates. The caustic treatment will remove protein soils and salts fouled at the walls of the tanks but will not act as a disinfectant. Also acidic treatment is sometimes essential to neutralize the caustic environment and/or remove inorganic soil deposition. So the total cleaning cycle steps as well as time is extended.
Several efforts have been taken by the inventors of present invention to develop a CIP process/protocol with reducing total cleaning steps like pre-treatment, caustic treatment and last essential step, i.e. rinsing step. The present invention provides the CIP protocol with enhance food compliance and ease of use including very effective tea/coffee soil cleaning performance.
The discussion of documents, acts, materials, devices, articles and the like is included in this specification solely for the purpose of providing a context for the present invention. It is not suggested or represented that any or all of these matters formed part of the prior art base or were common general knowledge in the field relevant to the present invention as it existed before the priority date of each claim of this application.
SUMMARY OF THE INVENTION:
In present invention, Cleaning-in-place method and cleaning composition surprising found that very effective wherein CIP process/protocol with reducing total cleaning steps like pre-treatment, caustic treatment and last essential step, i.e. rinsing step have been discovered. Further is stated that present invention provides the CIP protocol with enhance food compliance and ease of use including very effective tea/coffee soil cleaning performance.
More particularly, this invention is directed to cleaning process for removing food soil that are adhere to the internal metal surfaces or joints of food processing equipment’s and lines following preparation.

Yet one of the aspects of the present invention is to provide a method for cleaning processing equipment’s and line used for manufacturing of ready-to-drink/serve beverages.
A further aspect of this invention is to provide the cleaning method that is effectively oxidizes the organic and inorganic food soil deposited on metal surfaces.
Yet another aspect of the present invention is to provide a composition for cleaning processing equipment’s that can be re-use/re-circulated for several times without loss of effective cleaning performance.
A still further aspect of this invention is to provide a process for cleaning using a cleaning composition which comprises of cleaning agents which is metal non-corrosive.
As a result of extensive investigations, the inventor have found that the burnt soil can be removed effectively from metal surfaces using cleaning composition comprising of Potassium permanganate, in addition to inorganic acid.
One embodiment of the invention includes CIP cleaning process that is effective to remove inorganic and organic burnt food soil deposited in beverage manufacturing equipment’s comprising passing the cleaning composition containing of oxidizing agent and inorganic acid at temperature between 60 to 80 degC, that oxidize the burnt food soil. Further de-staining and rinsing the system with water.
Another embodiment of the invention relates to a CIP cleaning process for cleaning of beverage manufacturing equipment’s. The objective of cleaning process is to achieve chemical and bacteriological cleanliness, which means that the said process provides first thorough cleaning step with chemical oxidizing solution followed by disinfection with a disinfecting solution. The said CIP process comprising steps:
a) Optionally rinsing with water to remove liquid and loose particles,
b) Passing cleaning solution containing of oxidizing agent and inorganic acid above ambient temperature,
c) Passing water to rinse the excess cleaning solution
d) Passing the de-staining and sanitizing solution at ambient temperature as a part of rinsing step.

The best known and almost commonly used CIP systems are suitable to use or run this CIP process. The cleaning solutions are generally distributed to the CIP circuits from a central CIP station consisting of several tanks for storing of the cleaning solutions. The solutions are heated by steam and their concentration is constantly monitored and adjusted. The beverage equipment’s disclosed in this invention are not limited to pasteurizers, milk storage tanks, fermentation tanks for yogurt production, ready-to-drink beverage such as tea, coffee, juice, bear, carbonated drink, soup, ketchup, sauce, fruit and vegetable puree etc.
These and other aspects and features of the invention may be better understood with reference to the following description and accompanying drawings.

STATEMENT OF INVENTION:

A cleaning-in-place process for cleaning of food beverage processing equipments, the process comprising: (a) Contacting the soiled surface with cleaning composition comprising of at least one oxidizing agent and at least one conditioning agent, wherein the temperature of cleaning composition solution is raised at above 20 degC, and (b) Introducing water for rinsing the equipments, (c) Introducing the de-staining solution comprising at least one reducing agent in the water for rinsing of step (b), wherein, upon contact with the de-staining composition, the reducing agent reacts with the traces of oxidizing agent of step (a) and also sanitize the substrate surface; Wherein, the said process is integrated and runs continuously from Cleaning-in-place system into the enclosed processing equipments.

The said temperature of step a) is above ambient temperature, more specifically about 50 degC to 95 degC.
The avbove said process is run for sufficient period of time from 30 minute to 300 minutes, preferably from 45 minutes to 100 minutes.
The cleaning-in-place method as claimed in claim 1, wherein the oxidizing agent concentration in cleaning composition is in the range from 0.01 to 5% by weight.
The oxidizing agent in cleaning composition for step a) is Potassium permanganate and having concentration in range from 0.01 to 5% by weight.

The conditioning agent in cleaning composition for step a) is selected from Nitric acid, Phosphoric acid, Methanesulfonic acid, Hydrochloric acid or mixture thereof and having concentration in range from 0.01 to 10% by weight.
The reducing agent in de-staining composition for step c) is selected from hydrogen peroxide, peracetic acid or mixture thereof and having concentration in range from 0.01 to 5 % by weight.

BRIEF DESCRIPTION OF DRAWING(S):

Having thus described the invention in general terms, reference will now be made to the accompanying drawings, which are not necessarily drawn to scale, and wherein:
FIGURE 1: Represent the weight loss on black tea soil panel upon use of different cleaning solution.
FIGURE 2: Represent the weight loss on milk tea soil panel upon use of different cleaning solution.

DESCRIPTION OF INVENTION:
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, in which some, but not all embodiments of the inventions are shown. Indeed, these inventions may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will satisfy applicable legal requirements. Like numbers refer to like elements throughout.
It should be noted that while the making and using of various embodiments of the present invention are discussed in detail below, it should be appreciated that the present invention provides many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific embodiments discussed herein are merely illustrative of specific ways to make and use the invention and do not delimit the scope of the invention.
To facilitate the understanding of this invention, a number of terms are defined below. Terms defined herein have meanings as commonly understood by a person of ordinary skill in the areas relevant to the present invention. Terms such as "a", "an" and "the" are not intended to refer to only a singular entity, but include the general class of which a specific example may be used for illustration. The terminology herein is used to describe specific embodiments of the invention, but their usage does not delimit the invention, except as outlined in the claims.
Embodiments described herein relates to Cleaning-in-place (CIP) process that is effective to remove inorganic and organic burnt food soil deposited during beverage manufacturing process.
As introduced in the background section, there have been not only a problem of insufficient removal performance of soil, when cleaning composition consist of alkali hydroxide used for the CIP process along with suitable oxidizing agent, it has mild oxidizing properties and not re-usable, but also a problem of caustic residue on the surface of the equipments, resulting in need of additional neutralization step and inorganic soil removal step.
The method described herein is effective to remove burnt food soil. The present invention discloses the CIP cleaning method comprising passing soil oxidizing composition through the close loop of processing equipment’s, and having a high removability for inorganic and organic burnt soil and particulates, in particular complex residue. The said cleaning composition does not cause corrosion of a metal material such as stainless steel, and can further re-cycle for several wash cycles.
That is, the present invention is a cleaning method of internal metal surfaces of processing equipments and lines including the process which contacts metal surface to soil oxidizing composition, and further the process which contacts the metal surface with reducing agent. Optionally, temperature of the cleaning solution is increased at above ambient temperature and intermittent rinsing steps with water.
The soil oxidizing composition comprises of oxidizing agent and conditioning agent. The oxidizing agent is preferably present in the said composition in an amount ranging from 0.01 to 5% by weight, more preferably from 0.01 to 1.0% by weight, and most preferably from 0.01 to 0.5% by weight of water. Preferably, the oxidizing agent is Potassium permanganate.
The conditioning agent is preferably inorganic acid. The inorganic acid is preferably present in the said composition in an amount ranging from 0.01 to 10% by weight, more preferably from 0.1 to 10% by weight, and most preferably from 0.1 to 5% by weight of water. Preferably inorganic acid is selected from nitric acid, phosphoric acid or mixture thereof. Most preferably, the inorganic acid is nitric acid.
In accordance to second embodiment, an effective amount of de-staining solution comprising of reducing agent and it serve as a stain remover as well as sanitizing of the equipments in CIP process. Accordingly, in some embodiments, the reducing agent comprises a hydrogen peroxide and peracetic acid or mixture thereof, wherein the reducing agent is present in an amount ranging from 0.01 to 5 % by weight, more preferably from 0.01 to 1% by weight of water.

The form in particular of the food soil which is the target for washing is not restricted. Therefore, although it can be aimed at a substrate-like thing, the method of the present invention exerts an effect most to washing of the metal surfaces to remove food soil of the following form. Specifically, it is preferable to be aimed at milk and dairy based beverages, Soy-based beverages, juice, juice drinks, Coffee, Tea, soups soft drinks, sports drinks, energy drinks and alcoholic beverages.
The period of time for which the cleaning solutions contact the metal surfaces of processing equipments will generally depend on the temperature of Cleaning solution and its concentration. Typically, the period of time will range from about 1 minute to about 120 minutes in most embodiments, with a period of time within a range of about 1 minute to about 60 minutes in other embodiments.
In a preferred embodiment the invention provides a method for Cleaning-in-place for processing ready-to-drink equipments comprising steps:
a) Optionally introducing the water for rinsing
b) Introducing soil oxidizing composition comprising oxidizing agent at above 20 degC,
c) Introducing the water for rinsing ,
e) Introducing the de-staining and sanitizing solution.
In a more preferred embodiment the invention provides a method for Cleaning-in-place for processing ready-to-drink equipments comprising steps:
(a) Contacting the soiled surface with cleaning composition comprising of at least one oxidizing agent with a conditioning agent, wherein the temperature of cleaning solution is raised at above ambient temperature; and
(b) Introducing water for rinsing the equipments,
(c) Contacting the soiled substrate surface with de-staining solution comprising at least one reducing agent for reacting with the traces of oxidizing agent of step (a) and to sanitize the substrate surface;
wherein the said process is integrated and runs continuously from CIP system into the enclosed processing equipments having temperature controller.

In accordance with the preferred embodiment, soil oxidizing composition solution having oxidizing agent content between 0.01-5% are subjected to treatment with food soil at above 20 degC, more preferably at 60-80 degC. The oxidizing agent is potassium permanganate.
Treatment with soil oxidizing composition oxidized the burnt soil and dissolve in it at higher temperature thus helps to remove the soil from metal surfaces. The dissolved soil is removed from the food contact surfaces.
In the present invention of cleaning-in-place method wherein the temperature above ambient temperature is raised in step by step or linearly increases.
It is stated that cleaning-in-place method wherein step (b) introducing water for rinsing the equipments is optional.
In yet another embodiment the soil oxidizing composition comprising oxidizing agent and inorganic acid retains its active content even after cleaning of the soil and hence can be recycle it for several times.
The present invention is further described with the help of the following examples, which are given by way of illustration and therefore should not be construed to limit the scope of the invention as claimed in any manner.
EXAMPLES:
Example 1: Laboratory studies were conducted to generate cleaning efficiency data for different CIP composition and protocol stages. The basic CIP protocol is of five stages; a) Rinsing with Water, b) First chemical effect, c) Rinsing with water, d) Second chemical effect and e) Rinsing with Water; in addition to last sanitization step.
Preparation of Test Model: The stained food panels were obtained by following methods.
A. Stainless steel panel was cleaned with Ethanol and dried at 105 degC for 1 Hr in a hot air oven. It was weighed up to 4 digits. It was then placed in an oven preheated to 220 Deg C. 2 ml of liquid food sample (e.g. Lipton Ice tea/tomato soup) was applied over approx. 20 sq.cm area. It was allowed to bake at 220 degC for 1 Hr. Panel was then cooled and weighed again up to 4 digits.
B. The piece of pipes was collected from actual tea and coffee beverage manufacturing site which included tea soil and milk tea soil and cut into several small plates/panels. It was weighed up to 4 digits.

Example 2: The cleaning-in-place of plates with Black Tea and milk Tea soils obtained as per method mentioned in example 1, B), was demonstrated. After pre-rinsing step the test panel was placed in beaker containing first chemical solution mentioned at required temperature. It should be noted that the temperature is mentioned herein is temperature of reagents passing through CIP for given time. Further rinsed with water and placed in second chemical solution. Lastly again rinsed with water and dried in oven at 100 Deg C for 1 hour. The weight of each cleaned panel was recorded to calculate weight loss. Details of cleaning composition are reported in below table no.1.
In this cleaning evaluation, the visual observation as well as weight loss after cleaning of each test panel was evaluated.
It can be seen from the table no. 2 and 3 that there is a significant synergistic effect o0n cleaning of combining oxidizing agent and the acid, whereas caustic alkali fails to remove the burnt soil completely. The results are also depicted in Figure no. 1 and 2.
Test No. First Chemical Composition Second Chemical Composition CIP Temperature in degC
1 2% w/w Sodium Hydroxide 1% w/w Nitric acid 80 DegC
2 2% w/w Sodium Hydroxide 1% w/w Formic acid 80 DegC
3 2% w/w Sodium Hydroxide 0.45% w/w Phosphoric acid 80 DegC
4 1% w/w Sodium Hydroxide 0.45 % w/w Phosphoric acid and 0.09% w/w DiPropyleneglycolMethylether 80 DegC
5 1% w/w Sodium Hydroxide and 0.35% EDTA 1% w/w Nitric acid 80 DegC
6 1% w/w Sodium Hydroxide and 0.35% EDTA 1% w/w phosphoric acid and 0.35% w/w oxalic acid 80 DegC
7 2% w/w Sodium Hydroxide and 0.15% w/w hydrogen peroxide 1% Nitric acid 80 DegC
8 2% w/w Sodium Hydroxide and 200 ppm Chlorine 1% Nitric acid 60 DegC
9 5% Nitric acid, Rinsing and 2% w/w Sodium Hydroxide 1% w/w nitric acid 80 DegC
10 1.9% Nitric acid, 0.35% phosphoric acid and 0.5% Potassium Permanganate 0.005% w/w Peracetic acid and 0.02% w/w hydrogen peroxide 80 DegC
Table 1

Soil Type Test number Solutions Weight Loss (g)
Black tea 1 NaOH, HNO3 0.0020
2 NaOH, Formic acid 0.0010
3 NaOH, Phosphoric acid 0.0012
4 NaOH, Phosphoric acid+DPM 0.0018
5 NaOH+ETDA, Nitric acid 0.0012
6 NaOH+ETDA, Phosphoric acid+Ascorbic acid 0.0018
7 NaOH+H2O2 0.0017
8 NaOH+Chlorine 0.0013
9 Nitric acid, NaOH, Nitric acid 0.0009
10 1.9% Nitric acid, 0.35% phosphoric acid and 0.5% Potassium Permanganate 0.0056
Table 2
Soil Type Test number Solutions Weight Loss (g)
Milk Tea 1 NaOH, HNO3 0.0014
2 NaOH, Formic acid 0.0010
3 NaOH, Phosphoric acid 0.0012
4 NaOH, Phosphoric acid+DPM 0.0011
5 NaOH+ETDA, Nitric acid 0.0015
6 NaOH+ETDA,Phosphoricacid+Ascorbic acid 0.0006
7 NaOH+H2O2 0.0014
8 NaOH+Chlorine 0.0012
9 Nitric acid, NaOH, Nitric acid 0.0008

10 1.9% Nitric acid, 0.35% phosphoric acid and 0.5% Potassium Permanganate 0.0044
Table 3
It was visually observed that Test number 10 gives best cleaning with >99% removal of all types of soil from the panels.

Example 3: Further, two specific protocols were performed to check the cleaning efficiency of Potassium Permanganate as given below.
Protocol 1: Placed the soiled panel in solution containing 5% sodium hydroxide and 0.5% Potassium Permanganate at solution temperature 80 DegC for 30 min. Rinsed withwater at room temperature. Then panel was taken out and placed it in solution containing0.77% Nitric acid, 0.14% Phosphoric acid and 1% Ferrous sulphate, at temperature 80 DegC,Time 10 Min. Dried the panel in oven at 1000C for 1 hour.
Protocol 2: Placed the soiled panel in solution containing 1.9% Nitric acid and 0.35% phosphoric acid and 0.5% Potassium Permanganate at temperature 50 to 80 DegC for 30 min. Rinsed with water having 0.005% w/w Peracetic acid and 0.02% w/w hydrogen peroxide at room temperature. Dried the panel in oven at 100 DegC for 1 hour.
Visual Observation:
Protocol 1 based on Alkaline Potassium Permanganate does not clean Black tea soil panels, but Protocol 2 based on Acidic Potassium Permanganate cleans both Milk tea and Black tea soil panels.

Example 4: A CIP protocols were run wherein effect of first cleaning composition comprising Potassium Permanganate and inorganic acid is studied including de-staining program for Mn02 stain. The experiments were carried out as described below;
Protocol 3- Dipped the panel in 0.38% Nitric acid and 0.07% Phosphoric acid + 0.05% Potassium Permanganate solution at temperature 80 DegC for 30 minute. Rinsed with water at room temperature. Dipped it in 0.38% Nitric acid and 0.07% Phosphoric acid + 1% Ferrous sulphate de-staining solution having temperature 80 degC for 10 minutes.
Protocol 4- Dipped the panel in 3.8% Nitric acid and 0.7% Phosphoric acid + 1.5% Potassium Permanganate solution at temperature 80 degC for 10 minute. Rinsed with water at room temperature. Dipped it in 0.38% Nitric acid and 0.07% Phosphoric acid + 1% Ferrous sulphate de-staining solution having temperature 80 degC for 10 minutes.
Observation:
Soil Type Protocol Weight Loss (g)
Black Tea 3 0.0033
Milk Tea 3 0.0009
Black Tea 4 0.0178
Milk Tea 4 0.0121
Table 4
Example 5: Process of De-staining of potassium permanganate stain: The cleaning-in-place of plates with Black Tea and milk Tea soils obtained as per method mentioned in example 1, B), was demonstrated. The said Tea and coffee soiled panels were subjected to cleaning and de-staining using following process.
The soiled panel was placed in cleaning solution comprising Potassium Permanganate and conditioning agent for 5 to 30 min. Temperature of solution was maintained at 60 to 80 degC. Rinsed with water and place it in solution containing de-staining solution maintained at room temperature for 5 to 10 Min. The panel was dried in oven at 100 degC for 1 hour. Details of cleaning protocol and composition are reported in below table no.5.
Table No 6 shows that all the cleaning composition in accordance with the present invention demonstrated excellent cleaning and de-staining ability and also excellent solution stability including reusability.
The sanitizing ability of Peracetic acid is known for its sanitizing activity. Peracetic acid is an effective sanitizer that is active against many microorganisms and their spores. Mortality is produced by the disruption of chemical bonds within the cell membrane. In present invention, the Peracetic acid sanitizer is paired with hydrogen peroxide in de-staining step, thus producing acceptable microbial mortality on processing equipment.
Type of soil Test No. % of KMnO4 Conditioning acid Used Temperature and
Time for cleaning step Composition of
De-staining solution Temperature and
Time for De-staining step
Milk Tea 1 0.05 0.77% Nitric acid and 0.14% Phosphoric acid 80 DegC, 30 min 0.1% FeSO4 + 0.19% Nitric acid and 0.035% phosphoric acid, Room Temperature, 10min
2 0.05 0.9% Phosphoric acid 80 DegC, 30 min 0.1% FeSO4 + 0.19% Nitric acid and 0.035% phosphoric acid, Room Temperature, 10min
Black Tea 3 0.01 1% Nitric acid 80 DegC, 30 min 0.1%
FeSO4 + 0.25% Nitric acid, Room Temperature,
10 min
4 0.05 1% Nitric acid 60 DegC, 30 min 0.1%
FeSO4 + 0.25% Nitric acid, Room Temperature,
10 min
5 0.05 1% Nitric acid 60 DegC, 30 min 0.005%
% Peracetic acid + 0.023% Hydrogen peroxide, Room Temperature,
5 min
6 0.01 1% Nitric acid 60 DegC, 30 min 0.005%Peracetic acid + 0.023% Hydrogen peroxide, Room Temperature,
5 min
Table 5

Type of soil Test No. Visual observation Initial
Wt in gm
Final
Wt in gm Wt Loss in gm
% Wt
Loss
Milk Tea 1 Panel Clean, Cleaning solution remains purple.
Solution is Clear and Reusable. 24.1725 24.1706 0.0019 0.00786

2 Panel Clean, Brown precipitates seen in Cleaning
solution. Solution is not reusable. 22.9048 22.9005 0.0043 0.01877
Black Tea 3 Panel Clean, Cleaning solution remains purple.
Solution is Clear and Reusable. 25.4263 25.4232 0.0031 0.01219

4 Panel Clean, Cleaning solution remains purple.
Solution is Clear and Reusable. 18.9545 18.9481 0.0064 0.03377

5 Panel Clean, Cleaning solution remains purple.
Solution is Clear and Reusable. 20.4678 20.4606 0.0072 0.03518
6 Panel Clean, Cleaning solution remains purple.
Solution is Clear and Reusable. 25.2596 25.2519 0.0077 0.03048
Table 6
Example 6: Evaluating cleaning efficiency of CIP protocols on heat burnt Tomato soil: The cleaning-in-place of plates with Tomato soup soils obtained as per method mentioned in example 1, A), was demonstrated. The said tomato soiled panels were subjected to cleaning and de-staining using following process.
I. Methodology: Soiled panels were dipped in a beaker with cleaning solution with desired concentration of chemicals and temperature. Agitation of solution was done. After predefined time of cleaning panels were taken out and the percentage loss in soil weight was checked. Details of cleaning protocol, cleaning and de-staining composition used for this methodology are summarized in below table no.7.
The results are given in table no. 8.
Protocol No. Cleaning solution Composition Temperature and
Time for cleaning step Composition of
De-staining solution Temperature and
Time for De-staining step
5 1% nitric acid+ 0.03 % KMnO4 60 DegC for 45 min followed by 0.05% Peracetic acid &0.115% Hydrogen peroxide Room Temperature, 30 min
6 0.68% NaOH 80 DegC for 30 min 0.15% Hydrogen Peroxide Room Temperature, 10min
7 2% NaOH 80 DegC 30 min 1% nitric acid 60 DegC for 30 min
Table 7
Protocol No. Weight of empty Coupons in gm Weight of Coupons after soiling in gm Weight of coupon after cleaning in gm % Soil cleaning Avg. % soil removal
5 173.9589 178.3419 173.9622 99.92 99.83
173.6407 178.196 173.6527 99.74
6 174.634 178.5217 174.635 99.97 99.61
175.2419 178.7139 175.268 99.25
7 176.3801 180.0184 176.3986 99.49 99.52
176.2421 180.1079 176.2595 99.55
Table 8
II. Methodology: Soiled panels were hung on a plate that moves vertically. Panels thus get dipped in to the cleaning solutions with desired concentration of chemicals and temperature. After predefined number of dips, panels were taken out and weighed for percentage loss in soil weight. Details of cleaning protocol, cleaning and de-staining composition used for this methodology are summarized in below table no.9.The results are given in table no. 10.

Protocol No. Cleaning solution Composition Temperature and
Dips for cleaning step Composition of
De-staining solution Temperature and
Time for De-staining step
8 1% nitric acid+ 0.03 % KMnO4 at 60 DegC (80 dips) 0.05% Peracetic acid &0.115% Hydrogen peroxide Room Temperature,
(30 dips)
9 1% nitric acid with 0.03 % KMnO4 at 70 DegC (80 dips) 0.05% Peracetic acid &0.115% Hydrogen peroxide Room Temperature,
(30 dips)
10 1% nitric acid with 0.03 % KMnO4 at 80 DegC (80 dips) 0.05% Peracetic acid &0.115% Hydrogen peroxide Room Temperature,
(30 dips)
11 Tap Water at 80 DegC
(50 dips)
- -
12 2% NaOH at 80 DegC (50 dips) - -
13 0.68% NaOH + 0.15% Hydrogen Peroxide at 80 DegC for 30 min - -
14 2% NaOH at 80 DegC (50 dips) followed by 1% nitric acid at 60 DegC (30 dips)
Table 9

Protocol No. Weight of empty Coupons in gm Weight of Coupons after soiling in gm Weight of coupon after cleaning in gm % Soil cleaning Avg. % soil removal
8 173.6125 182.7408 173.623 99.88 99.89
172.8301 185.036 172.839 99.93
9 173.6384 184.5066 173.6493 99.90 99.91
172.8301 185.036 172.839 99.93
10 176.3421 188.397 176.349 99.94 99.96
174.6559 187.2118 174.659 99.98
11 173.9588 185.4026 174.1173 98.61 93.09
175.2669 187.527 176.7904 87.57
12 176.4042 187.836 176.4175 99.88 99.70
176.2668 189.391 176.3306 99.51
13 176.3157 186.0012 176.3214 99.94 99.96
176.3774 185.8525 176.38 99.97
14 173.9308 185.2864 173.9318 99.99 99.96
176.2287 185.2566 176.2354 99.93
Table 10
Example 7: Evaluating cleaning efficiency of CIP protocols on heat burnt tea soil:
I. Effect of Temperature:
The cleaning-in-place of plates with black Tea soup soils obtained as per method mentioned in example 1, A), was demonstrated.
Details of cleaning protocol, cleaning and de-staining composition used for respective methodology including Average % soil removal are summarized in below table no.11, 12 and 13.

Protocol No. Cleaning solution Composition Temperature and
Time for cleaning step Composition of
De-staining solution Temperature and
Time for De-staining step Avg. % soil removal
15 0.12% KMnO4 + 2% Nitric acid At 45 DegC For 30 min Followed by 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room temperature, 15 min 46.38
16 0.03% KMnO4 + 1% Nitric acid At 50 DegC, 30 min, Followed by 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room temperature, 15 min 80.13
17 0.03% KMnO4 + 1% Nitric acid At 60 DegC, 30 min, Followed by 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room Temperature, 15 min 99.12
18 0.01% KMnO4 + 1% Nitric acid At 80 DegC, 30 min, Followed by 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room Temperature, 15 min 100.00
19 0.03% KMnO4 + 1% Nitric acid At 95 DegC, 30 min, Followed by 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room Temperature, 15 min 100.00
20 DM water At 60 DegC, 30 min - - 35.08
21 DM water at 95 degC - - 78.88
Table 11

II. Effect of conditioning agents and mixture thereof:
Protocol No. Cleaning solution Composition Temperature and
Time for cleaning step Composition of
De-staining solution Temperature and
Time for
De-staining step Avg. % soil removal
22 0.03% KMnO4 + 1% Nitric acid At 60 DegC For 30 min 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room temperature, 15 min 99.12
23 0.03% KMnO4 + 1% Methane Sulfonic acid @60 DegC, 30 min, At 60 DegC, 30 min, 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room Temperature, 15 min 99.78
24 0.03%KMnO4 + 1% HCl At 60 DegC, 30 min, 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room temperature, 15 min 99.55
25 0.03% KMnO4 + 0.8% Nitric acid + 0.2% Phosphoric acid At 95 DegC, 30 min, 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room Temperature, 15 min 99.95
26 0.03% KMnO4 + 0.8% Nitric acid + 0.2% Phosphoric acid At 60 DegC, 30 min, 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room Temperature, 15 min 99.90
27 0.03% KMnO4 + 0.8% Nitric acid + 0.2% Methane Sulfonic acid At 60 DegC, 30 min 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room Temperature, 15 min 99.57
Table 12

III. Effect of Reducing agent
Protocol No. Cleaning solution Composition Temperature and
Time for cleaning step Composition of
De-staining solution Temperature and
Time for De-staining step Avg. % soil removal
28 0.03% KMnO4 + 1% Nitric acid At 60 DegC, For 30 min 0.05% Peracetic acid + 0.115% Hydrogen peroxide At Room temperature, 15 min 99.70
29 0.03% KMnO4 + 1% Nitric acid At 60 DegC, 30 min, 0.15% Hydrogen peroxide At Room temperature, 15 min 99.56
Table 13
Example 8: Evaluating of sanitization step: A de-staining Step and its composition according to another embodiment of the present invention includes reducing agent in water that resulting into discoloration of Potassium permanganate. The said reducing agent is selected from hydrogen peroxide, peracetic acid or mixture thereof. The sanitizing ability of Peracetic acid and hydrogen peroxide is known. Peracetic acid is an effective sanitizer that is active against many microorganisms and their spores. Examples of microorganisms that may be targeted by the composition of present invention include, but are not limited to, one or more strains of Escherichia coli and various species of bacteria within the genera Salmonella {e.g., Salmonella enlerica, etc.), Staphylococcus {e.g.. Staphylococcus aureus. Staphylococcus epidermidis, etc.), Pseudomonas {e.g., Pseudomonas aeruginosa, etc.), Shigella, Campylobacter, Bacillus (e.g., Bacillus anthracis. Bacillus cereus, etc.), Hemophilus, Borcletella, Francisella, Brucella (e.g.. Brucella abortus. Brucella suis, Brucella melitensis, etc.). Listeria, Yersinia, Streptococci, and Vancomycin-Resistant Enterococci (e.g., E.faecium, E.faecalis, E. gallinarium, etc.), one or more strains of fungi C. albicans and Aspergillus niger.
The typical experiments were conducted to check the bactericidal and fungicidal activity of final cleaning step as per one of the important embodiment of present invention as follows;
Methodology: Dilution Nutralisation
The different concentration of Solution comprising 5% of Peracetic acid and 21% of Hydrogen peroxide was prepared. Namely 0.5%, 1.0% and 2.0% v/v.
Strains Used: E. Coli, E. hirae, Ps Aeruginosa, A. Niger, C. Albicans.
In accordance with EN13697:2001E, the all above diluted solution possesses bactericidal activity on surface in 5min and fungicidal activity on surface in 15min for all of the referenced strain listed above.

Dated this 21st day of October 2016.
Poonam Dhake Kolhe
Of In10gible Innovations LLP
Applicant’s Agent
,CLAIMS:CLAIMS

We Claim;

1. A cleaning-in-place process for cleaning of food beverage processing equipments, the process comprising:
(a) Contacting the soiled surface with cleaning composition comprising of at least one oxidizing agent and at least one conditioning agent, wherein the temperature of cleaning composition solution is raised at above 20 degC, and
(b) Introducing water for rinsing the equipments,
(c) Introducing the de-staining solution comprising at least one reducing agent in the water for rinsing of step (b), wherein, upon contact with the de-staining composition, the reducing agent reacts with the traces of oxidizing agent of step (a) and also sanitize the substrate surface;
Wherein, the said process is integrated and runs continuously from Cleaning-in-place system into the enclosed processing equipments.

2. The cleaning-in-place method as claimed in claim 1, wherein the oxidizing agent concentration in cleaning composition is in the range from 0.01 to 5% by weight.
3. The cleaning-in-place method as claimed in claim 1, wherein the oxidizing agent is Potassium permanganate.
4. The cleaning-in-place method as claimed in claim 1, wherein the conditioning agent concentration in cleaning composition is in the range from 0.01 to 10% by weight.
5. The cleaning-in-place method as claimed in claim 1, wherein the conditioning agent is selected Nitric acid, Phosphoric acid, Methanesulfonic acid, Hydrochloric acid or mixture thereof.
6. The cleaning-in-place method as claimed in claim 1, wherein the reducing agent concentration in de-staining composition is in the range from 0.01 to 5 % by weight.
7. The cleaning-in-place method as claimed in claim 1, wherein the reducing agent is selected hydrogen peroxide, peracetic acid or mixture thereof.
8. The cleaning-in-place method as claimed in claim 1, wherein the temperature is above ambient temperature, more specifically about 50 degC to 95 degC.
9. The cleaning-in-place method as claimed in claim 1, wherein the said process is run for sufficient period of time from 30 minute to 300 minutes, preferably from 45 minutes to 100 minutes.

Dated this 21st day of October 2016.
Poonam Dhake Kolhe
Of In10gible Innovations LLP
Applicant’s Agent