GB2635117A

GB2635117A - Cocoa composition

Info

Publication number: GB2635117A
Application number: GB2316214.2A
Authority: GB
Inventors: Chilver Ian; Rowan Lee; Williams Timothy; Pirani Edoardo; Dos Santos Jean; Ciocan Adriana; Gaca Pawel
Original assignee: Intercontinental Great Brands LLC
Current assignee: Intercontinental Great Brands LLC
Priority date: 2023-10-23
Filing date: 2023-10-23
Publication date: 2025-05-07
Also published as: WO2025090491A1; GB202316214D0

Abstract

An alkalised cocoa powder having a pH of from 6.10 to 6.65, preferably 6.25 to 6.45. Preferably, the cocoa powder has a D90 value of less than 50.0μm and a colour L-value (measured by the White diluent method) of 17.0-26.0. Preferably, the alkalised cocoa powder is less than 15wt.% ash, less than 150mg/100g sodium and at least 3500mg/100g potassium. A method for preparing the alkalised cocoa powder is disclosed comprising adding cocoa powder and an alkali solution to a reaction vessel; adding a gas (preferably steam) to the reaction vessel until a first pressure (P1) is reached; releasing some of the gas after a time T1 to reduce the pressure to a second pressure (P2). More gas (preferably air) is added to the reaction vessel to reach a third pressure (P3). P1>3.0 bara (preferably 5-7 bara), P3>2.5 bara (preferably no greater than 6.0 bara), and P2< P1 and P3 (preferably P2 is no greater than 1.5 bara). Preferably, T1 is 14-46 minutes and T3 is 28-65 minutes. Preferably, the alkali is potassium carbonate. A food or beverage, preferably chocolate milk, comprising the cocoa powder is also claimed.

Description

Cocoa Composition

Technical Field of the Invention

The present invention relates to a cocoa composition, in particular an alkalised cocoa composition, more specifically, an alkalised cocoa powder, and a method for preparing an alkalised cocoa powder.

Background to the Invention

Processing of cocoa beans typically includes fermenting harvested beans, drying the beans, de-hulling the beans to produce nibs, sterilising and roasting the nibs, crushing the nibs into cocoa liquor, and optionally pressing the cocoa liquor to obtain I 0 cocoa butter and cocoa powder.

Properties of the resultant cocoa product, such as colour, flavour and solubility, can be modified by adding an alkali to the cocoa material in an alkalisation step during processing of the cocoa bean, nib or powder, resulting in an alkalised or 'clutched' cocoa material.

The use of alkalised cocoa materials has previously overcome problems associated with some cocoa products. For example, natural cocoa products arc light brown in colour but it is often desirable to produce a darker coloured, or more 'red-brown' coloured cocoa material. Cocoa material with significant colouring capacity has traditionally been obtained by using artificial colours. However_ many countries prohibit the use of artificial colours in foodstuffs, including cocoa products. Darker and more 'red-brown' colours in cocoa products can be generated by incorporating an alkalisation step in the processing of the cocoa bean and using specific alkalisation reaction conditions, such as temperature, pressure, pH, time and moisture content of the cocoa material.

Alkalised cocoa products may be used in applications such as bakery products, desserts, ice cream, cocoa beverages, toppings for ice cream, biscuits or confectionery and compound coatings. The alkalised cocoa can also be used in applications where the product requires further preparation to obtain a consumable product, for example, cake mixes, ice cream mixes, dessert powders and instant cocoa mixes.

Consumer demands require cocoa manufacturers to produce cocoa products in a broad range of flavours and colours, and to provide new and interesting sensory experiences for the consumer. These properties of a cocoa material can be directly affected by alkalisation of the cocoa material during processing of the cocoa bean, demonstrating the importance of the alkalisation of cocoa. Thus, there is a need in the market for cocoa products having new and interesting properties which are desirable to a consumer.

It is an object of embodiments of the present invention to at least partially overcome or alleviate at least one of the above problems and/or to provide an alkalised cocoa product with desirable properties, such as colour and flavour, and which improves on existing sensory experiences for the consumer.

Summary of the Invention

According to a first aspect of the invention, there is provided an alkalised cocoa powder having a pH of from about 6.10 to about 6.65.

A pH of about 6.10 to about 6.65 is relatively low compared to the pH of known alkalised cocoa powders. It is known from the prior art that some alkalised cocoa powders have a pH of greater than about pH 6.70, for example pH 7.00 or greater.

Advantageously, an alkalised cocoa powder having a pH of from about 6.10 to about 6.65 does not exhibit an undesirable powdery taste and mouthfecl as is common with alkalised cocoa powders having a pH of above about 6.65, for example pH 6.70 or above. Further, the alkalised cocoa powder of the invention does not possess an unpleasant alkali odour or taste, often recognisable with comparably higher pH alkalised cocoa powders, due to it having a pH of from about 6.10 to about 6.65.

Further, while the pH of the alkalised cocoa powder of the present invention is relatively low, the cocoa material is sufficiently alkalised to obtain the beneficial properties of alkalised cocoa powder. As such, the cocoa powder of the invention benefits from exhibiting darker and more 'red-brown' colours in cocoa products which it is used to produce.

The alkalised cocoa powder may have a pH of from about 6.15 to about 6.55, from about 6.20 to about 6.50, from about 6.25 to about 6.45, from about 6.30 to about 6.40, or about 6.35.

The alkalised cocoa powder may have a pH of from about 6.10 to about 6.60, from about 6.10 to about 6.55, from about 6.10 to about 6.50, from about 6.10 to about 6.45, from about 6.10 to about 6.40, from about 6.10 to about 6.35, from about 6.10 to about 6.30, from about 6.10 to about 6.25, from about 6.10 to about 6.20, or from about 6.10 to about 6.15.

The alkalised cocoa powder may have a pH of from about 6.15 to about 6.65, from about 6.15 to about 6.60, from about 6.15 to about 6.55, from about 6.15 to about 6.50, from about 6.15 to about 6.45, from about 6.15 to about 6.40, from about 6.15 to about 6.35, from about 6.15 to about 6.30, from about 6.15 to about 6.25, or from about 6.15 to about 6.20.

The alkalised cocoa powder may have a pH of from about 6.20 to about 6.65, from about 6.20 to about 6.60, from about 6.20 to about 6.55, from about 6.20 to about 6.50, from about 6.20 to about 6.45, from about 6.20 to about 6.40, from about 6.20 to about 6.35, from about 6.20 to about 6.30, or from about 6.20 to about 6.25.

The alkalised cocoa powder may have a pH of from about 6.25 to about 6.65, from about 6.25 to about 6.60, from about 6.25 to about 6.55, from about 6.25 to about 6.50, from about 6.25 to about 6.45, from about 6.25 to about 6.40, from about 6.25 to about 6.35, or from about 6.25 to about 6.30.

The alkalised cocoa powder may have a pH of from about 6.30 to about 6.65, from about 6.30 to about 6.60, from about 6.30 to about 6.55, from about 6.30 to about 6.50, from about 6.30 to about 6.45, from about 6.30 to about 6.40, or from about 6.30 to about 6.35.

The alkalised cocoa powder may have a pH of from about 6.35 to about 6.65, from about 6.35 to about 6.60, from about 6.35 to about 6.55, from about 6.35 to about 6.50, from about 6.35 to about 6.45, or from about 6.35 to about 6.40.

The alkalised cocoa powder may have a pH of from about 6.40 to about 6.65, from about 6.40 to about 6.60, from about 6.40 to about 6.55, from about 6.40 to about 6.50, or from about 6.40 to about 6.45.

The alkalised cocoa powder may have a pH of from about 6.45 to about 6.65, from about 6.45 to about 6.60, from about 6.45 to about 6.55, or from about 6.45 to about 6.50.

The alkalised cocoa powder may have a pH of from about 6.50 to about 6.65, from about 6.50 to about 6.60, or from about 6.50 to about 6.55.

The alkalised cocoa powder may have a pH of from about 6.55 to about 6.65, or from about 6.55 to about 6.60.

The alkalised cocoa powder may have a pH of from about 6.60 to about 6.65.

The alkalised cocoa powder may have a pH of about 6.10, about 6.15, about 6.20, about 6.25, about 6.30, about 6.35, about 6.40, about 6.45, about 6.50, about 6.55, about 6.60, or about 6.65.

Method of measuring pH of the alkalised cocoa powder The pH of the alkalised cocoa powder is measured at 25°C and ambient pressure, according to ICA method 15/1972 (formerly 9/1972). The method comprises adding a sample of the alkalised cocoa powder equal to 10 wt.% to water, and dispersing the alkalised cocoa powder therein. A pH meter is inserted into the solution of alkalised cocoa powder and its pH is measured.

The alkalised cocoa powder may have a D90 value of less than about 50 pm. Thus, 90% of a sample of the alkalised cocoa powder may have a particle size which is smaller than 50 pm.

Advantageously, an alkalised cocoa powder having a D90 value of less than about 50 pm results in a cocoa powder which comprises liner particles than a cocoa powder having a D90 value of greater than 50 pm. Advantageously, the particles of the alkalised cocoa powder of the invention are not as coarse and arc therefore more easily solubilised by a fluid, for example water, for example when the powder is being used to form a cocoa beverage or cocoa butter. As such, the resultant product (e.g., cocoa beverage or cocoa butter) does not provide undesirable 'sandy' texture and taste properties to the consumer.

The alkalised cocoa powder may have a D90 value of less than about. 45 pm, about 40 pm, about 35 pm, about 30 pm, about 25 pm, about 20 pm, about 15 pm, about 10 pm, or less than about 5 Rm.

The alkalised cocoa powder may have a D90 value of from about 5 pm to about 50 pm, from about 10 pm to about 50 pm, from about 15 pm to about 50 pm, from about 20 gm to about 50 pm, from about 25 pm to about 45 pm, from about 30 pm to about 40 pm, from about 33 pm to about 37 Rm, from about 34 pm to about 36 pm, or about 35 pm.

The alkalised cocoa powder may have a D90 value of from 5 pm to about 50 pm, from about 5 pm to about 45 pm, from about 5 pm to about 40 pm, from about 5 pm to about 35 pm, from about 5 pm to about 30 pm, from about 5 pm to about 25 gm. from about 5 pm to about 20 pm, from about 5 pm to about 15 pm, or from about 5 pm to about 10 pm.

The alkalised cocoa powder may have a D90 value of from 10 pm to about 50 pm, from about 10 pm to about 45 pm, from about 10 pm to about 40 pm, from about 10 pm to about 35 pm, from about 10 pm to about 30 pm, from about 10 pm to about 25 pm, from about 10 pm to about 20 pm, or from about 10 pm to about 15 Rm.

The alkalised cocoa powder may have a D90 value of from 15 pm to about 50 pm, from about 15 pm to about 45 pm, from about 15 pm to about 40 pm, from about 15 pm to about 35 pm, from about 15 gm to about 30 pm, from about 15 pm to about 25 pm, or from about 15 pm to about 20 pm.

The alkalised cocoa powder may have a D90 value of from 20 pm to about 50 25 pm, from about 20 pm to about 45 pm, from about 20 pm to about 40 p.m, from about 20 pm to about 35 pm, from about 20 pm to about 30 pm, or from about 20 pm to about 25 pm.

The alkalised cocoa powder may have a D90 value of from 25 pm to about 50 pm, from about 25 pm to about 45 pm, from about 25 pm to about 40 pm, from about 30 25 pm to about 35 pm, or from about 25 pm to about 30 pm.

The alkalised cocoa powder may have a D90 value of from 30 pm to about 50 pm, from about 30 pm to about 45 pm, from about 30 pm to about 40 pm, or from about 30 pm to about 35 Rm.

The alkalised cocoa powder may have a D90 value of from 35 pm to about 50 5 pm, from about 35 pm to about 45 tan, or from about 35 pm to about 40 pm.

The alkalised cocoa powder may have a D90 value of from 40 pm to about 50 pm, or from about 40 pm to about 45 pm.

The alkalised cocoa powder may have a D90 value of from 45 pm to about 50 pm.

The alkalised cocoa powder may have a D50 value of less than about 15 Rm.

Thus, 50% of a sample of the alkalised cocoa powder may have a particle size which is smaller than 15 pm.

The alkalised cocoa powder may have a D50 value of less than about 20 p.m, about 18 pm, about 16 tan, about 15 pm, about 14 pm, about 12 pm, about 10 pm, about 15 8 pm, about 6 pm, about 5 pm, about 4 pm, or less than about 2 pm.

The alkalised cocoa powder may have a D50 value of from about 2 pm to about 20 pm, from about 5 pm to about 20 pm, from about 8 pm to about 20 pm, from about 10 p.m to about 20 pm, from about 12 pm to about 20 pm, from about 15 pm to about 20 pm, or from about 18 pm to about 20 Rm.

The alkalised cocoa powder may have a D50 value of from 2 pm to about 20 pm, from about 2 pm to about 18 pm, from about 2 pm to about 16 tan, from about 2 pm to about 14 pm, from about 2 pm to about 12 pm, from about 2 pm to about 10 pm, from about 2 pm to about 8 pm, from about 2 pm to about 6 pm, or from about 2 pm to about 4 pm.

The alkalised cocoa powder may have a D50 value of from 4 pm to about 20 pm, from about 4 pm to about 18 pm, from about 4 pm to about 16 tan, from about 4 pm to about 14 pm, from about 4 pm to about 12 pm, from about 4 pm to about 10 gm, from about 4 pm to about 8 pm, or from about 4 pm to about 6 Rm.

The alkalised cocoa powder may have a D50 value of from 6 gm to about 20 pm, from about 6 pm to about 18 pm, from about 6 gm to about 16 gm, from about 6 pm to about 14 pm, from about 6 pm to about 12 pm, from about 6 gm to about 10 gm, or from about 6 gm to about 8 pm.

The alkalised cocoa powder may have a D50 value of from 8 gm to about 20 pm, from about 8 pm to about 18 pm, from about 8 gm to about 16 gm, from about 8 pm to about 14 gm, from about 8 pm to about 12 gm, or from about 8 pm to about 10 The alkalised cocoa powder may have a D50 value of from 10 gm to about 20 10 pna, from about 10 pna to about 18 gm, from about 10 gm to about 16 gm, from about 10 pm to about 14 gm, or from about 10 gm to about 12 pm.

The alkalised cocoa powder may have a D50 value of from 12 gm to about 20 pm, from about 12 gm to about 18 gm, from about 12 gm to about 16 gm, or from about 12 pm to about 14 gm.

The alkalised cocoa powder may have a D50 value of from 14 gm to about 20 pm, from about 14 pm to about 18 pm, or from about 14 gm to about 16 gm.

The alkalised cocoa powder may have a D50 value of from 16 grn to about 20 pm, or from about 16 pm to about 18 gm.

The alkalised cocoa powder may have a D50 value of from 18 gm to about 20 pm.

The alkalised cocoa powder may have a D10 value of less than about 5 pm. Thus, 10% of a sample of the alkalised cocoa powder may have a particle size which is smaller than 5 pm.

The alkalised cocoa powder may have a D 1 0 value of less than about 10 gm, 25 about 8 pm, about 6 gm, about 5 gm, about 4 gm, or less than about 2 gm.

The alkalised cocoa powder may have a DI 0 value of from about 2 gni to about 10 pm, from about 4 gm to about 10 gm, from about 5 gm to about 10 pm, from about 6 pm to about 10 gm, or from about 8 gm to about 10 pm.

The alkalised cocoa powder may have a Dl0 value of from 2 pm to about 10 pm, from about 2 pm to about 8 pm, from about 2 pm to about 6 pm, or from about 2 pm to about 4 pm.

The alkalised cocoa powder may have a Dl0 value of from 4 pm to about 10 5 pm, from about 4 pm to about 8 pm, or from about 4 pm to about 6 pm.

The alkalised cocoa powder may have a D10 value of from 6 pm to about 10 pm, or from about 6 pm to about 8 pm.

The alkalised cocoa powder may have a Dl0 value of from 8 pm to about 10 [AM.

Method of measuring D90, D50 and D10 values of the alkalised cocoa powder The D90, D50 and D10 values may be measured using a Malvern Mastersizer with Akomed dispersant. The Malvern Mastersizer is manufactured by Malvern Panalytical Ltd. based in the United Kingdom.

The method follows the ISO standard of ISO 13320:2020.

Laser diffraction is performed using a Malvern Mastersizer equipped with wet dispersion cell and Akomed oil dispersant. A small volume of clean dispersant oil is added to a sample of cocoa powder and ultrasonication is applied until deagglomeration of the cocoa powder into primary particles occurs, forming a pre-dispersion. The pre-dispersion is then added to the instrument which has clean Akomed dispersant oil circulating at a sufficiently high speed to maintain suspension of all cocoa powder particles through the measurement path. The D90, D50 and D 10 values are measured.

The alkalised cocoa powder may have an ash content of less than about 25 wt.%, about 22 wt.%, about 20 wt.%, about 18 wt.%, about 16 wt.%, about 15 wt.%, about 14 wt.%, about 13 wt.%, about 12 wt.%, about 11 wt.%, about 10 wt.%, about 9 wt.%, about 8 wt.%, about 7 wt.%, about 6 wl.%, about 5 wt.%, about 4 wt.%, about 3 wt.%, about 2 wt.%, or less than about 1 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 5 wt.% to about 25 wt.%, from about 8 wt.% to about 22 wt.%, from about 10 wt.% to about 20 wt.%, from about 11 wt.% to about 19 wt.%, from about 12 wt.% to about 18 wt.%, from about 13 wt.% to about 17 wt.%, from about 14 wt.% to about 16 wt.%, or about 15 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of about 1 wt.%, about 2 wt.%, about 3 wt.%, about 4 wt.%, about 5 wt.%, about 6 wt.%, about 7 wt.%, about 8 wt.%, about 9 wt.%, about 10 wt.%, about 11 wt.%, about 12 wt.%, about 13 wt.%, about 14 wt.%, about 15 wt.%, about 16 wt.%, about 17 wt.%, about 18 wt.%, about 19 wt.%, about 20 wt.%, about 21 wt.%, about 22 wt.%, about 23 wt.%, about 24 wt.%, or about 25 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 1 wt.% to about 25 wt.%, from about 1 wt.% to about 22 wt.%, from about 1 wt.% to about 20 wt.%, from about 1 wt.% to about 18 wt.%, from about 1 wt.% to about 16 wt.%, from about 1 wt.% to about 14 wt.%, from about 1 wt.% to about 12 wt.%, from about 1 wt.% to about 10 wt.%, from about 1 wt.% to about 8 wt.%, from about 1 wt.% to about 6 wt.%, from about 1 wt.% to about 4 wt.%, or from about 1 wt.% to about 2 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 2 wt.% to about 25 wt.%, from about 2 wt.% to about 22 wt.%, from about 2 wt.% to about 20 wt.%, from about 2 wt.% to about 18 wt.%, from about 2 wt.% to about 16 wt.%, from about 2 wt.% to about 14 wt.%, from about 2 wt.% to about 12 wt.%, from about 2 wt.% to about 10 wt.%, from about 2 wt.% to about 8 wt.%, from about 2 wt.% to about 6 wt.%, or from about 2 wt.% to about 4 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 4 wt.% to about 25 wt.%, from about 4 wt.% to about 22 wt.%, from about 4 wt.% to about 20 wt.%, from about 4 wt.% to about 18 wt.%, from about 4 wt.% to about 16 wt.%, from about 4 wt.% to about 14 wt.%, from about 4 wt.% to about 12 wt.%, from about 4 wt.% to about 10 wt.%, from about 4 wt.% to about 8 wt.%, or from about 4 wt.% to about 6 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 6 wt.% to about 25 wt.%, from about 6 wt.% to about 22 wt.%, from about 6 wt.% to about 20 wt.%, from about 6 wt.% to about 18 wt.%, from about 6 wt.% to about 16 wt.%, from about 6 wt.% to about 14 wt.%, from about 6 wt.% to about 12 wt.%, from about 6 wt.% to about 10 wt.%, or from about 6 wt.% to about 8 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 8 wt.% to about 25 wt.%, from about 8 wt.% to about 22 wt.%, from about 8 wt.% to about 20 wt.%, from about 8 wt.% to about 18 wt.%, from about 8 wt.% to about 16 wt.%, from about 8 wt.% to about 14 wt.%, from about 8 wt.% to about 12 wt.%, or from about 8 wt.% to about 10 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 10 wt.% to about 25 wt.%, from about 10 wt.% to about 22 wt.%, from about 10 wt.% to about 20 wt.%, from about 10 wt.% to about 18 wt.%, from about 10 wt.% to about 16 wt.%, from about 10 wt.% to about 14 wt.%, or from about 10 wt.% to about 12 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 12 wt.% to about 25 wt.%, from about 12 wt.% to about 22 wt.%, from about 12 wt.% to about 20 wt.%, from about 12 wt.% to about 18 wt.%, from about 12 wt.% to about 16 wt.%, or from about 12 wt.% to about 14 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 14 wt.% to about 25 wt.%, from about 14 wt.% to about 22 wt.%, from about 14 wt.% to about 20 wt.%, from about 14 wt.% to about 18 wt.%, or from about 14 wt.% to about 16 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 16 wt.% to about 25 wt.%, from about 16 wt.% to about 22 wt.%, from about 16 wt.% to about 20 wt.%, or from about 16 wt.% to about 18 wt.%, based on the total weight of the alkalised cocoa powder.

I I

The alkalised cocoa powder may have an ash content of from about 18 wt.% to about 25 wt.%, from about 18 wt.% to about 22 wt.%, or from about 18 wt.% to about 20 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 20 wt.% to about 25 wt.%, or from about 20 wt.% to about 22 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have an ash content of from about 22 wt.% to about 25 wt.%, based on the total weight of the alkalised cocoa powder.

Advantageously, the alkalised cocoa powder having an ash content as defined above, in particular having an ash content of from about 12 wt. % to about 16 wt.%, for example about 14 wt.%, is a relatively low ash content compared to some alkalised cocoa powders of the prior art. As such, the alkalised cocoa powder of the invention may comprise a relatively low concentration of minerals and, therefore, a higher concentration of cocoa. Further, the ash content means that the alkalised cocoa powder is not 'over-alkalised' which may result in a detrimental and off-putting flavour and taste for a consumer. Instead, advantageously, the ash content of the invention provides for a stronger cocoa flavour of the alkalised cocoa powder which is favourable to a consumer.

Method of measuring ash content The ash content of the alkalised cocoa powder is determined using a method based on AOAC 972.15 'Ash of Cocoa Products'. The method to determine ash content comprises weighing a sample of alkalised cocoa powder into a crucible and charring the alkalised cocoa powder on a hotplate then ashing the charred alkalised cocoa powder in a muffle furnace for at least 12 hours. The ashed alkalised cocoa powder is then weighed and its percentage relative to the initial sample of alkalised cocoa powder calculated to determine the ash content (wt.%).

The alkalised cocoa powder may have a potassium content of from about 3500 mg/100g to about 5500 mg/100g, from about 3600 mg/100g to about 5400 mg/100g, from about 3700 mg/100g to about 5300 mg/100g, from about 3800 mg/100g to about 30 5200 mg/100g, from about 3900 ma/1008 to about 5100 mg/1008, from about 4000 mg/100g to about 5000 mg/100g, from about 4100 mg/100g to about 4900 mg/100g, from about 4200 mg/100g to about 4800 mg/100g, from about 4300 mg/100g to about 4700 mg/100g, from about 4400 mg/100g to about 4600 mg/100g, or about 4590 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of about 3500 mg/100g, about 3600 mg/100g, about 3700 mg/100g, about 3800 mg/100g, about 3900 mg/100g, about 4000 me/100e, about 4100 mg/100g, about 4200 me/100e, about 4300 mg/100g. about 4400 mg/100g, about 4500 mg/100g. about 4590 mg/100g, about 4600 mg/100g, about 4700 mg/100g, about 4800 mg/100g, about 4900 mg/100g, about 5000 mg/100g, about 5100 me/100e, about 5200 me/100g, about 5300 mg/100g, about 5400 mg/100g, or about 5500 mg/100a, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of at least about 3500 mg/100g, about 3600 mg/100g, about 3700 mg/100g, about 3800 mg/100g, about 3900 I 5 mg/100g. about 4000 mg/100g, about 4100 mg/100g. about 4200 mg/100g, about 4300 mg/100g, about 4400 ma/1008, about 4500 me/100g, about 4590 ma/1008, about 4600 mg/100g, about 4700 mg/100g, about 4800 mg/100g, about 4900 mg/100g, about 5000 mg/100g. about 5100 mg/100g, about 5200 mg/100g. about 5300 mg/100g, about 5400 mg/100g, or at least about 5500 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 3500 mg/100g to about 5500 me/100g, from about 3500 mg/100g to about 5400 ma/100g, from about 3500 mg/100g to about 5300 mg/100g, from about 3500 mg/100g to about 5200 mg/100g, from about 3500 me/100e to about 5100 mg/100e, from about 3500 mg/100g to about 5000 mg/100g, from about 3500 mg/100g to about 4900 mg/100g, from about 3500 mg/1008 to about 4800 me/100g, from about 3500 ma/100g to about 4700 mg/100g, from about 3500 ma/1008 to about 4600 ma/1008, from about 3500 mg/100g to about 4500 mg/100g, from about 3500 mg/100g to about 4400 mg/100g, from about 3500 mg/100g to about 4300 mg/100g, from about 3500 mg/100g to about 4200 mg/100g, from about 3500 ma/1008 to about 4100 ma/1008, from about 3500 mg/100g to about 4000 me/100g, from about 3500 mg/100g to about 3900 ma/100g, from about 3500 mg/100g to about 3800 mg/100g, from about 3500 mg/100g to about 3700 mg/100g, or from about 3500 mg/100g to about 3600 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 3600 mg/100g to about 5500 mg/100g, from about 3600 mg/100g to about 5400 mg/100g, from about 3600 mg/100g to about 5300 mg/100g, from about 3600 mg/100g to about 5200 mg/100g, from about 3600 mg/100g to about 5100 mg/100g, from about 3600 mg/100g to about 5000 mg/100g, from about 3600 mg/100g to about 4900 mg/100g, from about 3600 mg/100g to about 4800 mg/100g, from about 3600 mg/100g to about.

4700 mg/100g, from about 3600 ma/100g to about 4600 mg/100g, from about 3600 mg/100g to about 4500 mg/100g, from about 3600 mg/100g to about 4400 ma/100g, from about 3600 mg/100g to about 4300 mg/100g, from about 3600 mg/100g to about 4200 mg/100g, from about 3600 mg/100g to about 4100 mg/100g, from about 3600 mg/100g to about 4000 ma/100g, from about 3600 mg/100g to about 3900 ma/100g, from about 3600 mg/100g to about 3800 mg/100g, or from about 3600 mg/1008 to about 3700 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 3700 mg/100g to about 5500 mg/100g, from about 3700 mg/100g to about 5400 rng/100g, from about 3700 mg/100g to about 5300 mg/100g, from about 3700 mg/100g to about 5200 mg/100g, from about 3700 ma/100g to about 5100 mg/100g, from about 3700 mg/100g to about 5000 mg/100g, from about 3700 mg/100g to about 4900 ma/100g, from about 3700 mg/100g to about 4800 mg/100g, from about 3700 mg/100g to about 4700 mg/100g, from about 3700 mg/100g to about 4600 mg/100g, from about 3700 mg/100g to about 4500 mg/100g, from about 3700 mg/100g to about 4400 mg/100g, from about 3700 ma/100g to about 4300 mg/100g, from about 3700 ma/100g to about 4200 mg/100g, from about 3700 mg/100g to about 4100 mg/100g, from about 3700 mg/100g to about 4000 mg/100g, from about 3700 mg/100g to about 3900 mg/100g, or from about 3700 mg/100g to about 3800 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 3800 mg/100g to about 5500 ma/100g, from about 3800 mg/100g to about 5400 ma/100g, from about 3800 mg/100g to about 5300 mg/100g, from about 3800 mg/100g to about 5200 mg/100g, from about 3800 mg/100g to about 5100 mg/100g, from about 3800 mg/100g to about 5000 mg/100g, from about 3800 mg/100g to about 4900 mg/100g, from about 3800 mg/100g to about 4800 mg/100a, from about 3800 mg/100g to about 5 4700 mg/100g, from about 3800 mg/100g to about 4600 mg/100g, from about 3800 mg/100g to about 4500 mg/100g, from about 3800 mg/100g to about 4400 ma/100g, from about 3800 mg/1008 to about 4300 mg/100g, from about 3800 ma/100g to about 4200 mg/100g, from about 3800 mg/100g to about 4100 mg/100g, from about 3800 mg/100g to about 4000 mg/100g, or from about 3800 mg/100g to about 3900 mg/100g, 10 based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 3900 mg/100g to about 5500 mg/100g, from about 3900 mg/100g to about 5400 mg/100g, from about 3900 mg/100g to about 5300 mg/100g, from about 3900 mg/100g to about 5200 mg/100g, from about 3900 mg/100g to about 5100 mg/100g, from about 3900 mg/100g to about 5000 mg/100g, from about 3900 mg/100g to about 4900 ma/100g, from about 3900 mg/100g to about 4800 mg/100g, from about 3900 mg/100g to about 4700 mg/100g, from about 3900 ma/1002 to about 4600 ma/1002, from about 3900 mg/100g to about 4500 mg/100g, from about 3900 mg/100g to about 4400 mg/100g, from about 3900 mg/100g to about 4300 mg/100g, from about 3900 mg/100g to about 4200 mg/100g, from about 3900 mg/100g to about 4100 mg/100g, or from about 3900 mg/100g to about 4000 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4000 mg/100g to about 5500 mg/100g, from about 4000 mg/100g to about 5400 mg/100g, from about 4000 mg/100g to about 5300 mg/100g, from about 4000 ma/100g to about 5200 mg/100g, from about 4000 mg/100g to about 5100 mg/100g, from about 4000 mg/100g to about 5000 mg/100g, from about 4000 mg/100g to about 4900 mg/100g, from about 4000 mg/100g to about 4800 mg/100g, from about 4000 ma/100g to about. 4700 mg/100g, from about 4000 mg/100g to about 4600 mg/100g, from about 4000 mg/100g to about 4500 mg/100g, from about 4000 mg/100g to about 4400 mg/100g, from about 4000 mg/100g to about 4300 mg/100g, from about 4000 mg/100g to about 4200 mg/100g, or from about 4000 mg/100g to about 4100 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4100 mg/100g to about 5500 mg/100g, from about 4100 mg/100g to about 5400 mg/100g, 5 from about 4100 mg/100g to about 5300 mg/100g, from about 4100 mg/100g to about 5200 mg/100g, from about 4100 mg/100g to about 5100 mg/100g, from about 4100 mg/100g to about 5000 mg/100g, from about 4100 mg/100g to about 4900 ma/100g, from about 4100 mg/100g to about 4800 mg/100g, from about 4100 mg/100g to about 4700 mg/100g, from about 4100 mg/100g to about 4600 mg/100g, from about 4100 10 mg/100g to about 4500 ma/100g, from about 4100 mg/100g to about 4400 ma/100g, from about 4100 mg/100a to about 4300 mg/100g, or from about 4100 mg/100g to about 4200 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4200 mg/100g to about 5500 mg/100g, from about 4200 mg/100g to about 5400 mg/100g, from about 4200 mg/100g to about 5300 mg/100g, from about 4200 mg/100g to about 5200 mg/100g, from about 4200 ma/1008 to about 5100 ma/1008, from about 4200 mg/100g to about 5000 mg/100g, from about 4200 mg/100g to about 4900 mg/100g, from about 4200 mg/100g to about 4800 mg/100g, from about 4200 mg/100g to about 4700 mg/100g, from about 4200 mg/100g to about 4600 mg/100g, from about 4200 mg/100g to about 4500 mg/100g, from about 4200 ma/100g to about 4400 ma/100g, or from about 4200 mg/100g to about 4300 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4300 mg/100g to about 5500 ma/100g, from about 4300 mg/100g to about 5400 ma/100g, from about 4300 mg/100g to about 5300 mg/100g, from about 4300 mg/100g to about 5200 mg/100g, from about 4300 ma/1008 to about 5100 ma/1008, from about 4300 mg/100g to about 5000 ma/100g, from about 4300 mg/100g to about 4900 ma/100g, from about 4300 mg/100g to about 4800 mg/100g, from about 4300 mg/100g to about 4700 mg/100g, from about 4300 mg/100g to about 4600 mg/100g, from about 4300 mg/100g to about 4500 mg/100g, or from about 4300 ma/100g to about 4400 ma/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4400 mg/100g to about 5500 mg/100g, from about 4400 mg/100g to about 5400 mg/100g, from about 4400 mg/100g to about 5300 mg/100g, from about 4400 mg/100g to about 5200 mg/100g, from about 4400 ma/1008 to about 5100 mg/1008, from about 4400 mg/100g to about 5000 mg/100g, from about 4400 mg/100g to about 4900 mg/100g, from about 4400 mg/100g to about 4800 mg/100g, from about 4400 ma/100g to about. 4700 mg/100g, from about 4400 mg/100g to about 4600 mg/100g, or from about 4400 mg/100g to about 4500 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4500 mg/100g to about 5500 mg/100g, from about 4500 mg/100g to about 5400 ma/100g, from about 4500 mg/100g to about 5300 mg/100g, from about 4500 mg/100g to about 5200 mg/100g, from about 4500 mg/100g to about 5100 mg/100g, from about 4500 mg/100g to about 5000 mg/100g, from about 4500 mg/100g to about 4900 ma/100g, from about 4500 mg/100g to about 4800 mg/100g, from about 4500 ma/100g to about 4700 mg/100g, or from about 4500 mg/100g to about 4600 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4600 mg/100g to about 5500 mg/100g, from about 4600 mg/100g to about 5400 mg/100g, from about 4600 mg/100g to about 5300 mg/100g, from about 4600 ma/100g to about. 5200 mg/100g, from about 4600 mg/100g to about 5100 mg/100g, from about 4600 mg/100g to about 5000 mg/100g, from about 4600 mg/100g to about 4900 nag/100g, from about 4600 mg/100g to about 4800 mg/100g, or from about 4600 mg/100g to about 4700 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4700 mg/100g to about 5500 mg/100g, from about 4700 mg/100g to about 5400 ma/100g, from about 4700 mg/100g to about 5300 mg/100g, from about 4700 ma/100g to about 5200 mg/100g, from about 4700 mg/100g to about 5100 mg/100g, from about 4700 mg/100g to about 5000 mg/100g, from about 4700 mg/100g to about 4900 mg/100g, or from about 4700 mg/100g to about 4800 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4800 mg/100g to about 5500 mg/100g, from about 4800 mg/100g to about 5400 mg/100g, from about 4800 mg/100g to about 5300 mg/100g, from about 4800 mg/100g to about 5200 mg/100g, from about 4800 ma/1008 to about 5100 mg/1008, from about 4800 mg/100g to about 5000 mg/100g, or from about 4800 mg/100g to about 4900 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 4900 mg/100g to about 5500 mg/100g, from about 4900 mg/100g to about 5400 mg/100g, from about 4900 mg/100g to about 5300 mg/100g, from about 4900 mg/100g to about.

5200 mg/100e, from about 4900 mg/100g to about 5100 mg/100g, or from about 4900 mg/100g to about 5000 ma/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 5000 mg/100g to about 5500 mg/100g, from about 5000 mg/100g to about 5400 mg/100g, from about 5000 mg/100g to about 5300 mg/100g, from about 5000 mg/100g to about 5200 mg/100g, or from about 5000 mg/100g to about 5100 ma/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 5100 mg/100g to about 5500 ma/100g, from about 5100 mg/100g to about 5400 ma/100g, 20 from about 5100 mg/100g to about 5300 mg/100g, or from about 5100 mg/100g to about 5200 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 5200 mg/100g to about 5500 mg/100g, from about 5200 me/100g to about 5400 me/100g, or from about 5200 mg/100g to about 5300 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 5300 mg/100g to about 5500 mg/100g, or from about 5300 mg/100g to about 5400 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a potassium content of from about 5400 mg/100g to about 5500 mg/100g, based on the total weight of the alkalised cocoa powder.

Advantageously, an alkalised cocoa powder having a potassium content of from about 3500 mg/100g to about 5500 mg/100g provides significant health benefits to the consumer of the cocoa powder. For example, an alkalised cocoa powder having a potassium content of from about 3500 mg/100g to about 5500 mg/100g can lower the blood pressure of the consumer. This health benefit is enhanced in embodiments of the invention which comprise an alkalised cocoa powder having a sodium content of less than about 150 mg/100g, in particular less than about 100 mg/100g, particularly less than about 50 ma/100g, and even more particularly less than about 40 ma/100g, for example about 32 mg/100g, based on the total weight of the alkalised cocoa powder.

Moreover, embodiments of the invention having a potassium content as described above is such that the alkalised cocoa powder is sufficiently alkalised to provide desirable colour and flavour profiles without requiring the quantities of sodium and/or ammonium alkalis of alkalised cocoa powders of the prior art. Thus, comparatively to known alkalised cocoa powders comprised in the prior art, the invention may have a reduced sodium and/or ammonia content, for example the invention may have a reduced sodium content and may not comprise any ammonium alkali compound.

The alkalised cocoa powder may be formed using an alkali agent which does not comprise any ammonium compounds.

The alkalised cocoa powder may not comprise ammonium compounds. The alkalised cocoa powder may not comprise ammonium alkali compounds.

Thus, in respect of the reduced sodium content, it is advantageous that the alkalised cocoa powder of the invention may have a sodium content which is no greater than the natural sodium content of cocoa beans. This is beneficial at least in respect of marketing the alkalised cocoa powder whereby it can be marketed as having no artificial sodium added to it, making the product more appealing to consumers, in particular in relation to corresponding health benefits of foodstuffs comprising relatively low quantities of sodium.

Further, in respect of ammonia-based alkalis, the alkalised cocoa powder of the invention may avoid the toxicity and volatility associated with ammonia-based compounds used in preparing alkalised cocoa powders. Avoiding the use of ammonia is beneficial for operators, the environment and handling, as it is volatile and environmentally toxic.

Surprisingly, the present invention may provide for an alkalised cocoa powder which is sufficiently alkalised to provide desirable colour and flavour profiles without the use of relatively strong ammonium-based alkalis, and without the use of large quantities of a sodium-based alkali, for example sodium hydroxide, which is often used in the prior art as a substitute for strong ammonium-based alkalis, or to supplement strong ammoni urn-based alkalis.

Moreover, in embodiments comprising a sodium content of less than about 150 mg/100g, the alkalised cocoa powder can be advantageously used to produce food and beverage products. This is because the alkalised cocoa powder does not contribute a significant addition of sodium to the resulting product, therefore, does not disadvantageously affect labelling or marketing of the resulting product. As such, the alkalised cocoa powder of the invention may find particular benefit in being used to produce products in which it is desired to maintain a low sodium content.

The alkalised cocoa powder may have a sodium content of less than about 150 mg/100g, about 140 mg/100g, about 130 mg/100g, about 120 mg/100g, about 110 mg/100g, about 100 mg/100g, about 90 mg/100g, about 80 mg/100g, about 70 mg/100g, about 60 mg/100g, about 50 mg/100g, about 40 mg/100g, about 30 nag/100g, about 20 mg/100g, about 10 mg/100g, or less than about 5 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of about 5 mg/100g, about 10 mg/100g, about 15 mg/100g, about 20 mg/100g, about 25 mg/100g, about 30 mg/100g, about 32 mg/100g, about 35 mg/100g, about 40 rng/100g, about 45 mg/100g, 30 about 50 mg/100g, about 55 mg/100g. about 60 mg/100g. about 65 mg/100g, about 70 mg/100g, about 75 mg/100g, about 80 mg/100g, about 85 mg/100g, about 90 mg/100g, about 95 mg/100g, about 100 mg/100g, about 105 mg/100g, about 110 mg/100g, about 115 mg/100g, about 120 mg/100g, about 125 mg/100g, about 130 mg/100g, about 135 mg/100g, about 140 mg/100g, about 145 mg/1008, or about 150 me/100e, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about IS mg/100g to about 45 mg/100e, from about 20 mg/100e to about 40 me/100g, from about 25 mg/100g to about 38 mg/100g, from about 28 mg/100g to about 35 mg/100g, from about 30 mg/100g to about 34 mg/100g, from about 31 mg/100g to about 33 mg/100g, or about 32 me/100e, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 5 mg/100g to about 150 mg/100g, from about 5 mg/100g to about 140 mg/100g, from about 5 mg/100g to about 130 mg/100e, from about 5 ma/100g to about 120 ma/100g, from about 5 mg/100g to about 110 mg/100g, from about 5 mg/100g to about 100 mg/100g, from about 5 mg/100g to about 90 mg/100g, from about 5 mg/100g to about mg/100g, from about 5 mg/100g to about 70 mg/100g, from about 5 mg/100g to about 60 mg/100g, from about 5 mg/100g to about 50 mg/100g, from about 5 mg/100g to about 40 mg/100g, from about 5 mg/100g to about 30 mg/100g, from about 5 mg/100g to about 20 mg/100g, or from about 5 mg/100g to about 10 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 10 mg/100g to about 150 mg/100g, from about 10 ma/100g to about 140 mg/1008, from about 10 mg/100g to about 130 mg/100g, from about 10 mg/100g to about 120 mg/100g, from about 10 mg/100g to about 110 mg/100g, from about 10 mg/100g to about 100 mg/100g, from about 10 mg/100g to about 90 mg/100g, from about 10 mg/100g to about 80 mg/1008, from about 10 mg/1008 to about 70 ma/100g, from about 10 mg/100g to about 60 mg/100e, from about 10 mg/100g to about 50 ma/100g, from about 10 mg/100g to about 40 mg/100g, from about 10 mg/100g to about 30 mg/100g, or from about 10 mg/100g to about 20 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 20 mg/100g to about 150 mg/100g, from about 20 mg/100g to about 140 mg/100g, from about 20 mg/100g to about 130 mg/100g, from about 20 mg/100g to about 120 mg/100g, from about 20 mg/100g to about 110 mg/100g, from about 20 mg/100g to about 100 mg/100g, from about 20 mg/100g to about 90 nig/100g, from about 20 mg/100g to about 80 mg/1008, from about 20 mg/1008 to about 70 ma/100g, from about 20 mg/100g to about 60 mg/1002, from about 20 mg/100g to about 50 ma/100g, from about 20 mg/1008 to about 40 mg/100g, or from about 20 mg/100g to about 30 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 30 mg/100g to about 150 ma/100g, from about 30 ma/100g to about 140 mg/1008, from about 30 mg/100g to about 130 mg/100g, from about 30 mg/100g to about 120 mg/100g, from about 30 mg/100g to about 110 mg/100g, from about 30 mg/100g to about 100 mg/100g, from about 30 mg/100g to about 90 ma/100g, from about 30 mg/100g to about 80 mg/1008, from about 30 mg/1008 to about 70 ma/100g, from about 30 mg/100g to about 60 mg/100g, from about 30 mg/100g to about 50 rng/100g, or from about 30 mg/1008 to about 40 ma/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 40 mg/100g to about 150 ma/100g, from about 40 ma/100g to about 140 mg/1008, from about 40 mg/100g to about 130 mg/100g, from about 40 mg/100g to about 120 mg/100g, from about 40 mg/100g to about 110 mg/100g, from about 40 mg/100g to about 100 mg/100g, from about 40 mg/100g to about 90 mg/100g, from about 40 mg/100g to about 80 mg/100g, from about 40 mg/100g to about 70 mg/100g, from about 40 ma/100g to about 60 mg/100g, or from about 40 mg/100g to about 50 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 50 mg/100g to about 150 mg/100g, from about 50 mg/100g to about 140 mg/100g, from about 50 mg/100g to about 130 mg/100g, from about 50 mg/100g to about 120 mg/100g, from about 50 mg/100g to about 110 mg/100g, from about 50 mg/100g to about 100 mg/100g, from about 50 mg/100g to about 90 ma/100g, from about 50 mg/100g to about 80 mg/100g, from about 50 mg/100g to about 70 mg/100g, or from about 50 mg/100g to about 60 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 60 mg/100g to about 150 mg/100g, from about 60 mg/100g to about 140 mg/100g, from about 60 mg/100g to about 130 mg/100g, from about 60 mg/100g to about 120 mg/100g, from about 60 mg/100g to about 110 mg/100g, from about 60 mg/100g to about 100 mg/100g, from about 60 mg/100g to about 90 mg/100g, from about 60 mg/100g to about 80 mg/100g, or from about 60 mg/100g to about 70 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 70 mg/100g to about 150 mg/100g, from about 70 mg/100g to about 140 mg/100g, from about 70 ma/100g to about 130 mg/1008, from about 70 mg/100g to about 120 mg/100g, from about 70 mg/100g to about 110 mg/100g, from about 70 mg/100g to about 100 mg/100g, from about 70 mg/100g to about 90 mg/100g, or from about 70 mg/100g to about 80 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 80 mg/100g to about 150 ma/100g, from about 80 ma/100g to about 140 mg/1008, from about 80 ma/100g to about 130 mg/1008, from about 80 mg/100g to about 120 mg/100g, from about 80 mg/100g to about 110 mg/100g, from about 80 mg/100g to about 100 mg/100g, or from about 80 mg/100g to about 90 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 90 mg/100g to about 150 nag/100g, from about 90 mg/100g to about 140 mg/100g, from about 90 ma/100g to about 130 mg/100a, from about 90 mg/100g to about 120 mg/100g, from about 90 mg/100g to about 110 mg/100g, or from about 90 mg/100g to about 100 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 100 mg/100g to about 150 mg/100g, from about 100 mg/100g to about 140 mg/100g, from 30 about 100 mg/100g to about 130 mg/100g, from about 100 mg/100g to about 120 mg/100g, or from about 100 mg/100g to about 110 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 110 mg/100g to about 150 mg/100g, from about 110 mg/100g to about 140 mg/100g, from 5 about 110 mg/100g to about 130 mg/100g, or from about 110 mg/100g to about 120 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 120 mg/100g to about 150 mg/100a, from about 120 mg/100g to about 140 mg/100g, or from about 120 mg/100g to about 130 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 130 mg/100g to about 150 mg/100g, or from about 130 mg/100g to about 140 mg/100g, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may have a sodium content of from about 140 mg/100g to about 150 mg/100g, based on the total weight of the alkalised cocoa powder. As such, the alkalised cocoa powder of the invention may have a sodium content which is no greater than the natural sodium content of cocoa beans. Thus, the alkalised cocoa powder of the invention may have no sodium artificially added. This is beneficial not least from a marketing perspective whereby the cocoa powder can he marketed as having no artificial sodium added to it, making the product more appealing to consumers.

It follows that it is also advantageous that the alkalised cocoa powder comprises a relatively low sodium content. As such, the cocoa powder provides health benefits (for example, lowering blood pressure) to a consumer, compared to cocoa powders of the prior art which comprise a sodium level greater than the natural sodium content of cocoa beans.

Method of measuring sodium and potassium content 2g samples of alkalised cocoa powder are prepared by ashing a sample portion of alkalised cocoa powder in a muffle furnace for at least 12 hours at 550'C. The ashed 30 alkalised cocoa powder is then mixed with 5m1 50% HC1 dilute acid to form a mixture and the mixture is gently heated (until convection is observed) for no longer than 30 minutes. The mixture is then cooled and made to a standard volume using ultrapure water. The standard volume of the sample is then diluted as necessary to a working range of a wavelength selected on an atomic absorption apparatus, to form prepared test.

solutions.

A process blank and duplicate preparations should also he prepared, along with a spiked sample.

Standards are prepared in matrix-matched solutions. Calibrations are prepared to he appropriate to the level of analyte in the samples to minimise dilutions while ensuring the samples are within a calibration range.

The prepared test solution is aspirated into a flame, which produces ground-state atoms of the elements present. A hollow cathode lamp consisting of, or containing, the element to be analysed emits light of a wavelength specific to the element and this passes through the flame. The ground-state atoms absorb light and are transformed to an excited state by absorption of light-energy equal to the difference in energy between the two states. The light then passes through a monochromator that isolates the specific wavelength and passes it to a detector. Since the amount of light absorbed by the element is proportional to its concentration, by comparing the absorbance due to the element in the test solution to that of standard solutions of the element, the amount of element present in the test solution, and hence the sample, can be determined.

After analysis on the atomic absorption apparatus, the concentration of the element is calculated and reported.

The colour of cocoa powders can be expressed using the Hunter colour coordinate scale or CIE 1976 (CIELAB) colour system which uses three coordinates (or values) to define the colour profile of a cocoa powder. The L coordinate represents brightness and can assume values between 0 (for black) and 100 (for white); the a value represents the red component (a>0); and the h value represents the yellow component (b>0).

The alkalised cocoa powder may have a colour L-value of from about 17.0 to about 26.0, from about 17.5 to about 25.5, from about 18.0 to about 25.0, from about 18.5 to about 24.5, from about 19.0 to about 24.0, from about 19.5 to about 23.5, from about 20.0 to about 23.0, from about 20.5 to about 22.5, from about 21.0 to about 22.0, or about 21.5.

The alkalised cocoa powder may have a colour L-value of about 17.0, about 17.5, about 18.0, about 18.5, about 19.0, about 19.5, about 20.0, about 20.5, about 21.0, about 21.5, about 22.0, about 22.5, about 23.0, about 23.5, about 24.0, about 24.5, about 25.0, about 25.5, or about 26.0.

The alkalised cocoa powder may have a colour L-value of from about 17.0 to about 26.0, from about 17.0 to about 25.5, from about 17.0 to about 25.0, from about 17.0 to about 24.5, from about 17.0 to about 24.0, from about 17.0 to about 23.5, from about 17.0 to about 23.0, from about 17.0 to about 22.5, from about 17.0 to about 22.0, from about 17.0 to about 21.5. from about 17.0 to about 21.0, from about 17.0 to about 20.5, from about 17.0 to about 20.0, from about 17.0 to about 19.5, from about 17.0 to about 19.0, from about 17.0 to about 18.5, from about 17.0 to about 18.0, or from about 17.0 to about 17.5.

The alkalised cocoa powder may have a colour L-value of from about 17.5 to about 26.0, from about 17.5 to about 25.5, from about 17.5 to about 25.0, from about 17.5 to about 24.5, from about 17.5 to about 24.0. from about 17.5 to about 23.5, from about 17.5 to about 23.0, from about 17.5 to about 22.5, from about 17.5 to about 22.0, from about 17.5 to about 21.5, from about 17.5 to about 21.0, from about 17.5 to about 20.5, from about 17.5 to about 20.0, from about 17.5 to about 19.5, from about 17.5 to about 19.0, from about 17.5 to about 18.5, or from about 17.5 to about 18.0.

The alkalised cocoa powder may have a colour L-value of from about 18.0 to about 26.0, from about 18.0 to about 25.5, from about 18.0 to about 25.0, from about 18.0 to about 24.5. from about 18.0 to about 24.0, from about 18.0 to about 23.5, from about 18.0 to about 23.0, from about 18.0 to about 22.5, from about 18.0 to about 22.0, from about 18.0 to about 21.5, from about 18.0 to about 21.0, from about 18.0 to about 20.5, from about 18.0 to about 20.0, from about 18.0 to about 19.5, from about 18.0 to about 19.0, or from about 18.0 to about 18.5.

The alkalised cocoa powder may have a colour L-value of from about 18.5 to about 26.0, from about 18.5 to about 25.5, from about 18.5 to about 25.0, from about 18.5 to about 24.5, from about 18.5 to about 24.0, from about 18.5 to about 23.5, from about 18.5 to about 23.0, from about 18.5 to about 22.5, from about 18.5 to about 22.0, from about 18.5 to about 21.5, from about 18.5 to about 21.0, from about 18.5 to about 20.5, from about 18.5 to about 20.0, from about 18.5 to about 19.5, or from about 18.5 to about 19.0.

The alkalised cocoa powder may have a colour L-value of from about 19.0 to about 26.0, from about 19.0 to about 25.5, from about 19.0 to about 25.0, from about 19.0 to about 24.5, from about 19.0 to about 24.0, from about 19.0 to about 23.5, from about 19.0 to about 23.0, from about 19.0 to about 22.5, from about 19.0 to about 22.0, from about 19.0 to about 21.5, from about 19.0 to about 21.0, from about 19.0 to about 20.5, from about 19.0 to about 20.0, or from about 19.0 to about 19.5.

The alkalised cocoa powder may have a colour L-value of from about 19.5 to about 26.0, from about 19.5 to about 25.5, from about 19.5 to about 25.0, from about 19.5 to about 24.5, from about 19.5 to about 24.0, from about 19.5 to about 23.5, from about 19.5 to about 23.0, from about 19.5 to about 22.5, from about 19.5 to about 22.0, from about 19.5 to about 21.5, from about 19.5 to about 21.0, from about 19.5 to about 20.5, or from about 19.5 to about 20.0.

The alkalised cocoa powder may have a colour L-value of from about 20.0 to about 26.0, from about 20.0 to about 25.5, from about 20.0 to about 25.0, from about 20.0 to about 24.5, from about 20.0 to about 24.0, from about 20.0 to about 23.5, from about 20.0 to about 23.0, from about 20.0 to about 22.5, from about 20.0 to about 22.0, from about 20.0 to about 21.5, from about 20.0 to about 21.0, or from about 20.0 to about 20.5.

The alkalised cocoa powder may have a colour L-value of from about 20.5 to about 26.0, from about 20.5 to about 25.5. from about 20.5 to about 25.0, from about 20.5 to about 24.5, from about 20.5 to about 24.0, from about 20.5 to about 23.5, from about 20.5 to about 23.0, from about 20.5 to about 22.5, from about 20.5 to about 22.0, from about 20.5 to about 21.5. or from about 20.5 to about 21.0.

The alkalised cocoa powder may have a colour L-value of from about 21.0 to about 26.0, from about 21.0 to about 25.5, from about 21.0 to about 25.0, from about 21.0 to about 24.5, from about 21.0 to about 24.0, from about 21.0 to about 23.5, from about 21.0 to about 23.0, from about 21.0 to about 22.5, from about 21.0 to about 22.0, or from about 21.0 to about 21.5.

The alkalised cocoa powder may have a colour L-value of from about 21.5 to about 26.0, from about 21.5 to about 25.5, from about 21.5 to about 25.0, from about 21.5 to about 24.5, from about 21.5 to about 24.0, from about 21.5 to about 23.5, from about 21.5 to about 23.0, from about 21.5 to about 22.5, or from about 21.5 to about 22.0.

The alkalised cocoa powder may have a colour L-value of from about 22.0 to about 26.0, from about 22.0 to about 25.5, from about 22.0 to about 25.0, from about 22.0 to about 24.5, from about 22.0 to about 24.0, from about 22.0 to about 23.5, from about 22.0 to about 23.0, or from about 22.0 to about 22.5.

The alkalised cocoa powder may have a colour L-value of from about 22.5 to about 26.0, from about 22.5 to about 25.5, from about 22.5 to about 25.0, from about 22.5 to about 24.5, from about 22.5 to about 24.0, from about 22.5 to about 23.5, or from about 22.5 to about 23.0.

The alkalised cocoa powder may have a colour L-value of from about 23.0 to about 26.0, from about 23.0 to about 25.5, from about 23.0 to about 25.0, from about 23.0 to about 24.5, from about 23.0 to about 24.0, or from about 23.0 to about 23.5.

The alkalised cocoa powder may have a colour L-value of from about 23.5 to about 26.0, from about 23.5 to about 25.5, from about 23.5 to about 25.0, from about 23.5 to about 24.5, or from about 23.5 to about 24.0.

The alkalised cocoa powder may have a colour L-value of from about 24.0 to about 26.0, from about 24.0 to about 25.5, from about 24.0 to about 25.0, or from about 24.0 to about 24.5.

The alkalised cocoa powder may have a colour L-value of from about 24.5 to about 26.0, or from about 24.5 to about 25.5, from about 24.5 to about 25.0.

The alkalised cocoa powder may have a colour L-value of from about 25.0 to about 26.0, or from about 25.0 to about 25.5.

The alkalised cocoa powder may have a colour L-value of from about 25.5 to about 26.0.

Advantageously, a colour L-value of from about 17.0 to about 26.0 is indicative of a cocoa powder with a darker and more 'red-brown' colour. The cocoa powder of the invention may therefore be suitable for producing a food or beverage product having a tailored colour profile.

It is further advantageous that the alkalised cocoa powder of the present invention may exhibit a darker colour profile compared to non-alkalised cocoa powder while not comprising a relatively high pH as is common in alkalised cocoa powders of the prior art. As such relatively high pH values, for example pH 6.70 or above, can provide an undesirable alkaline flavour and odour profile. It is therefore favourable that this embodiment of the invention has a colour L-value of from about 17.0 to about 26.0 and therefore exhibits a darker colour profile compared to non-alkalised cocoa powders, and has a pH of about 6.10 to about 6.65 and therefore does not provide an undesirable alkaline flavour and odour profile as found with some alkalised cocoa powders.

An alkalised cocoa powder having a colour L-value of from about 17.0 to about 26.0 is further advantageous because the alkalised cocoa powder of the present invention may be used on its own or may be mixed with other cocoa powders to produce food and beverage products with tailored colour and flavour profiles. Advantageously, the alkalised cocoa powder can he used to decrease costs or increase cost margins, since smaller quantities of the alkalised cocoa powder can be used to achieve the same colour impact as larger quantities of standard, non-alkalised cocoa powders.

Method of measuring colour L-value -White diluent method Overview Guar gum solution A guar gum solution is prepared by combining 4.0g sodium chloride in 390g deionized water with 4.00g guar gum in 10m1 ethanol, at room temperature and ambient pressure.

Cornstarch solution A cornstarch solution is prepared by slowly adding 100g cornstarch to 100g deionized water while mixing at room temperature and ambient pressure.

White diluent solution The guar gum solution and the cornstarch solution are then combined, at room temperature and ambient pressure, while mixing to form a while diluent solution.

Alkalised cocoa powder preparation A sample of alkalised cocoa powder is prepared according to the following method: A. Turn on a heating bath containing water and heat the water to 60°C; B. Place a beaker containing an excess of deionized water for the number of analyses into the water bath; C. Insert a thermometer into the beaker containing the water to monitor the temperature; D. Alternately, a sufficient volume of freshly boiled deionized water is mixed with cold water until a temperature of 60°C is achieved; E. Weigh 2.0+/-0.02g of cocoa powder into a 250 ml plastic sample container with a metal screw-top lid; F. Use an automated 2-20m1 pipette to transfer 10m1 of deionized water at 60°C from the beaker into the plastic sample container containing the cocoa powder; G. Use a spatula to mix the cocoa powder and water into a smooth paste.

Ensure that all of the powder is incorporated into the paste, as any non-suspended powder will cause measurement error; H. Place the plastic sample container containing the cocoa paste on a technical balance; I. Tare the balance and add 100g white diluent solution into the plastic sample container. Screw lid hack onto container. Homogenize the sample by shaking vigorously to ensure complete sample dispersion. Ensure no black cocoa paste is sticking to the side or the bottom of the cup/beaker prior to analysing the solution.

The sample is then analysed using a spectrophotometer (Konica Minolta. CM5 or HunterLab Colorquest XE) with specular reflectance excluded.

Instrument parameter set up Geometry: Diffuse illumination 8° viewing Standard Observer: CIELAB 10° Standard light source: D65 Measurement mode: Reflectance specular excluded Colour space: L*, a*, b* Port* 30mm (Minolta CM 5) Port: Large Port (Colorquest XE) The diffuse reflected light is collected, and from the spectral data obtained, the Standard Colour values X, Y and Z (Y, x, y depending on the instrument) are calculated.

These are then transformed to the colour parameters L, a and b according to the CIE LAB system.

Definition of GE LAB system The colour of products is represented by the following parameters: L, brightness (scale from 0 = dark to 100 = white).

a, red-green scale (+a for red; -a for green; the higher the numerical value, the more intensive the colour impression).

b, yellow-blue scale (+1) for yellow; -h for blue; the higher the numerical value, the more intensive the colour impression).

Analytical Quality Control A batch of High Flavour Cocoa (HFC) powder comparator with known measured L-value should he set aside to perform quality control (QC) checks on the sample assay. The L-values are measured using the instrument parameter conditions defined above. The HFC powder used can be independently sourced by the user laboratories, or for best practice, a powder shall be supplied by Mondelez or the manufacturer and, used by both Mondelez and manufacturer for assay QC purposes.

For each new batch of white diluent a fresh QC sample must be prepared in order to assess correct preparation of the samples. The use of a Shewhart chart to follow measured L-values, to determine if the measured L-values are trending over time, to ensure consistency with previous results, and to determine replacement of the QC lot of powder, should he undertaken.

The alkalised cocoa powder may be a high-fat cocoa powder, with more than 12% fat by weight, a standard-fat cocoa powder having 10-12% fat by weight, or a low-fat, or fat-free, cocoa powder having less than 10% fat by weight.

The alkalised cocoa powder may comprise a fat content of less than about 15 wt.%, about 14 wt.%, about 13 wt.%, about 12 wt.%, about 11 wt.%, about 10 wt.%, about 9 wt.%, about 8 wt.%, about 7 wt.%, about 6 wt.%, about 5 wt.%, about 4 wt.%, about 3 wt.%, about 2 wt.%, or less than about 1 wt.%.

The alkalised cocoa powder may comprise a fat content of about 15 wt.%, about 14 wt.%, about 13 wt.%, about 12 wt.%, about 11 wt.%, about 10 wt.%, about 9 wt.%, about 8 wt.%, about 7 wt.%, about 6 wt,%, about 5 wt.%, about 4 wt,%, about 3 wt.%, about 2 wt.%, or about 1 wt.%.

The alkalised cocoa powder may comprise a fat content of from about 1 wt.% to about 15 wt.%, from about 1 wt.% to about 14 wt.%, from about 1 wt.% to about 13 wt.%, from about 1 wt.% to about 12 wt.%, from about 1 wt.% to about 11 wt.%, from about 1 wt.% to about 10 wt,%, from about 1 wt.% to about 9 wt.%, from about 1 wt.% to about 8 wt.%, from about 1 wt.% to about 7 wt.%, from about 1 wt.% to about 6 wt.%, from about 1 wt.% to about 5 wt.%, from about 1 wt.% to about 4 wt.%, from about 1 wt.% to about 3 wt.%, or from about 1 wt.% to about 2 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 2 wt.% to about 15 wt.%, from about 2 wt.% to about 14 wt.%, from about 2 wt.% to about 13 wt.%, from about 2 wt.% to about 12 wt.%, from about 2 wt.% to about 11 wt.%, from about 2 wt.% to about 10 wt.%, from about 2 wt.% to about 9 wt.%, from about 2 wt.% to about 8 wt.%, from about 2 wt.% to about 7 wt.%, from about 2 wt.% to about 6 wt.%, from about 2 wt.% to about 5 wt.%, from about 2 wt.% to about 4 wt.%, or from about 2 wt.% to about 3 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 3 wt.% to about 15 wt.%, from about 3 wt.% to about 14 wt.%, from about 3 wt.% to about 13 wt.%, from about 3 wt.% to about 12 wt.%, from about 3 wt.% to about 11 wt.%, from about 3 wt.% to about 10 wt.%, from about 3 wt.% to about 9 wt.%, from about 3 wt.% to about 8 wt.%, from about 3 wt.% to about 7 wt.%, from about 3 wt.% to about 6 wt.%, from about 3 wt.% to about 5 wt.%, or from about 3 wt.% to about 4 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 4 wt.% to about 15 wt.%, from about 4 wt.% to about 14 wt.%, from about 4 wt.% to about 13 wt.%, from about 4 wt.% to about 12 wt.%, from about 4 wt.% to about 11 wt.%, from about 4 wt.% to about 10 wt.%, from about 4 wt.% to about 9 wt.%, from about 4 wt.% to about 8 wt.%, from about 4 wt.% to about 7 wt.%, from about 4 wt.% to about 6 wt.%, or from about 4 wt.% to about 5 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 5 wt.% to about 15 wt.%, from about 5 wt.% to about 14 wt.%, from about 5 wt.% to about 13 wt.%, from about 5 wt.% to about 12 wt.%, from about 5 wt.% to about 11 wt.%, from about 5 wt.% to about 10 wt.%, from about 5 wt.% to about 9 wt.%, from about 5 wt.% to about 8 wt.%, from about 5 wt.% to about 7 wt.%, or from about 5 wt.% to about 6 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 6 wt.% to about 15 wt.%, from about 6 wt.% to about 14 wt.%, from about 6 wt.% to about 13 wt.%, from about 6 wt.% to about 12 wt.%, from about 6 wt.% to about 11 wt.%, from about 6 wt.% to about 10 wt.%, from about 6 wt.% to about 9 wt.%, from about 6 wt.% to about 8 wt.%, or from about 6 wt.% to about 7 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 7 wt.% to about 15 wt.%, from about 7 wt.% to about 14 wt.%, from about 7 wt.% to about 13 wt.%, from about 7 wt.% to about 12 wt.%, from about 7 wt.% to about 11 wt.%, from about 7 wt.% to about 10 wt.%, from about 7 wt.% to about 9 wt.%, or from about 7 wt.% to about 8 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 8 wt.% to about 15 wt.%, from about 8 wt.% to about 14 wt.%, from about 8 wt.% to about 13 wt.%, from about 8 wt.% to about 12 wt.%, from about 8 wt.% to about 11 wt.%, from about 8 wt.% to about 10 wt.%, or from about 8 wt.% to about 9 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 9 wt.% to about 15 wt.%, from about 9 wt.% to about 14 wt.%, from about 9 wt.% to about 13 wt.%, from about 9 wt.% to about 12 wt.%, from about 9 wt.% to about 11 wt.%, or from about 9 wt.% to about 10 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 10 wt.% to about 15 wt.%, from about 10 wt.% to about 14 wt.%, from about 10 wt.% to about 13 wt.%, from about 10 wt.% to about 12 wt.%, or from about 10 wt.% to about 11 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 11 wt.% to about 15 wt.%, from about 11 wt.% to about 14 wt.%, from about 11 wt.% to about 13 wt.%, or from about 11 wt.% to about 12 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 12 wt.% to about 15 wt.%, from about 12 wt.% to about 14 wt.%, or from about 12 wt.% to about 13 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 13 wt.% to about 15 wt.%, or from about 13 wt.% to about 14 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a fat content of from about 14 wt.% to about 15 wt.%, based on the total weight of the alkalised cocoa powder.

The alkalised cocoa powder may comprise a final mean particle size of less than 75 1.tm, and which condition is fulfilled by at least 99.5% of particles of the alkalised cocoa powder. The particle size, or fineness, may be measured according to ICA 38/1990.

According to a second aspect of the invention, there is provided a method for preparing the alkalised cocoa powder of the first aspect, the method comprising the steps: a. Adding a sample of cocoa powder to a reaction vessel; b. Adding an alkali solution to the reaction vessel; c. Adding a gas to the reaction vessel such that the pressure in the reaction vessel reaches a first pressure (P1); d. Releasing at least a portion of the gas from the reaction vessel to reduce the pressure in the reaction vessel to a second pressure (P2); e. Adding a gas to the reaction vessel such that the pressure in the reaction vessel reaches a third pressure (P3); wherein PI is greater than 3.0 Kara, P3 is greater than 2.5 Kara, and P2 is less than PI and P3.

Advantageously, the method of the second aspect of the invention comprises a combination of operating parameters which allows for the alkalisation of cocoa powder to produce an alkalised cocoa powder having favourable properties.

It is known in the art that to achieve a darker coloured alkalised cocoa powder, a greater quantity of alkali or a more strongly concentrated alkali need to be used in the alkalisation process for forming alkalised cocoa powder. Typically, relatively strong, ammonia-based alkalis are used. However, such alkalis exhibit toxic and volatile properties which are disadvantageous for the environment and for ease of operator handling in the preparation of the alkalised cocoa powder, respectively. Weaker alkalis may be preferred, such as sodium-based alkalis, for example sodium hydroxide. However, it is noted from the prior art that to achieve sufficient alkalisation of the cocoa powder to form a darker coloured alkalised cocoa powder, using a relatively weaker alkali, for example sodium hydroxide, a significant quantity of the alkali must be used.

This is also disadvantageous in terms of the cost of manufacture and the handling and processing of such large quantities of alkali. Further, using large quantities of alkali increase the difficulties in obtaining desired flavour and organoleptic profiles of the alkalised cocoa powder. Beneficially, the alkalised cocoa powder of the invention is formed without the need to use ammonia-based alkalis and without requiring significant quantities of comparatively weaker alkalis, such as sodium-based alkalis, for example sodium hydroxide. This is, at least in part, due to the two-step pressure profile of the method for preparing alkalised cocoa powder, as defined herein.

Further advantageously, the pressure profile of the method according to the second aspect of the invention provides for the alkalised cocoa powder according to the first aspect comprising a tailored colour profile and a tailored flavour profile. In particular, the alkalised cocoa powder according to the first aspect prepared according to the method of the second aspect may comprise a colour L-v al ue of from about 17.0 to about 26.0.

The alkalised cocoa powder of the invention provides for an improved sensory profile compared to alkalised cocoa powders known in the art.

Step (b) may be carried out after step (a).

Step (c) may be carried out after step (b) and/or step (a).

Step (d) may be carried out after step (c) and/or step (h) and/or step (a).

Step (e) may he carried out after step (d) and/or step (c) and/or step (b) and/or step (a).

Regarding step (b), the alkali solution may comprise an alkali agent. The alkali agent may he one or more compounds selected from the group consisting of: carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia, magnesium, sodium, calcium or potassium, for example, ammonium carbonate, magnesium carbonate, sodium carbonate, calcium carbonate and potassium carbonate, ammonium hydrogen carbonate, magnesium hydrogen carbonate, sodium hydrogen carbonate, calcium hydrogen carbonate and potassium hydrogen carbonate, ammonium sesquicarbonate, sodium sesquicarbonate, and potassium sesquicarbonate, ammonium hydroxide, magnesium hydroxide, sodium hydroxide, calcium hydroxide and potassium hydroxide, and magnesium oxide, and combinations thereof. In particular, the alkali agent may be potassium carbonate.

Advantageously, potassium carbonate is a sufficiently strong alkali to alkalise cocoa powder to obtain a desirable dark colour profile and desirable flavour profile, while avoiding the drawbacks associated with sodium-and ammonium-based alkali compounds, as described herein.

The alkali agent may not comprise any of the compounds selected from the group consisting of: carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of 20 ammonia, for example, ammonium carbonate, ammonium hydrogen carbonate, ammonium sesquicarbonate, and ammonium hydroxide.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of no more than about 10 %, about 9 %, about 8 %, about 7 %, about 6 %, about 5 %, about 4 %, about 3 %, about 2 %, or no more than about 1 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 1 % to about 10 %, from about 1 % to about 9 %, from about 1 % to about 8%, from about 1 % to about 7 %, from about 1 % to about 6 %, from about 1 % to about 5 %, from about 1 % to about 4 %, from about 1 % to about 3 %, or from about 1 % to about 2 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 2 % to about 10 %, from about 2 % to about 9 %, from about 2 % to about 8 %, from about 2 % to about 7 %, from about 2 % to about 6 %, from about 2 % to about 5 %, from about 2 % to about 4 %, or from about 2 % to about 3 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 3 % to about 10 %, from about 3 % to about 9 %, from about 3 % to about 8 %, from about 3 % to about 7 %, from about 3 % to about 6 %, from about 3 % to about 5 %, or from about 3 % to about 4 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 4 % to about 10 %, from about 4 % to about 9 %, from about 4 % to about 8 %, from about 4 % to about 7 %, from about 4 % to about 6 %, or from about 4 % to about 5 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 5 % to about 10 %, from about 5 % to about 9 %, from about 5 % to about 8 %, from about 5 % to about 7 %, or from about 5 % to about 6 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, 20 sesquicarbonate or hydroxide of ammonia in an amount of from about 6 % to about 10 %, from about 6 % to about 9 %, from about 6 % to about 8 %, or from about 6 % to about 7 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 7 % to about 10 25 %, from about 7 % to about 9 %, or from about 7 % to about 8 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 8 % to about 10 %, or from about 8 % to about 9 %.

The alkali agent may comprise a carbonate, hydrogen carbonate, sesquicarbonate or hydroxide of ammonia in an amount of from about 9 % to about 10 Thus, the alkalised cocoa powder of the invention avoids the toxicity and volatility associated with ammonia-based compounds used in preparing alkalised cocoa powders of the prior art. Avoiding the use of ammonia is beneficial for operators, the environment and handling, as it is volatile and environmentally toxic.

The preferred alkali agent for alkalising cocoa powder in accordance with the invention may depend on the specific colour and flavour of alkalised cocoa powder 10 required. For example, for more 'red-brown' colours of alkalised cocoa powder, a potassium-based alkali agent may be preferable, for example potassium carbonate.

The alkali agent may be present in the alkali solution in an amount of no more than about 7 wt.% based on the weight of the cocoa powder added to the reaction vessel in step (a). For example, the alkali agent may be present in an amount of no more than about 0.2 wt.%, about 0.4 wt.%, about 0.6 wt.%, about 0.8 wL%, about 1 wt.%, about 1.5 wt.%, about 2 wt.%, about 2.5 wt.%, about 3 wt.%, about 3.5 wt.%, about 4 wt.%, about 4.5 wt.%, about 5 wt.%, about 5.5 wt.%, about 6 wt.%, about 6.5 wt.%, or no more than about 7 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in the alkali solution in all amount of from about 0.20 wt.% to about 7.00 wt.%, from about 0.40 wt.% to about 6.75 wt.%, from about 0.60 wt.% to about 6.50 wt.%, from about 0.80 wt.% to about 6.25 wt.%, from about 1.00 wt.% to about 6.00 wt.%, from about 1.50 wt.% to about 5.75 wt.%, from about 2.00 wt.% to about 5.50 wt.%, from about 2.50 wt.% to about 5.25 wt.%, from about 3.00 wt.% to about 5.00 wt.%, from about 3.50 wt.% to about 5.00 wt.%, from about 4.00 wt.% to about 5.00 wt.%, from about 4.50 wt.% to about 5.00 wt.%, or about 4.75 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of about 0.2 wt.%, about 0.4 wt.%, about 0.6 wt.%, about 0.8 wt.%, about 1 wt.%. about 1.5 wt.%, about 2 wt.%, about 2.5 wt.%, about 3 wt.%, about 3.5 wt.%, about 4 wt.%, about 4.5 wt.%, about 5 wt.%, about 5.5 wt.%, about 6 wt.%, about 6.5 wt.%, or about 7 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 0.20 wt.% to about 7.00 wt.% from about 0.20 wt.% to about 6.50 wt.%, from about 0.20 wt.% to about 6.00 wt.%, from about 0.20 wt.% to about 5.50 wt.%, from about 0.20 wt.% to about 5.00 wt.% from about 0.20 wt.% to about 4.50 wt.%, from about 0.20 wt.% to about 4.00 wt.%, from about 0.20 wt.% to about 3.50 wt.%, from about 0.20 wt.% to about 3.00 wt.%, from about 0.20 wt.% to about 2.50 wt.%, from about 0.20 wt.% to about 2.00 wt.%, from about 0.20 wt.% to about 1.50 wt.%, from about 0.20 wt.% to about 1.00 wt.%, from about 0.20 wt.% to about 0.80 wt.%, from about 0.20 wt.% to about 0.60 wt.%, or from about 0.20 wt.% to about 0.40 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 0.40 wt.% to about 7.00 wt.%, from about 0.40 wt.% to about 6.50 wt.%, from about 0.40 wt.% to about 6.00 wt.%, from about 0.40 wt.% to about 5.50 wt.%, from about 0.40 wt.% to about 5.00 wt.%, from about 0.40 wt.% to about 4.50 wt.%, from about 0.40 wt.% to about 4.00 wt.%, from about 0.40 wt.% to about 3.50 wt.%, from about 0.40 wt.% to about 3.00 wt.%, from about 0.40 wt.% to about 2.50 wt.%, from about 0.40 wt.% to about 2.00 wt.%, from about 0.40 wt.% to about 1.50 wt.%, from about 0.40 wt.% to about 1.00 wt.%, from about 0.40 wt.% to about 0.80 wt.%, or from about 0.40 wt.% to about 0.60 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 0.60 wt.% to about 7.00 wt.%, from about 0.60 wt.% to about 6.50 wt.%, from about 0.60 wt.% to about 6.00 wt.%, from about 0.60 wt.% to about 5.50 wt.%, from about 0.60 wt.% to about 5.00 wt.%, from about 0.60 wt.% to about 4.50 wt.%, from about 0.60 wt.% to about 4.00 wt.%, from about 0.60 wt.% to about 3.50 wt.%, from about 0.60 wt.% to about 3.00 wt.%, from about 0.60 wt.% to about 2.50 wt.%, from about 0.60 wt.% to about 2.00 wt.%, from about 0.60 wt.% to about 1.50 wt.%, from about 0.60 wt.% to about 1.00 wt.%, or from about 0.60 wt.% to about 0.80 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may he present in an amount of from about 0.80 wt.% to about 7.00 wt.%, from about 0.80 wt.% to about 6.50 wt.%, from about 0.80 wt.% to about 6.00 wt.%, from about 0.80 wt.% to about 5.50 wt.%, from about 0.80 wt.% to about 5.00 wt.%, from about 0.80 wt.% to about 4.50 wt.%, from about 0.80 wt.% to about 4.00 wt.%, from about 0.80 wt.% to about 3.50 wt.%, from about 0.80 wt.% to about 3.00 wt.%, from about 0.80 wt.% to about 2.50 wt.%, from about 0.80 wt.% to about 2.00 wt.%, from about 0.80 wt.% to about 1.50 wt.%, or from about 0.80 wt.% to about 1.00 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 1.00 wt.% to about 7.00 wt.%, from about 1.00 wt.% to about 6.50 wt.%, from about 1.00 wt.% to about 6.00 wt.%, from about 1.00 wt.% to about 5.50 wt.%, from about 1.00 wt.% to about 5.00 wt.%, from about 1.00 wt.% to about 4.50 wt.%, from about 1.00 wt.% to about 4.00 wt.%, from about 1.00 wt.% to about 3.50 wt.%, from about 1.00 wt.% to about 3.00 wt.%, from about 1.00 wt.% to about 2.50 wt.%, from about 1.00 wt.% to about 2.00 wt.%, or from about 1.00 wt.% to about 1.50 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 1.50 wt.% to about 7.00 wt.%, from about 1.50 wt.% to about 6.50 wt.%, from about 1.50 wt.% to about 6.00 wt.%, from about 1.50 wt.% to about 5.50 wt.%, from about 1.50 wt.% to about 5.00 wt.%, from about 1.50 wt.% to about 4.50 wt.%, from about 1.50 wt.% to about 4.00 wt.%, from about 1.50 wt.% to about 3.50 wt.%, from about 1.50 wt.% to about 3.00 wt.%, from about 1.50 wt.% to about 2.50 wt.%, or from about 1.50 wt.% to about 2.00 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 2.00 wt.% to about 7.00 wt.%, from about 2.00 wt.% to about 6.50 wt.%, from about 2.00 wt.% to about 6.00 wt.%, from about 2.00 wt.% to about 5.50 wt.%, from about 2.00 wt.% to about 5.00 wt.%, from about 2.00 wt.% to about 4.50 wt.%, from about 2.00 wt.% to about 4.00 wt.%, from about 2.00 wt.% to about 3.50 wt.%, from about 2.00 wt.% to about 3.00 wt.%, or from about 2.00 wt.% to about 2.50 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 2.50 wt.% to about 7.00 wt.% from about 2.50 wt.% to about 6.50 wt.%, from about 2.50 wt.% to about 6.00 wt.%, from about 2.50 wt.% to about 5.50 wt.%, from about 2.50 wt.% to about 5.00 wt.% from about 2.50 wt.% to about 4.50 wt.%, from about 2.50 wt.% to about 4.00 wt.%, from about 2.50 wt.% to about 3.50 wt.%, or from about 2.50 wt.% to about 3.00 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 3.00 wt.% to about 7.00 wt.%, from about 3.00 wt.% to about 6.50 wt.%, from about 3.00 wt.% to about 6.00 wt.%, from about 3.00 wt.% to about 5.50 wt.%, from about 3.00 wt.% to about 5.00 wt.%, from about 3.00 wt.% to about 4.50 wt.%, from about 3.00 wt.% to about 4.00 wt.%, or from about 3.00 wt.% to about 3.50 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may he present in an amount of from about 3.50 wt.% to about 7.00 wt.%, from about 3.50 wt.% to about 6.50 wt.%, from about 3.50 wt.% to about 6.00 wt.%, from about 3.50 wt.% to about 5.50 wt.%, from about 3.50 wt.% to about 5.00 wt.%, from about 3.50 wt.% to about 4.50 wt.%, or from about 3.50 wt.% to about 4.00 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 4.00 wt.% to about 7.00 wt.%, from about 4.00 wt.% to about 6.50 wt.%, from about 4.00 wt.% to about 6.00 wt.%, from about 4.00 wt.% to about 5.50 wt.%, from about 4.00 wt.% to about 5.00 wt.%, or from about 4.00 wt.% to about 4.50 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 4.50 wt.% to about 7.00 wt.%, from about 4.50 wt.% to about 6.50 wt.%, from about 4.50 wt.% to about 6.00 wt.%, from about 4.50 wt.% to about 5.50 wt.%, or from about 4.50 wt.% to about 5.00 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 5.00 wt.% to about 7.00 wt.%, from about 5.00 wt.% to about 6.50 wt.%, from about 5.00 wt.% to about 6.00 wt.%, or from about 5.00 wt.% to about 5.50 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 5.50 wt.% to about 7.00 wt.%, from about 5.50 wt.% to about 6.50 wt.%, or from about 5.50 wt.% to about 6.00 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 6.00 wt.% to about 7.00 wt.%, or from about 6.00 wt.% to about 6.50 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

The alkali agent may be present in an amount of from about 6.50 wt.% to about 7.00 wt.%, based on the weight of the cocoa powder added to the reaction vessel in step (a).

Regarding step (c), the gas in the reaction vessel may be an oxygen-containing gas, including mixtures of oxygen and nitrogen. Advantageously, the oxygen-containing gas facilitates the alkalisation reaction.

The unit of pressure provided herein are values of absolute pressure, also referred to in the art as 'bar absolute', bar(a)' or 'ban'.

The first pressure (P1) may he any pressure greater than 3.0 bara. The first pressure (P1) may he at least about 3.0 bara, about 3.5 bara, about 4.0 bara, about 4.5 bara, about 5.0 bara, about 5.5 bara, about 6.0 bara, about 6.5 bara, about 7.0 bara, about 7.5 bara, about 8.0 bara, about 8.5 bara, about 9.0 bara, about 9.5 bara, or at least about 10.0 bara.

The first pressure may be about 3.5 bara, about 4.0 bara, about 4.5 bara, about 5.0 bara, about 5.5 bara, about 6.0 bara, about 6.5 bara, about 7.0 bara, about 7.5 bara, about 8.0 bara, about 8.5 bara, about 9.0 bara, about 9.5 bara, or about 10.0 ban.

The first pressure (P1) may he no more than about 3.0 bara, about 3.5 bara, about 4.0 bara, about 4.5 bara, about 5.0 bara, about 5.5 bara, about 6.0 bara, about 6.5 bara, about 7.0 bara, about 7.5 bara, about 8.0 bara, about 8.5 bara, about 9.0 tiara, about 9.5 bara, or no more than about 10.0 bara.

The first pressure (P1) may be from about 3.0 bara to about 9.0 bara, from about 3.5 bara to about 8.5 bara, from about 4.0 bara to about 8.0 bara, from about 4.5 bara to about 7.5 bara, from about 5.0 bara to about 7.0 bara, from about 5.5 bara to about 6.5 bara, or about 6.0 bara.

The first pressure (P1) may be from about 3.0 bara to about 10.0 bara, from about 3.0 bara to about 9.5 bara, from about 3.0 bara to about 9.0 ban, from about 3.0 bara to about 8.5 bara, from about 3.0 bara to about 8.0 bara, from about 3.0 bara to about 7.5 bara, from about 3.0 bara to about 7.0 bara, from about 3.0 bara to about 6.5 bara, from about 3.0 bara to about 6.0 bara, from about 3.0 hara to about 5.5 bara, from about 3.0 bara to about 5.0 bara, from about 3.0 bara to about 4.5 hara, from about 3.0 bara to about 4.0 bara, or from about 3.0 bara to about 3.5 bara.

The first pressure (P1) may be from about 3.5 bara to about 10.0 bara, from about 3.5 bara to about 9.5 bara, from about 3.5 bara to about 9.0 tiara, from about 3.5 bara to about 8.5 bara, from about 3.5 bara to about 8.0 bara, from about 3.5 bara to about 7.5 bara, from about 3.5 bara to about 7.0 bara, from about 3.5 bara to about 6.5 bara, from about 3.5 bara to about 6.0 bara, from about 3.5 bara to about 5.5 bara, from about 3.5 bara to about 5.0 bara, from about 3.5 bara to about 4.5 bara, or from about 3.5 bara to about 4.0 bara.

The first pressure (P1) may be from about 4.0 bara to about 10.0 bara, from about 4.0 bara to about 9.5 bara, from about 4.0 bara to about 9.0 ban, from about 4.0 bara to about 8.5 bara, from about 4.0 hara to about 8.0 bara, from about 4.0 hara to about 7.5 bara, from about 4.0 bara to about 7.0 bara, from about 4.0 bara to about 6.5 bara, from about 4.0 bara to about 6.0 bara, from about 4.0 bara to about 5.5 bara, from about 4.0 bara to about 5.0 bara, or from about 4.0 bara to about 4.5 bara.

The first pressure (P1) may be from about 4.5 bara to about 10.0 ham, from about 4.5 bara to about 9.5 bara, from about 4.5 bara to about 9.0 Nu-a, from about 4.5 Kara to about 8.5 bara, from about 4.5 bara to about 8.0 bara, from about 4.5 bara to about 7.5 bara, from about 4.5 bara to about 7.0 bara, from about 4.5 bara to about 6.5 bara, from about 4.5 bara to about 6.0 butt, from about 4.5 bara to about 5.5 btu-a, or from about 4.5 bara to about 5.0 bara.

The first pressure (P1) may be from about 5.0 bara to about 10.0 bara, from about 5.0 bara to about 9.5 bara, from about 5.0 bara to about 9.0 bara, from about 5.0 bara to about 8.5 bara, from about 5.0 bara to about 8.0 bara, from about 5.0 bara to about 7.5 bara, from about 5.0 bara to about 7.0 bara, from about 5.0 bara to about 6.5 bara, from about 5.0 bara to about 6.0 bara, or from about 5.0 bara to about 5.5 bara.

The first pressure (P1) may be from about 5.5 bara to about 10.0 bara, from about 5.5 bara to about 9.5 bara, from about 5.5 bara to about 9.0 bara, from about 5.5 bara to about 8.5 bara, from about 5.5 btu-a to about 8.0 bara, from about 5.5 bara to about 7.5 bara, from about 5.5 bara to about 7.0 bara, from about 5.5 bara to about 6.5 bara, or from about 5.5 ham to about 6.0 bara.

The first pressure (P1) may be from about 6.0 bara to about 10.0 bara, from about 6.0 bara to about 9.5 bara, from about 6.0 bara to about 9.0 bara, from about 6.0 bara to about 8.5 bara, from about 6.0 btu-a to about 8.0 bara, from about 6.0 bara to about 7.5 bara, from about 6.0 bara to about 7.0 bara, or from about 6.0 bara to about 6.5 bara.

The first pressure (P1) may be from about 6.5 bara to about 10.0 bara, from about 6.5 bara to about 9.5 bara, from about 6.5 bara to about 9.0 bara, from about 6.5 bara to about 8.5 bara, from about 6.5 bara to about 8.0 bara, from about 6.5 bara to about 7.5 bara, or from about 6.5 bara to about 7.0 bara.

The first pressure (P1) may be from about 7.0 bara to about 10.0 bara, from about 7.0 bara to about 9.5 bara, from about 7.0 bara to about 9.0 ban, from about 7.0 bara to about 8.5 bara, from about 7.0 bara to about 8.0 btu-a, or from about 7.0 btu-a to about 7.5 bara.

The first pressure (P1) may be from about 7.5 bara to about 10.0 bara, from about 7.5 bara to about 9.5 bara, from about 7.5 bara to about 9.0 bara, from about 7.5 bara to about 8.5 bara, or from about 7.5 bara to about 8.0 bara.

The first pressure (P1) may be from about 8.0 bara to about 10.0 bara, from about 8.0 ban to about 9.5 bara, from about 8.0 ban to about 9.0 bara, or from about 8.0 bara to about 8.5 ban.

The first pressure (P1) may be from about 8.5 bara to about 10.0 bara, from about 8.5 bara to about 9.5 ban, or from about 8.5 bara to about 9.0 bara.

The first pressure (P1) may be from about 9.0 bara to about 10.0 bara, or from about 9.0 bara to about 9.5 ban.

The first pressure (P1) may be from about 9.5 bara to about 10.0 ham.

The method may comprise increasing the pressure in the reaction vessel from approximately atmospheric pressure to the first pressure (P1) over the course of from about 8 minutes to about 28 minutes, from about 10 minutes to about 26 minutes, from about 12 minutes to about 24 minutes, from about 14 minutes to about 22 minutes, from about 16 minutes to about 20 minutes, or about 18 minutes.

The method may comprise increasing the pressure in the reaction vessel from approximately atmospheric pressure to the first pressure (P1) over the course of about 8 minutes, 9 minutes, about 10 minutes, about 1 1 minutes, about 12 minutes, about 13 minutes, about 14 minutes, about 15 minutes, about 16 minutes, about 17 minutes, about 18 minutes, about 19 minutes, about 20 minutes, about 21 minutes, about 22 minutes, about 23 minutes, about 24 minutes, about 25 minutes, about 26 minutes, about 27 minutes, about 28 minutes, about 29 minutes, or about 30 minutes.

The method may comprise increasing the pressure in the reaction vessel from approximately atmospheric pressure to the first pressure (P1) over the course of at least about 8 minutes, 9 minutes, about 10 minutes, about 11 minutes, about 12 minutes, about 13 minutes, about 14 minutes, about 15 minutes, about 16 minutes, about 17 minutes, about 18 minutes, about 19 minutes, about 20 minutes, about 21 minutes, about 22 minutes, about 23 minutes, about 24 minutes, about 25 minutes, about 26 minutes, about 27 minutes, about 28 minutes, about 29 minutes, or at least about 30 minutes.

The method may comprise increasing the pressure in the reaction vessel from approximately atmospheric pressure to the first pressure (P1) over the course of no more than about 8 minutes, 9 minutes, about 10 minutes, about 11 minutes, about 12 minutes, about 13 minutes, about 14 minutes, about 15 minutes, about 16 minutes, about 17 minutes, about 18 minutes, about 19 minutes, about 20 minutes, about 21 minutes, about 22 minutes, about 23 minutes, about 24 minutes, about 25 minutes, about 26 minutes, about 27 minutes, about 28 minutes, about 29 minutes, or no more than about minutes.

The first pressure may be held for a first time period (T1).

The first time period (T1) may be from about 1 minute to about 60 minutes, from about 5 minutes to about 60 minutes, from about 10 minutes to about 55 minutes, from about 15 minutes to about 50 minutes, from about 20 minutes to about 45 minutes, from about 25 minutes to about 40 minutes, from about 25 minutes to about 35 minutes, from about 27 minutes to about 33 minutes, or about 30 minutes.

The first time period (T1) may be from about 1 minute to about 60 minutes, from about 1 minute to about 55 minutes, from about 1 minute to about 50 minutes, from about 1 minute to about 45 minutes, from about 1 minute to about 40 minutes, from about 1 minute to about 35 minutes, from about 1 minute to about 30 minutes, from about 1 minute to about 25 minutes, from about 1 minute to about 20 minutes, from about 1 minute to about 15 minutes, from about 1 minute to about 10 minutes, or from about 1 minute to about 5 minutes.

The first time period (T1) may be from about 5 minutes to about 60 minutes, from about 5 minutes to about 55 minutes, from about 5 minutes to about 50 minutes, from about 5 minutes to about 45 minutes, from about 5 minutes to about 40 minutes, from about 5 minutes to about 35 minutes, from about 5 minutes to about 30 minutes, from about 5 minutes to about 25 minutes, from about 5 minutes to about 20 minutes, from about 5 minutes to about 15 minutes, or from about 5 minutes to about 10 minutes.

The first time period (T1) may be from about 10 minutes to about 60 minutes, from about 10 minutes to about 55 minutes, from about 10 minutes to about 50 minutes, from about 10 minutes to about 45 minutes, from about 10 minutes to about 40 minutes, from about 10 minutes to about 35 minutes, from about 10 minutes to about 30 minutes, from about 10 minutes to about 25 minutes, from about 10 minutes to about 20 minutes, or from about 10 minutes to about 15 minutes.

The first time period (T1) may be from about 15 minutes to about. 60 minutes, from about 15 minutes to about 55 minutes, from about 15 minutes to about 50 minutes, from about 15 minutes to about 45 minutes, from about 15 minutes to about 40 minutes, from about 15 minutes to about 35 minutes, from about 15 minutes to about 30 minutes, from about 15 minutes to about 25 minutes, or from about 15 minutes to about 20 minutes.

The first time period (T1) may be from about 20 minutes to about 60 minutes, from about 20 minutes to about 55 minutes, from about 20 minutes to about 50 minutes, from about 20 minutes to about 45 minutes, from about 20 minutes to about 40 minutes, from about 20 minutes to about 35 minutes, from about 20 minutes to about 30 minutes, or from about 20 minutes to about 25 minutes.

The first time period (T1) may be from about 25 minutes to about 60 minutes, from about 25 minutes to about 55 minutes, from about 25 minutes to about 50 minutes, from about 25 minutes to about 45 minutes, from about 25 minutes to about 40 minutes, from about 25 minutes to about 35 minutes, or from about 25 minutes to about 30 minutes.

The first time period (T1) may be from about 30 minutes to about 60 minutes, 20 from about 30 minutes to about 55 minutes, from about 30 minutes to about 50 minutes, from about 30 minutes to about 45 minutes, from about 30 minutes to about 40 minutes, or from about 30 minutes to about 35 minutes.

The first time period (T1) may be from about 35 minutes to about 60 minutes, from about 35 minutes to about 55 minutes, from about 35 minutes to about 50 minutes, 25 from about 35 minutes to about 45 minutes, or from about 35 minutes to about 40 minutes.

The first time period (T1) may he from about 40 minutes to about 60 minutes, from about 40 minutes to about 55 minutes, from 40 minutes to about 50 minutes, or from about 40 minutes to about 45 minutes.

The first time period (T1) may be from about 45 minutes to about 60 minutes, from about 45 minutes to about 55 minutes, or from 45 minutes to about 50 minutes.

The first time period (Ti) may be from about 50 minutes to about 60 minutes, or from about 50 minutes to about 55 minutes.

The first time period (T1) may he from about 55 minutes to about 60 minutes.

The first time period (Ti) may be about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or about 60 minutes.

The first time period (T1) may be at least about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or at least about 60 minutes.

The first time period (T1) may be no more than about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or no more than about 60 minutes.

It will be understood by those skilled in the art that to hold a pressure for a specific time period should be interpreted with appreciation that the pressure may fluctuate from the target pressure. For example, in embodiments of the invention where the first pressure (P1) is about 6 bara and this is held for a first time period (T1) of 30 minutes, it should be understood that this does not necessarily mean that the pressure for the entirety of the first time period is exactly 6 ban. There will be, as is understood in the art, minor fluctuations in the pressure during the first time period. For example, to hold the first pressure at 6 ban for a first time period of 30 minutes may mean that the pressure is held within a pressure range of, for example, from 5.90 bara to 6.10 barn, or 5.85 bara to 6.05 bara, for the 30 minute period, possibly depending on instrument variation.

The third pressure (P3) may be any pressure greater than 2.5 bara.

The third pressure may he at least about 2.5 bara, about 3.0 bara, about 3.5 bara, about 4.0 btu-a, about 4.5 bara, about 5.0 bara, about 5.5 bara, about 6.0 btu-a, about 6.5 bara, about 7.0 btu-a, about 7.5 butt, about 8.0 ban, about 8.5 butt, about 9.0 bara, about 9.5 bara, or at least about 10.0 bara.

The third pressure may be about 2.5 bara, about 3.0 bunt, about 3.5 butt, about 4.0 bara, about 4.5 bara, about 5.0 bara, about 5.5 bara, about 6.0 ham, about 6.5 bara, about 7.0 hara, about 7.5 hara, about 8.0 bara about 8.5 hara, about 9.0 ham, about 9.5 bara, or about 10.0 bara.

The third pressure may be no more than about 2.5 ham, about 3.0 ham, about 3.5 bara, about 4.0 bara, about 4.5 bara, about 5.0 bara, about 5.5 bara, about 6.0 ban, about 6.5 bara, about 7.0 bara, about 7.5 bara, about 8.0 bara, about 8.5 bara, about 9.0 bara, about 9.5 bara, or no more than about 10.0 bara.

The third pressure (P3) may be from about 2.50 bara to about 7.0 bara, from about 2.55 bara to about 6.5 btu-a, from about 2.60 btu-a to about 6.0 bara, from about 2.65 bara to about 5.5 bara, from about 2.70 bara to about 5.0 bara, from about 2.75 hara to about 4.5 bara, from about 2.80 hara to about 4.0 ham, from about 2.85 hara to about 3.75 bara, from about 2.90 btu-a to about 3.50 btu-a, from about 2.95 bara to about 3.25 bara, or about 3.0 bara.

The third pressure (P3) may be from about 2.5 hara to about 10.0 hara, from about 2.5 bara to about 9.5 btu-a, from about 2.5 bara to about 9.0 bran, from about 2.5 bara to about 8.5 bara, from about 2.5 bara to about 8.0 bara, from about 2.5 ban to about 7.5 bara, from about 2.5 hara to about 7.0 hara, from about 2.5 hara to about 6.5 hara, from about 2.5 hara to about 6.0 hara, from about 2.5 hara to about 5.5 bara, from about 2.5 bara to about 5.0 bara, from about 2.5 bara to about 4.5 ban, from about 2.5 hara to about 4.0 hara, or from about 2.5 bara to about 3.5 hara.

The third pressure (P3) may be from about 3.0 bara to about 10.0 bara, from about 3.0 bara to about 9.5 ban, from about 3.0 bara to about 9.0 btu-a, from about 3.0 hara to about 8.5 hara, from about 3.0 hara to about 8.0 bara, from about 3.0 hara to about 7.5 bara, from about 3.0 hara to about 7.0 hara, from about 3.0 ham to about 6.5 bara, from about 3.0 bara to about 6.0 ban, from about 3.0 btu-a to about 5.5 bara, from about 3.0 bara to about 5.0 bara, from about 3.0 bara to about 4.5 bara, from about 3.0 bara to about 4.0 btu-a, or from about 3.0 bara to about 3.5 bara.

The third pressure (P3) may be from about 3.5 bara to about 10.0 bara, from about 3.5 bara to about 9.5 bara, from about 3.5 bara to about 9.0 bara, from about 3.5 bara to about 8.5 bara, from about 3.5 bara to about 8.0 btu-a, from about 3.5 bara to about 7.5 bara, from about 3.5 bara to about 7.0 bara, from about 3.5 bara to about 6.5 bara, from about 3.5 bara to about 6.0 bara, from about 3.5 bara to about 5.5 bara, from about 3.5 bara to about 5.0 bara, from about 3.5 bara to about 4.5 bara, or from about 3.5 bara to about 4.0 btu-a.

The third pressure (P3) may be from about 4.0 bara to about 10.0 bara, from about 4.0 bara to about 9.5 bara, from about 4.0 bara to about 9.0 bara, from about 4.0 bara to about 8.5 bara, from about 4.0 bara to about 8.0 bara, from about 4.0 bara to about 7.5 bara, from about 4.0 bara to about 7.0 bara, from about 4.0 bara to about 6.5 bara, from about 4.0 bara to about 6.0 bara, from about 4.0 bara to about 5.5 bara, from about 4.0 bara to about 5.0 bara, or from about 4.0 bara to about 4.5 bara.

The third pressure (P3) may be from about 4.5 bara to about 10.0 bara, from about 4.5 bara to about 9.5 btu-a, from about 4.5 bara to about 9.0 btu-a, from about 4.5 bara to about 8.5 bara, from about 4.5 bara to about 8.0 bara, from about 4.5 bara to about 7.5 bara, from about 4.5 bara to about 7.0 bara, from about 4.5 bara to about 6.5 bara, from about 4.5 bara to about 6.0 bara, from about 4.5 bara to about 5.5 bara, or from about 4.5 bara to about 5.0 bara.

The third pressure (P3) may he from about 5.0 bara to about 10.0 bara, from about 5.0 bara to about 9.5 bara, from about 5.0 bara to about 9.0 bara, from about 5.0 bara to about 8.5 bara, from about 5.0 bara to about 8.0 bara, from about 5.0 bara to about 7.5 bara, from about 5.0 bara to about 7.0 bara, from about 5.0 bara to about 6.5 bara, from about 5.0 bara to about 6.0 bara, or from about 5.0 bara to about 5.5 bara.

The third pressure (P3) may be from about 5.5 btu-a to about 10.0 btu-a, from about 5.5 bara to about 9.5 bara, from about 5.5 bara to about 9.0 bara, from about 5.5 bara to about 8.5 bara, from about 5.5 bara to about 8.0 bara, from about 5.5 bara to about 7.5 bara, from about 5.5 bara to about 7.0 bara, from about 5.5 bara to about 6.5 bara, or from about 5.5 bara to about 6.0 bara.

The third pressure (P3) may be from about 6.0 bara to about 10.0 bara, from about 6.0 bara to about 9.5 bara, from about 6.0 bara to about 9.0 bara, from about 6.0 bara to about 8.5 bara, from about 6.0 bara to about 8.0 ban, from about 6.0 tiara to about 7.5 bara from about 6.0 bara to about 7.0 bara, or from about 6.0 bara to about 6.5 bara.

The third pressure (P3) may be from about 6.5 bara to about 10.0 bara, from about 6.5 bara to about 9.5 bara, from about 6.5 bara to about 9.0 bara, from about 6.5 bara to about 8.5 bara, from about 6.5 bara to about 8.0 bara, from about 6.5 bara to about 7.5 bara, or from about 6.5 bara to about 7.0 bara.

The third pressure (P3) may be from about 7.0 bara to about 10.0 bara, from about 7.0 bara to about 9.5 bara, from about 7.0 bara to about 9.0 bara, from about 7.0 bara to about 8.5 bara, from about 7.0 bara to about 8.0 Nu-a, or from about 7.0 Nu-a to about 7.5 bara.

The third pressure (P3) may be from about 7.5 bara to about 10.0 bara, from about 7.5 bara to about 9.5 bara, from about 7.5 bara to about 9.0 bara, from about 7.5 bara to about 8.5 bara, or from about 7.5 bara to about 8.0 bara.

The third pressure (P3) may be from about 8.0 bara to about 10.0 bara, from about 8.0 bara to about 9.5 bara, from about 8.0 bara to about 9.0 bara, or from about 8.0 bara to about 8.5 bara.

The third pressure (P3) may be from about 8.5 bara to about 10.0 bara, from about 8.5 bara to about 9.5 bara, or from about 8.5 bara to about 9.0 bara.

The third pressure (P3) may be from about 9.0 bara to about 10.0 bara, or from about 9.0 bara to about 9.5 bara.

The third pressure (P3) may be from about 9.5 bara to about 10.0 bara. The third pressure (P3) may be held for a third time period (T3).

The third time period (T3) may be from about 5 minutes to about 120 minutes, from about 10 minutes to about 115 minutes, from about 15 minutes to about 110 minutes, from about 20 minutes to about 105 minutes, from about 25 minutes to about 100 minutes, from about 30 minutes to about 95 minutes, from about 35 minutes to about 90 minutes, from about 40 minutes to about 85 minutes, from about 45 minutes to about 80 minutes, from about 50 minutes to about 75 minutes, from about 50 minutes to about 70 minutes, from about 55 minutes to about 65 minutes, from about 58 minutes to about 62 minutes, or about 60 minutes.

The third time period (T3) may be from about 5 minutes to about 120 minutes, from about 5 minutes to about 115 minutes, from about 5 minutes to about 110 minutes, from about 5 minutes to about 105 minutes, from about 5 minutes to about 100 minutes, from about 5 minutes to about 95 minutes, from about 5 minutes to about 90 minutes, from about 5 minutes to about 85 minutes, from about 5 minutes to about 80 minutes, from about 5 minutes to about 75 minutes, from about 5 minutes to about 70 minutes, from about 5 minutes to about 65 minutes, from about 5 minutes to about 60 minutes, from about 5 minutes to about 55 minutes, from about 5 minutes to about 50 minutes, from about 5 minutes to about 45 minutes, from about 5 minutes to about 40 minutes, from about 5 minutes to about 35 minutes, from about 5 minutes to about 30 minutes, from about 5 minutes to about 25 minutes, from about 5 minutes to about 20 minutes, from about 5 minutes to about 15 minutes, or from about 5 minutes to about 10 minutes.

The third time period (T3) may be from about 10 minutes to about 120 minutes, from about 10 minutes to about 115 minutes, from about 10 minutes to about 110 minutes, from about 10 minutes to about 105 minutes, from about 10 minutes to about 100 minutes, from about 10 minutes to about 95 minutes, from about 10 minutes to about 90 minutes, from about 10 minutes to about 85 minutes, from about 10 minutes to about 80 minutes, from about 10 minutes to about 75 minutes, from about 10 minutes to about 70 minutes, from about 10 minutes to about 65 minutes, from about 10 minutes to about 60 minutes, from about 10 minutes to about 55 minutes, from about 10 minutes to about 50 minutes, from about 10 minutes to about 45 minutes, from about 10 minutes to about 40 minutes, from about 10 minutes to about 35 minutes, from about 10 minutes to about 30 minutes, from about 10 minutes to about 25 minutes, from about 10 minutes to about 20 minutes, or from about 10 minutes to about 15 minutes.

The third time period (T3) may be from about 15 minutes to about 120 minutes, from about 15 minutes to about 115 minutes, from about 15 minutes to about 110 minutes, from about 15 minutes to about 105 minutes, from about 15 minutes to about 100 minutes, from about 15 minutes to about 95 minutes, from about 15 minutes to about 90 minutes, from about 15 minutes to about 85 minutes, from about 15 minutes to about 80 minutes, from about 15 minutes to about 75 minutes, from about 15 minutes to about 70 minutes, from about 15 minutes to about 65 minutes, from about 15 minutes to about 60 minutes, from about 15 minutes to about 55 minutes, from about 15 minutes to about 50 minutes, from about 15 minutes to about 45 minutes, from about 15 minutes to about 40 minutes, from about 15 minutes to about 35 minutes, from about 15 minutes to about 30 minutes, from about 15 minutes to about 25 minutes, or from about 15 minutes to about 20 minutes.

The third time period (T3) may be from about 20 minutes to about 120 minutes, from about 20 minutes to about 115 minutes, from about 20 minutes to about 110 minutes, from about 20 minutes to about 105 minutes, from about 20 minutes to about minutes, from about 20 minutes to about 95 minutes, from about 20 minutes to about 90 minutes, from about 20 minutes to about 85 minutes, from about 20 minutes to about 80 minutes, from about 20 minutes to about 75 minutes, from about 20 minutes to about 70 minutes, from about 20 minutes to about 65 minutes, from about 20 minutes to about 60 minutes, from about 20 minutes to about 55 minutes, from about 20 minutes to about 50 minutes, from about 20 minutes to about 45 minutes, from about 20 minutes to about 40 minutes, from about 20 minutes to about 35 minutes, from about 20 minutes to about 30 minutes, or from about 20 minutes to about 25 minutes.

The third time period (T3) may be from about 25 minutes to about 120 minutes, from about 25 minutes to about 115 minutes, from about 25 minutes to about 110 minutes, from about 25 minutes to about 105 minutes, from about 25 minutes to about 100 minutes, from about 25 minutes to about 95 minutes, from about 25 minutes to about 90 minutes, from about 25 minutes to about 85 minutes, from about 25 minutes to about 80 minutes, from about 25 minutes to about 75 minutes, from about 25 minutes to about 70 minutes, from about 25 minutes to about 65 minutes, from about 25 minutes to about 60 minutes, from about 25 minutes to about 55 minutes, from about 25 minutes to about 50 minutcs, from about 25 minutes to about 45 minutes, from about 25 minutes to about 40 minutes, from about 25 minutes to about 35 minutes, or from about 25 minutes to about 30 minutes.

The third time period (T3) may he from about 30 minutes to about 120 minutes, from about 30 minutes to about 115 minutes, from about 30 minutes to about 110 minutes, from about 30 minutes to about 105 minutes, from about 30 minutes to about 100 minutes, from about 30 minutes to about 95 minutes, from about 30 minutes to about 90 minutes, from about 30 minutes to about 85 minutes, from about 30 minutes to about 80 minutes, from about 30 minutes to about 75 minutes, from about 30 minutes to about 70 minutes, from about 30 minutes to about 65 minutes, from about 30 minutes to about 60 minutes, from about 30 minutes to about 55 minutes, from about 30 minutes to about 50 minutes, from about 30 minutes to about 45 minutes, from about 30 minutes to about 40 minutes, or from about 30 minutes to about 35 minutes.

The third time period (T3) may he from about 35 minutes to about 120 minutes, S from about 35 minutes to about 115 minutes, from about 35 minutes to about 110 minutes, from about 35 minutes to about 105 minutes, from about 35 minutes to about 100 minutes, from about 35 minutes to about 95 minutes, from about 35 minutes to about 90 minutes, from about 35 minutes to about 85 minutes, from about 35 minutes to about 80 minutes, from about 35 minutes to about 75 minutes, from about 35 minutes to about 70 minutes, from about 35 minutes to about 65 minutes, from about 35 minutes to about 60 minutes, from about 35 minutes to about 55 minutes, from about 35 minutes to about 50 minutes, from about 35 minutes to about 45 minutes, or from about 35 minutes to about 40 minutes.

The third time period (T3) may he from about 40 minutes to about 120 minutes, from about 40 minutes to about 115 minutcs, from about 40 minutes to about 110 minutes, from about 40 minutes to about 105 minutes, from about 40 minutes to about 100 minutes, from about 40 minutes to about 95 minutes, from about 40 minutes to about 90 minutes, from about 40 minutes to about 85 minutes, from about 40 minutes to about 80 minutes, from about 40 minutes to about 75 minutes, from about 40 minutes to about 70 minutes, from about 40 minutes to about 65 minutes, from about 40 minutes to about 60 minutes, from about 40 minutes to about 55 minutes, from about 40 minutes to about 50 minutes, or from about 40 minutes to about 45 minutes.

The third time period (T3) may be from about 45 minutes to about 120 minutes, from about 45 minutes to about 115 minutes, from about 45 minutes to about 110 minutes, from about 45 minutes to about 105 minutes, from about 45 minutes to about minutes, from about 45 minutes to about 95 minutes, from about 45 minutes to about 90 minutes, from about 45 minutes to about 85 minutes, from about 45 minutes to about 80 minutes, from about 45 minutes to about 75 minutes, from about 45 minutes to about 70 minutes, from about 45 minutes to about 65 minutes, from about 45 minutes to about 60 minutes, from about 45 minutes to about 55 minutes, or from about 45 minutes to about 50 minutes.

The third time period (T3) may be from about 50 minutes to about 120 minutes, from about 50 minutes to about 115 minutes, from about 50 minutes to about 110 minutes, from about 50 minutes to about 105 minutes, from about 50 minutes to about 100 minutes, from about 50 minutes to about 95 minutes, from about 50 minutes to about 90 minutes, from about 50 minutes to about 85 minutes, from about 50 minutes to about 80 minutes, from about 50 minutes to about 75 minutes, from about 50 minutes to about 70 minutes, from about 50 minutes to about 65 minutes, from about 50 minutes to about 60 minutes, or from about 50 minutes to about 55 minutes.

The third time period (T3) may he from about 55 minutes to about 120 minutes, from about 55 minutes to about 115 minutes, from about 55 minutes to about 110 minutes, from about 55 minutes to about 105 minutes, from about 55 minutes to about 100 minutes, from about 55 minutes to about 95 minutes, from about 55 minutes to about 90 minutes, from about 55 minutes to about 85 minutes, from about 55 minutes to about 80 minutes, from about 55 minutes to about 75 minutes, from about 55 minutes to about 70 minutes, from about 55 minutes to about 65 minutes, or from about 55 minutes to about 60 minutes.

The third time period (T3) may be from about 60 minutes to about 120 minutes, from about 60 minutes to about 115 minutes, from about 60 minutes to about 110 minutes, from about 60 minutes to about 105 minutes, from about 60 minutes to about minutes, from about 60 minutes to about 95 minutes, from about 60 minutes to about 90 minutes, from about 60 minutes to about 85 minutes, from about 60 minutes to about 80 minutes, from about 60 minutes to about 75 minutes, from about 60 minutes to about 70 minutes, or from about 60 minutes to about 65 minutes.

The third time period (T3) may he from about 65 minutes to about 120 minutes, from about 65 minutes to about 115 minutes, from about 65 minutes to about 110 minutes, from about 65 minutes to about 105 minutes, from about 65 minutes to about 100 minutes, from about 65 minutes to about 95 minutes, from about 65 minutes to about 90 minutes, from about 65 minutes to about 85 minutes, from about 65 minutes to about 80 minutes, from about 65 minutes to about 75 minutes, or from about 65 minutes to about 70 minutes.

The third time period (T3) may be from about 70 minutes to about 120 minutes, from about 70 minutes to about 115 minutes, from about 70 minutes to about 110 minutes, from about 70 minutes to about 105 minutes, from about 70 minutes to about 100 minutes, from about 70 minutes to about 95 minutes, from about 70 minutes to about 90 minutes, from about 70 minutes to about 85 minutes, from about 70 minutes to about 80 minutes, or from about 70 minutes to about 75 minutes.

The third time period (T3) may be from about 75 minutes to about 120 minutes, from about 75 minutes to about 115 minutes, from about 75 minutes to about 110 minutes, from about 75 minutes to about 105 minutes, from about 75 minutes to about 100 minutes, from about 75 minutes to about 95 minutes, from about 75 minutes to about 90 minutes, from about 75 minutes to about 85 minutes, or from about 75 minutes to about 80 minutes.

The third time period (T3) may he from about 80 minutes to about 120 minutes, from about 80 minutes to about 115 minutes, from about 80 minutes to about 110 minutes, from about 80 minutes to about 105 minutes, from about 80 minutes to about minutes, from about 80 minutes to about 95 minutes, from about 80 minutes to about 90 minutes, or from about 80 minutes to about 85 minutes.

The third time period (T3) may he from about 85 minutes to about 120 minutes, from about 85 minutes to about 115 minutes, from about 85 minutes to about 110 30 minutes, from about 85 minutes to about 105 minutes, from about 85 minutes to about minutes, from about 85 minutes to about 95 minutes, or from about 85 minutes to about 90 minutes.

The third time period (T3) may be from about 90 minutes to about 120 minutes, from about 90 minutes to about 115 minutes, from about 90 minutes to about 110 minutes, from about 90 minutes to about 105 minutes, from about 90 minutes to about minutes, or from about 90 minutes to about 95 minutes.

The third time period (T3) may be from about 95 minutes to about 120 minutes, from about 95 minutes to about 115 minutes, from about 95 minutes to about 110 minutes, from about 95 minutes to about 105 minutes, or from about 95 minutes to about 100 minutes.

The third time period (T3) may be from about 100 minutes to about 120 minutes, from about 100 minutes to about 115 minutes, from about 100 minutes to about 110 minutes, or from about 100 minutes to about 105 minutes.

The third time period (T3) may be from about 105 minutes to about 120 minutes, from about 105 minutes to about 115 minutes. or from about 105 minutes to about 110 minutes.

The third time period (T3) may be from about 110 minutes to about 120 minutes, or from about 110 minutes to about 115 minutes.

The third time period (T3) may be from about 115 minutes to about 120 minutes.

The third time period (T3) may be about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 60 minutes, 65 minutes, about 70 minutes, about 75 minutes, about 80 minutes, about 85 minutes, about 90 minutes, about 95 minutes, about 100 minutes, about 105 minutes, about 110 minutes, about 115 minutes, or about 120 minutes.

The third time period (T3) may be at least about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 60 minutes, 65 minutes, about 70 minutes, about 75 minutes, about 80 minutes, about 85 minutes, about 90 minutes, about 95 minutes, about 100 minutes, about 105 minutes, about 110 minutes, about 115 minutes, or at least about 120 minutes.

The third time period (T3) may be no more than about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 60 minutes, 65 minutes, about 70 minutes, about 75 minutes, about 80 minutes, about 85 minutes, about 90 minutes, about 95 minutes, about 100 minutes, about 105 minutes, about 110 minutes, about 115 minutes, or no more than about 120 minutes.

The first pressure (P1) may be about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or about 5.0 times greater than the third pressure (P3).

The first pressure (P1) may be at least about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or at least about 5.0 times greater than the third pressure (P3).

The first pressure (P1) may be no more than about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 limes, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or no more than about 5.0 times greater than the third pressure (P3).

The first pressure (P1) may be from about 0.25 to about 5.0 times greater than the third pressure (P3), from about 0.50 times to about 4.5 times, from about 0.75 times to about 4.0 times, from about 1.0 times to about 3.5 times, from about 1.5 times to about 3.0 times, from about 1.5 times to about 2.5 times, or about 2.0 times greater than the third pressure (P3).

The first pressure (P1) may be from about 0.25 to about 5.0 times greater than the third pressure (P3), from about 0.25 to about 4.5 times, from about 0.25 to about 4.0 times, from about 0.25 to about 3.5 times, from about 0.25 to about 3.0 times, from about 0.25 to about 2.5 times, from about 0.25 to about 2.0 times, from about 0.25 to about 1.5 times, from about 0.25 to about 1.0 times, from about 0.25 to about 0.75 times, or from about 0.25 to about 0.50 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 0.50 to about 5.0 times greater than the third pressure (P3), from about 0.50 to about 4.5 times, from about 0.50 to about 4.0 times, from about 0.50 to about 3.5 times, from about 0.50 to about 3.0 times, from about 0.50 to about 2.5 times, from about 0.50 to about 2.0 times, from about 0.50 to about 1.5 times, from about 0.50 to about 1.0 times, or from about 0.50 to about 0.75 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 0.75 to about 5.0 times greater than the third pressure (P3), from about 0.75 to about 4.5 times, from about 0.75 to about 4.0 times, from about 0.75 to about 3.5 times, from about 0.75 to about 3.0 times, from about 0.75 to about 2.5 times, from about 0.75 to about 2.0 times, from about 0.75 to about 1.5 times, or from about 0.75 to about 1.0 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 1.0 to about 5.0 times greater than the third pressure (P3), from about 1.0 to about 4.5 times, from about 1.0 to about 4.0 times, from about 1.0 to about 3.5 times, from about 1.0 to about 3.0 times, from about 1.0 to about 2.5 times, from about 1.0 to about 2.0 times, or from about 1.0 to about 1.5 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 1.5 to about 5.0 times greater than the third pressure (P3), from about 1.5 to about 4.5 times, from about 1.5 to about 4.0 times, from about 1.5 to about 3.5 times, from about 1.5 to about 3.0 times, from about 1.5 to about 2.5 times, or from about 1.5 to about 2.0 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 2.0 to about 5.0 times greater than the third pressure (P3), from about 2.0 to about 4.5 times, from about 2.0 to about 4.0 times, from about 2.0 to about 3.5 times, from about 2.0 to about 3.0 times, or from about 2.0 to about 2.5 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 2.5 to about 5.0 times greater than the third pressure (P3), from about 2.5 to about 4.5 times, from about 2.5 to about 4.0 times, from about 2.5 to about 3.5 times, or from about 2.5 to about 3.0 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 3.0 to about 5.0 times greater than the third pressure (P3), from about 3.0 to about 4.5 times, from about 3.0 to about 4.0 times, or from about 3.0 to about 3.5 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 3.5 to about 5.0 times greater than the third pressure (P3), from about 3.5 to about 4.5 times, or from about 3.5 to about 4.0 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 4.0 to about 5.0 times greater than the third pressure (P3), or from about 4.0 to about 4.5 times, greater than the third pressure (P3).

The first pressure (P1) may be from about 4.5 to about 5.0 times greater than the third pressure (P3).

The third pressure (P3) may be about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or about 5.0 times greater than the first pressure (P1).

The third pressure (P3) may be at least about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or at least about 5.0 times greater than the first pressure (P1).

The third pressure (P3) may be no more than about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 limes, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or no more than about 5.0 times greater than the first pressure (P1).

The third pressure (P3) may be from about 0.25 to about 5.0 times greater than the first pressure (P1), from about 0.5 times to about 4.5 times, from about 0.75 times to about 4.0 times, from about 1.0 times to about 3.5 times, from about 1.5 times to about 3.0 times, from about 1.5 times to about 2.5 times, or about 2.0 times greater than the first pressure (P1).

The third pressure (P3) may be from about 0.25 to about 5.0 times greater than the first pressure (P1), from about 0.25 to about 4.5 times, from about 0.25 to about 4.0 times, from about 0.25 to about 3.5 times, from about 0.25 to about 3.0 times, from about 0.25 to about 2.5 times, from about 0.25 to about 2.0 times, from about 0.25 to about 1.5 times, from about 0.25 to about 1.0 times, from about 0.25 to about 0.75 times, or from about 0.25 to about 0.50 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 0.50 to about 5.0 times greater than the first pressure (PI), from about 0.50 to about 4.5 times, from about 0.50 to about 4.0 times, from about 0.50 to about 3.5 times, from about 0.50 to about 3.0 times, from about 0.50 to about 2.5 times, from about 0.50 to about 2.0 times, from about 0.50 to about 1.5 times, from about 0.50 to about 1.0 times, or from about 0.50 to about 0.75 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 0.75 to about 5.0 times greater than the first pressure (P1), from about 0.75 to about 4.5 times, from about 0.75 to about 4.0 times, from about 0.75 to about 3.5 times, from about 0.75 to about 3.0 times, from about 0.75 to about 2.5 times, from about 0.75 to about 2.0 times, from about 0.75 to about 1.5 times, or from about 0.75 to about 1.0 ti mes, greater than the first pressure (P1).

The third pressure (P3) may he from about 1.0 to about 5.0 times greater than the first pressure (P1), from about 1.0 to about 4.5 times, from about 1.0 to about 4.0 times, from about 1.0 to about 3.5 times, from about 1.0 to about 3.0 times, from about 1.0 to about 2.5 times, from about 1.0 to about 2.0 times, or from about 1.0 to about 1.5 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 1.5 to about 5.0 times greater than the first pressure (P1), from about 1.5 to about 4.5 times, from about 1.5 to about 4.0 times, from about 1.5 to about 3.5 times, from about 1.5 to about 3.0 times, from about 1.5 to about 2.5 times, or from about 1.5 to about 2.0 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 2.0 to about 5.0 times greater than the first pressure (P1), from about 2.0 to about 4.5 times, from about 2.0 to about 4.0 times, from about 2.0 to about 3.5 times, from about 2.0 to about 3.0 times, or from about 2.0 to about 2.5 times, greater than the first pressure (P1).

The third pressure (P3) may he from about 2.5 to about 5.0 times greater than the first pressure (P1), from about 2.5 to about 4.5 times, from about 2.5 to about 4.0 times, from about 2.5 to about 3.5 times, or from about 2.5 to about 3.0 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 3.0 to about 5.0 times greater than the first pressure (P1), from about 3.0 to about 4.5 times, from about 3.0 to about 4.0 times, or from about 3.0 to about 3.5 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 3.5 to about 5.0 times greater than the first pressure (P1), from about 3.5 to about 4.5 times, or from about 3.5 to about 4.0 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 4.0 to about 5.0 times greater than the first pressure (P1), or from about 4.0 to about 4.5 times, greater than the first pressure (P1).

The third pressure (P3) may be from about 4.5 to about 5.0 times greater than the first pressure (P1).

The first pressure (P1) and the third pressure (P3) may be substantially equal.

The first time period (TO) may be about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or about 5.0 times greater than the third time period (T3).

The first time period (T1) may be at least about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or at least about 5.0 times greater than the third time period (T3).

The first time period (Ti) may be no more than about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or no more than about 5.0 times greater than the third time period (T3).

The first time period (T1) may be from about 0.25 times to about 5.0 times greater than the third time period (T3), from about 0.5 times to about 4.5 times, from about 0.75 times to about 4.0 times, from about 1.0 limes to about 3.5 times, from about 1.5 times to about 3.0 times, from about 1.5 times to about 2.5 times, or about 2.0 times greater than the third time period (T3).

The first time period (T1) may be from about 0.25 to about 5.0 times greater than the third time period (T3), from about 0.25 to about 4.5 times, from about 0.25 to about 4.0 times, from about 0.25 to about 3.5 times, from about 0.25 to about 3.0 times, from about 0.25 to about 2.5 times, from about 0.25 to about 2.0 times, from about 0.25 to about 1.5 times, from about 0.25 to about 1.0 times, from about 0.25 to about 0.75 times, or from about 0.25 to about 0.50 times, greater than the third time period (T3).

The first time period (T1) may be from about 0.50 to about 5.0 times greater than the third time period (T3), from about 0.50 to about 4.5 times, from about 0.50 to about 4.0 times, from about 0.50 to about 3.5 times, from about 0.50 to about 3.0 times, from about 0.50 to about 2.5 times, from about 0.50 to about 2.0 times, from about 0.50 to about 1.5 times, from about 0.50 to about 1.0 times, or from about 0.50 to about 0.75 times, greater than the third time period (T3).

The first time period (T1) may be from about 0.75 to about 5.0 times greater than the third time period (T3), from about 0.75 to about 4.5 times, from about 0.75 to about 4.0 times, from about 0.75 to about 3.5 times, from about 0.75 to about 3.0 times, from about 0.75 to about 2.5 times, from about 0.75 to about 2.0 times, from about 0.75 to about 1.5 times, or from about 0.75 to about 1.0 times, greater than the third time period (T3).

The first time period (rl) may be from about 1.0 to about 5.0 times greater than the third time period (T3), from about 1.0 to about 4.5 times, from about 1.0 to about 4.0 times, from about 1.0 to about 3.5 times, from about 1.0 to about 3.0 times, from about 1.0 to about 2.5 times, from about 1.0 to about 2.0 times, or from about 1.0 to about 1.5 times, greater than the third time period (T3).

The first time period (T1) may be from about 1.5 to about 5.0 times greater than the third time period (T3), from about 1.5 to about 4.5 times, from about 1.5 to about 4.0 times, from about 1.5 to about 3.5 times, from about 1.5 to about 3.0 times, from about 1.5 to about 2.5 times, or from about 1.5 to about 2.0 times, greater than the third time period (T3).

The first time period (T1) may be from about 2.0 to about 5.0 times greater than the third time period (T3), from about 2.0 to about 4.5 times, from about 2.0 to about 4.0 times, from about 2.0 to about 3.5 times, from about 2.0 to about 3.0 times, or from about 2.0 to about 2.5 times, greater than the third time period (T3).

The first time period (T1) may be from about 2.5 to about 5.0 times greater than the third time period (T3), from about 2.5 to about 4.5 times, from about 2.5 to about 4.0 times, from about 2.5 to about 3.5 times, or from about 2.5 to about 3.0 times, greater than the third time period (T3).

The first time period (T1) may be from about 3.0 to about 5.0 times greater than the third time period (T3), from about 3.0 to about 4.5 times, from about 3.0 to about 4.0 times, or from about 3.0 to about 3.5 times, greater than the third time period (T3).

The first time period (T1) may be from about 15 to about 5.0 times greater than the third time period (T3). from about 3.5 to about 4.5 times, or from about 3.5 to about 4.0 times, greater than the third time period (T3).

The first time period (T1) may be from about 4.0 to about 5.0 times greater than the third time period (T3), or from about 4.0 to about 4.5 times, greater than the third time period (T3).

The first time period (T1) may be from about 4.5 to about 5.0 times greater than the third time period (T3).

The third time period (T3) may he about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or about 5.0 times greater than the first time period (T1).

The third time period (T3) may he at least about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or at least about 5.0 times greater than the first time period (T1).

The third time period (T3) may be no more than about 0.5 times, about 1.0 times, about 1.5 times, about 2.0 times, about 2.5 times, about 3.0 times, about 3.5 times, about 4.0 times, about 4.5 times, or no more than about 5.0 times greater than the first time period (T1).

The third time period (T3) may be from about 0.25 times to about 5.0 times greater than the first time period (T1), from about 0.5 times to about 4.5 times, from about 0.75 times to about 4.0 times, from about 1.0 times to about 3.5 times, from about 1.5 times to about 3.0 times, from about 1.5 times to about 2.5 times, or about 2.0 times greater than the first time period (T1).

The third time period (T3) may be from about 0.25 to about 5.0 times greater than the first time period (T1), from about 0.25 to about 4.5 times, from about 0.25 to about 4.0 times, from about 0.25 to about 3.5 times, from about 0.25 to about 3.0 times, from about 0.25 to about 2.5 times, from about 0.25 to about 2.0 times, from about 0.25 to about 1.5 times, from about 0.25 to about 1.0 times, from about 0.25 to about 0.75 times, or from about 0.25 to about 0.50 times, greater than the first time period (T1).

The third time period (T3) may be from about 0.50 to about 5.0 times greater than the first time period (T1), from about 0.50 to about 4.5 times, from about 0.50 to about 4.0 times, from about 0.50 to about 3.5 times, from about 0.50 to about 3.0 times, from about 0.50 to about 2.5 times, from about 0.50 to about 2.0 times, from about 0.50 to about 1.5 times, from about 0.50 to about 1.0 times, or from about 0.50 to about 0.75 times, greater than the first time period (T1).

The third time period (T3) may be from about 0.75 to about 5.0 times greater than the first time period (T1), from about 0.75 to about 4.5 times, from about 0.75 to about 4.0 times, from about 0.75 to about 3.5 times, from about 0.75 to about 3.0 times, from about 0.75 to about 2.5 times, from about 0.75 to about 2.0 times, from about 0.75 to about 1.5 times, or from about 0.75 to about 1.0 times, greater than the first time period (T1).

The third time period (T3) may be from about 1.0 to about 5.0 times greater than the first time period (T1), from about 1.0 to about 4.5 times, from about 1.0 to about 4.0 times, from about 1.0 to about 3.5 times, from about 1.0 to about 3.0 times, from about 1.0 to about 2.5 times, from about 1.0 to about 2.0 times, or from about 1.0 to about 1.5 times, greater than the first time period (T1).

The third time period (T3) may be from about 1.5 to about 5.0 times greater than the first time period (T1), from about 1.5 to about 4.5 times, from about 1.5 to about 4.0 times, from about 1.5 to about 3.5 times, from about 1.5 to about 3.0 times, from about 1.5 to about 2.5 times, or from about 1.5 to about 2.0 times, greater than the first time period (T1).

The third time period (T3) may be from about 2.0 to about 5.0 times greater than the first time period (T1), from about 2.0 to about 4.5 times, from about 2.0 to about 4.0 times, from about 2.0 to about 3.5 times, from about 2.0 to about 3.0 times, or from about 2.0 to about 2.5 times, greater than the first time period (T1).

The third time period (T3) may be from about 2.5 to about 5.0 times greater than the first time period (T1), from about 2.5 to about 4.5 times, from about 2.5 to about 4.0 times, from about 2.5 to about 3.5 times, or from about 2.5 to about 3.0 times, greater than the first time period (T1).

The third time period (T3) may be from about 3.0 to about 5.0 times greater than the first time period (Ti), from about 3.0 to about 4.5 times, from about 3.0 to about 4.0 times, or from about 3.0 to about 3.5 times, greater than the first time period (T1).

The third time period (T3) may be from about 3.5 to about 5.0 times greater than the first time period (T1), from about 3.5 to about 4.5 times, or from about 3.5 to about 4.0 times, greater than the first time period (T1).

The third time period (T3) may be from about 4.0 to about 5.0 times greater than the first time period (T1), or from about 4.0 to about 4.5 times, greater than the first time period (T1).

The third time period (T3) may be from about 4.5 to about 5.0 times greater than the first time period (T1).

The first time period (T1) and the third time period (T3) may be substantially equal.

The second pressure (P2) may be any pressure below the first pressure (P1) and the third pressure (P3).

The second pressure (P2) may he about 0.1 bara, about 0.2 bara, about 0.3 bara, about 0.4 btu-a, about 0.5 bara, about 1.0 bara, about 1.5 bara, about 2.0 btu-a, about 2.5 bara, about 3.0 btu-a, about 3.5 bara, about 4.0 btu-a, about 4.5 bara, about 5.0 bara, about 5.5 ban, about 6.0 bara, about 6.5 bara, about 7.0 bara, about 7.5 bara, about 8.0 bara, about 8.5 bara, or about 9.0 bara.

The second pressure (P2) may he no more than about 0.1 bara, about 0.2 bara, about 0.3 bara, about 0.4 bara, about 0.5 bara, about 1.0 bara, about 1.5 bara, about 2.0 bara, about 2.5 bara, about 3.0 bara, about 3.5 bara, about 4.0 bara, about 4.5 btu-a, about 5.0 ban, about 5.5 bara, about 6.0 bara, about 6.5 bara, about 7.0 bara, about 7.5 bara, about 8.0 bara, about 8.5 hara, or no more than about 9.0 bara.

The second pressure (P2) may be from about 0.1 bara to about 9.0 bara, from about 0.1 bara to about 8.5 bara, from about 0.1 bara to about 8.0 btu-a, from about 0.1 hara to about 7.5 hara, from about 0.1 hara to about 7.0 hara, from about 0.1 hara to about 6.5 hara, from about 0.1 hara to about 6.0 hara, from about 0.1 bara to about 5.5 hara, from about 0.1 hara to about 5.0 hara, from about 0.1 hara to about 4.5 hara, from about 0.1 bara to about 4.0 bara, from about 0.1 bara to about 3.5 bara, from about 0.1 hara to about 3.0 hara, from about 0.1 hara to about 2.5 hara, from about 0.1 hara to about 2.0 bara, from about 0.1 btu-a to about 1.5 bara, from about 0.1 bara to about 1.0 bara, or from about 0.1 btu-a to about 0.5 bara.

The second pressure (P2) may he from about 0.1 hara to about 9.0 bara, from about 0.2 bara to about 8.5 bara, from about 0.2 bara to about 8.0 bara, from about 0.2 bara to about 7.5 bara, from about 0.2 bara to about 7.0 bara, from about 0.2 bara to about 6.5 bara, from about 0.2 bara to about 6.0 bara, from about 0.2 bara to about 5.5 hara, from about 0.2 hara to about 5.0 hara, from about 0.2 hara to about 4.5 bara, from about 0.2 bara to about 4.0 bara, from about 0.2 bara to about 3.5 bara, from about 0.2 hara to about 3.0 hara, from about 0.2 hara to about 2.5 hara, from about 0.2 hara to about 2.0 bara, from about 0.2 bara to about 1.5 bara, from about 0.2 bara to about 1.0 hara, or from about 0.2 hara to about 0.5 hara.

The second pressure (P2) may be from about 0.3 bara to about 9.0 bara, from about 0.3 hara to about 8.5 bara, from about 0.3 bara to about 8.0 hara, from about 0.3 hara to about 7.5 hara, from about 0.3 hara to about 7.0 hara, from about 0.3 hara to about 6.5 bara, from about 0.3 bara to about 6.0 bara, from about 0.3 bara to about 5.5 bara, from about 0.3 bara to about 5.0 bara, from about 0.3 bara to about 4.5 bara, from about 0.3 bara to about 4.0 btu-a, from about 0.3 btu-a to about 3.5 bares, from about 0.3 bara to about 3.0 bara, from about 0.3 bara to about 2.5 bara, from about 0.3 bara to about 2.0 bara, from about 0.3 bara to about 1.5 bara, from about 0.3 bara to about 1.0 bara, or from about 0.3 bara to about 0.5 bara.

The second pressure (P2) may he from about 0.4 bara to about 9.0 bara, from about 0.4 bara to about 8.5 bara, from about 0.4 bara to about 8.0 butt, from about 0.4 bara to about 7.5 bara, from about 0.4 bara to about 7.0 bara, from about 0.4 bara to about 6.5 bara, from about 0.4 hara to about 6.0 bara, from about 0.4 bara to about 5.5 bara, from about 0.4 bara to about 5.0 bara, from about 0.4 hara to about 4.5 bara, from about 0.4 bara to about 4.0 bara, from about 0.4 bara to about 3.5 hara, from about 0.4 bara to about 3.0 bara, from about 0.4 bara to about 2.5 bara, from about 0.4 bara to about 2.0 bara, from about 0.4 bara to about 1.5 bara, from about 0.4 bara to about 1.0 bara, or from about 0.4 bara to about 0.5 bara.

The second pressure (P2) may be from about 0.5 bara to about 9.0 bara, from about 0.5 bara to about 8.5 bara, from about 0.5 bara to about 8.0 bara, from about 0.5 bara to about 7.5 bara, from about 0.5 bara to about 7.0 bara, from about 0.5 bara to about 6.5 bara, from about 0.5 bat-a to about 6.0 bara, from about 0.5 bara to about 5.5 bara, from about 0.5 bara to about 5.0 bara, from about 0.5 bara to about 4.5 bara, from about 0.5 bara to about 4.0 bara, from about 0.5 bara to about 3.5 bara, from about 0.5 bara to about 3.0 bara, from about 0.5 bara to about 2.5 bara, from about 0.5 bara to about 2.0 bara, from about 0.5 bara to about 1.5 bara, or from about 0.5 bara to about 1.0 bara.

The second pressure (P2) may be from about 1.0 bara to about 9.0 bara, from about 1.0 bara to about 8.5 bara, from about 1.0 bara to about 8.0 hara, from about 1.0 bara to about 7.5 bara, from about 1.0 bara to about 7.0 bara, from about 1.0 bara to about 6.5 bara, from about 1.0 bara to about 6.0 bara, from about 1.0 bara to about 5.5 bara, from about 1.0 bara to about 5.0 bara, from about 1.0 bara to about 4.5 bara, from about 1.0 bara to about 4.0 bara, from about 1.0 bara to about 3.5 bara, from about 1.0 Kara to about 3.0 bara, from about 1.0 bara to about 2.5 bara, from about 1.0 bara to about 2.0 bara, or from about 1.0 ban to about 1.5 bara.

The second pressure (P2) may be from about 1.5 bara to about 9.0 bara, from about 1.5 bara to about 8.5 bara, from about 1.5 bara to about 8.0 bara, from about 1.5 bara to about 7.5 bara, from about 1.5 bara to about 7.0 bara, from about 1.5 tiara to about 6.5 bara, from about 1.5 bara to about 6.0 bara, from about 1.5 bara to about 5.5 Kara, from about 1.5 bara to about 5.0 bara, from about 1.5 bara to about 4.5 bara, from about 1.5 bara to about 4.0 bara, from about 1.5 bara to about 3.5 bara, from about 1.5 bara to about 3.0 bara, from about 1.5 bara to about 2.5 bara, or from about 1.5 bara to about 2.0 bara.

The second pressure (P2) may be from about 2.0 bara to about 9.0 bara, from about 2.0 bara to about 8.5 bara, from about 2.0 bara to about 8.0 Nu-a, from about 2.0 bara to about 7.5 bara, from about 2.0 hara to about 7.0 bara, from about 2.0 hara to about 6.5 bara, from about 2.0 hara to about 6.0 bara, from about 2.0 barn to about 5.5 bara, from about 2.0 bara to about 5.0 bara, from about 2.0 bara to about 4.5 bara, from about 2.0 bara to about 4.0 bara, from about 2.0 bara to about 3.5 bara, from about 2.0 bara to about 3.0 bara, or from about 2.0 bara to about 2.5 bara.

The second pressure (P2) may be from about 2.5 bara to about 9.0 bara, from about 2.5 bara to about 8.5 bara, from about 2.5 bara to about 8.0 bara, from about 2.5 bara to about 7.5 bara, from about 2.5 bara to about 7.0 bara, from about 2.5 bara to about 6.5 bara, from about 2.5 bara to about 6.0 bara, from about 2.5 ban to about 5.5 bara, from about 2.5 bara to about 5.0 bara, from about 2.5 bara to about 4.5 bara, from about 2.5 bara to about 4.0 bara, from about 2.5 bara to about 3.5 bara, or from about 2.5 bara to about 3.0 bara.

The second pressure (P2) may he from about 3.0 bara to about 9.0 bara, from about 3.0 bara to about 8.5 bara, from about 3.0 bara to about 8.0 bara, from about 3.0 bara to about 7.5 bara, from about 3.0 bara to about 7.0 bara, from about 3.0 bara to about 6.5 bara, from about 3.0 Nu-a to about 6.0 bara, from about 3.0 bara to about 5.5 bara, from about 3.0 bara to about 5.0 bara, from about 3.0 bara to about 4.5 bara, from about 3.0 bara to about 4.0 bara, or from about 3.0 bara to about 3.5 bara.

The second pressure (P2) may he from about 3.5 bara to about 9.0 bara, from about 3.5 bara to about 8.5 bara, from about 3.5 ban to about 8.0 bara, from about 3.5 bara to about 7.5 bara, from about 3.5 bara to about 7.0 ban, from about 3.5 bara to about 6.5 bara, from about 3.5 bara to about 6.0 bara, from about 3.5 bara to about 5.5 bara, from about 3.5 bara to about 5.0 bara, from about 3.5 bara to about 4.5 bara, or from about 3.5 bara to about 4.0 bara.

The second pressure (P2) may he from about 4.0 bara to about 9.0 bara, from about 4.0 bara to about 8.5 bara, from about 4.0 bara to about 8.0 bara, from about 4.0 bara to about 7.5 bara, from about 4.0 bara to about 7.0 bara, from about 4.0 bara to about 6.5 bara, from about 4.0 bara to about 6.0 bara, from about 4.0 bara to about 5.5 bara, from about 4.0 bara to about 5.0 hara, or from about 4.0 bara to about 4.5 bara.

The second pressure (P2) may be from about 4.5 bara to about 9.0 bara, from about 4.5 bara to about 8.5 bara, from about 4.5 bara to about 8.0 bara, from about 4.5 bara to about 7.5 bara, from about 4.5 ham to about 7.0 bara, from about 4.5 bara to about 6.5 hara, from about 4.5 bara to about 6.0 bara, from about 4.5 hara to about 5.5 bara, or from about 4.5 bara to about 5.0 bara.

The second pressure (P2) may be from about 5.0 bara to about 9.0 bara, from about 5.0 bara to about 8.5 bara, from about 5.0 bara to about 8.0 bara, from about 5.0 bara to about 7.5 bara, from about 5.0 bara to about 7.0 bara, from about 5.0 bara to about 6.5 hara, from about 5.0 hara to about 6.0 bara, or from about 5.0 hara to about 5.5 bara.

The second pressure (P2) may he from about 5.5 hara to about 9.0 bara, from about 5.5 hara to about 8.5 hara, from about 5.5 hara to about 8.0 hara, from about 5.5 bara to about 7.5 bara, from about 5.5 bara to about 7.0 bara, from about 5.5 bara to about 6.5 bara, or from about 5.5 hara to about 6.0 hara.

The second pressure (P2) may be from about 6.0 bara to about 9.0 bara, from about 6.0 bara to about 8.5 bara, from about 6.0 bara to about 8.0 Nu-a, from about 6.0 hara to about 7.5 hara, from about 6.0 hara to about 7.0 hara, or from about 6.0 hara to about 6.5 hara.

The second pressure (P2) may he from about 6.5 bara to about 9.0 bara, from about 6.5 bara to about 8.5 bara, from about 6.5 ban to about 8.0 bara, from about 6.5 bara to about 7.5 tiara, or from about 6.5 bara to about 7.0 bara.

The second pressure (P2) may he from about 7.0 bara to about 9.0 bara from about 7.0 bara to about 8.5 bara, from about 7.0 ban to about 8.0 bara, or from about 7.0 bara to about 7.5 bara.

The second pressure (P2) may be from about 7.5 bara to about 9.0 bara, from about 7.5 bara to about 8.5 bara, or from about 7.5 bara to about 8.0 bara.

The second pressure (P2) may be from about 8.0 bara to about 9.0 bara, or from about 8.0 bara to about 8.5 bara.

The second pressure (P2) may he from about 8.5 bara to about 9.0 bara. The second pressure (P2) may be atmospheric pressure.

The second pressure (P2) may be below atmospheric pressure.

The second pressure (P2) may the lowest pressure value of a range of pressure values which are less than the first pressure and the third pressure, and which occurs between the first pressure and the third pressure.

The method may comprise decreasing the pressure from the first pressure (P1) to the second pressure (P2) over the course of from about 25 minutes to about 55 minutes, from about 28 minutes to about 52 minutes, from about 30 minutes to about 50 minutes, from about 32 minutes to about 48 minutes, from about 34 minutes to about 46 minutes, from about 36 minutes to about 44 minutes, from about 38 minutes to about 42 minutes, or about 40 minutes.

The method may comprise decreasing the pressure from the first pressure (P1) to the second pressure (P2) over the course of about 25 minutes, 26 minutes, about 27 minutes, about 28 minutes, about 29 minutes, about 30 minutes, about 31 minutes, about 32 minutes, about 33 minutes, about 34 minutes, about 35 minutes, about 36 minutes, about 37 minutes, about 38 minutes, about 39 minutes, about 40 minutes, about 41 minutes, about 42 minutes, about 43 minutes, about 44 minutes, about 45 minutes, about 46 minutes, about 47 minutes, about 48 minutes, about 49 minutes, about 50 minutes, about 51 minutes, about 52 minutes, about 53 minutes, about 54 minutes, or about 55 minutes.

The method may comprise decreasing the pressure from the first pressure (P1) to the second pressure (P2) over the course of at least about 25 minutes, 26 minutes, about 27 minutes, about 28 minutes, about 29 minutes, about 30 minutes, about 31 minutes, about 32 minutes, about 33 minutes, about 34 minutes, about 35 minutes, about 36 minutes, about 37 minutes, about 38 minutes, about 39 minutes, about 40 minutes, about 41 minutes, about 42 minutes, about 43 minutes, about 44 minutes, about 45 minutes, about 46 minutes, about 47 minutes, about 48 minutes, about 49 minutes, about 50 minutes, about 51 minutes, about 52 minutes, about 53 minutes, about 54 minutes, or at least about 55 minutes.

The method may comprise decreasing the pressure from the first pressure (P1) to the second pressure (P2) over the course of no more than about 25 minutes, 26 minutes, about 27 minutes, about 28 minutes, about 29 minutes, about 30 minutes, about 31 minutes, about 32 minutes, about 33 minutes, about 34 minutes, about 35 minutes, about 36 minutes, about 37 minutes, about 38 minutes, about 39 minutes, about 40 minutes, about 41 minutes, about 42 minutes, about 43 minutes, about 44 minutes, about 45 minutes, about 46 minutes, about 47 minutes, about 48 minutes, about 49 minutes, about 50 minutes, about 51 minutes, about 52 minutes, about 53 minutes, about 54 minutes, or no more than about 55 minutes.

The method may comprise increasing the pressure from the second pressure (P2) to the third pressure (P3) over the course of from about 2 minutes to about 18 minutes, from about 4 minutes to about 16 minutes, from about 6 minutes to about 14 minutes, from about 8 minutes to about 12 minutes, or about 10 minutes.

The method may comprise increasing the pressure from the second pressure (P2) to the third pressure (P3) over the course of about 2 minutes, about 4 minutes, about 6 minutes. about 8 minutes, about 10 minutes. about 12 minutes. about 14 minutes, about 16 minutes, about 18 minutes, or about 20 minutes.

The method may comprise increasing the pressure from the second pressure (P2) to the third pressure (P3) over the course of at least about 2 minutes, about 4 minutes, about 6 minutes, about 8 minutes, about 10 minutcs, about 12 minutes, about 14 minutes, about 16 minutes, about 18 minutes, or at least about 20 minutes.

The method may comprise increasing the pressure from the second pressure (P2) to the third pressure (P3) over the course of no more than about 2 minutes, about 4 minutes, about 6 minutes, about 8 minutes, about 10 minutes, about 12 minutes, about 14 minutes, about 16 minutes, about 18 minutes, or no more than about 20 minutes.

A second time period (T2) may define the duration of the second pressure (P2). The second time period (T2) may be from about 0.1 minutes to about 100 minutes, from about 0.2 minutes to about 95 minutes, from about 0.3 minutes to about 90 minutes, from about 0.4 minutes to about 85 minutes, from about 0 5 minutes to about 85 minutes, from about 1 minute to about 80 minutes, from about 2 minutes to about 75 minutes, from about 3 minutes to about 70 minutes, from about 4 minutes to about 65 minutes, from about 5 minutes to about 60 minutes, from about 10 minutes to about 55 minutes, from about 15 minutes to about 50 minutes, from about 20 minutes to about 45 minutes, from about 25 minutes to about 40 minutes, from about 30 minutes to about minutes, from about 33 minutes to about 37 minutes, or about 35 minutes.

The second time period (T2) may be from about 0 1 minutes to about 100 minutes, from about 0.1 minutes to about 95 minutes, from about 0.1 minutes to about 90 minutes, from about 0.1 minutes to about 85 minutes, from about 0.1 minutes to about 80 minutes, from about 0.1 minutes to about 75 minutes, from about 0.1 minutes to about 70 minutes, from about 0.1 minutes to about 65 minutes, from about 0.1 minutes to about 60 minutes, from about 0.1 minutes to about 55 minutes, from about 0.1 minutes to about 50 minutes, from about 0.1 minutes to about 45 minutes, from about 0.1 minutes to about 40 minutes, from about 0.1 minutes to about 35 minutes, from about 0.1 minutes to about 30 minutcs, from about 0.1 minutes to about 25 minutes, from about 0.1 minutes to about 20 minutes, from about 0.1 minutes to about minutes, from about 0.1 minutes to about 10 minutes, from about 0.1 minutes to about 5 minutes, from about 0.1 minutes to about 4 minutes, from about 0.1 minutes to about 3 minutes, from about 0.1 minutes to about 2 minutes, from about 0.1 minutes to about 1 minute, or from about 0.1 minutes to about 0.5 minutes.

The second time period (T2) may be from about 0.5 minutes to about 100 minutes, from about 0.5 minutes to about 95 minutes, from about 0 5 minutes to about 90 minutes, from about 0.5 minutes to about 85 minutes, from about 0.5 minutes to about 80 minutes, from about 0.5 minutes to about 75 minutes, from about 0.5 minutes to about 70 minutes, from about 0.5 minutes to about 65 minutes, from about 0.5 minutes to about 60 minutes, from about 0.5 minutes to about 55 minutes, from about 0.5 minutes to about 50 minutes, from about 0.5 minutes to about 45 minutes, from about 0.5 minutes to about 40 minutes, from about 0.5 minutes to about 35 minutes, from about 0.5 minutes to about 30 minutes, from about 0 5 minutes to about 25 minutes, from about 0.5 minutes to about 20 minutes, from about 0.5 minutes to about 15 minutes, from about 0.5 minutes to about 10 minutes, from about 0.5 minutes to about 5 minutes, from about 0.5 minutes to about 4 minutes, from about 0.5 minutes to about 3 minutes, from about 0.5 minutes to about 2 minutes, or from about 0.5 minutes to about 1 minute The second time period (T2) may be from about 1 minute to about 100 minutes, from about 1 minute to about 95 minutes, from about 1 minute to about 90 minutes, from about 1 minute to about 85 minutes, from about 1 minute to about 80 minutes, from about 1 minute to about 75 minutes, from about 1 minute to about 70 minutes, from about 1 minute to about 65 minutes, from about 1 minute to about 60 minutes, from about 1 minute to about 55 minutes, from about 1 minute to about 50 minutes, from about 1 minute to about 45 minutes, from about 1 minute to about 40 minutes, from about 1 minute to about 35 minutes, from about 1 minute to about 30 minutes, from about 1 minute to about 25 minutes, from about 1 minute to about 20 minutes, from about 1 minute to about 15 minutes, from about 1 minute to about 10 minutes, from about 1 minute to about 5 minutes, from about 1 minute to about 4 minutes, from about 1 minute to about 3 minutes, or from about 1 minute to about 2 minutes.

The second time period (T2) may be from about 2 minutes to about 100 minutes, from about 2 minutes to about 95 minutes, from about 2 minutes to about 90 minutes, from about 2 minutes to about 85 minutes, from about 2 minutes to about 80 minutes, from about 2 minutes to about 75 minutes, from about 2 minutes to about 70 minutes, from about 2 minutes to about 65 minutes, from about 2 minutes to about 60 minutes, from about 2 minutes to about 55 minutes, from about 2 minutes to about 50 minutes, from about 2 minutes to about 45 minutes, from about 2 minutes to about 40 minutes, from about 2 minutes to about 35 minutes, from about 2 minutes to about 30 minutes, from about 2 minutes to about 25 minutes, from about 2 minutes to about 20 minutes, from about 2 minutes to about 15 minutes, from about 2 minutes to about 10 minutes, from about 2 minutes to about 5 minutes, from about 2 minutes to about 4 minutes, or from about 2 minutes to about 3 minutes.

The second time period (T2) may be from about 3 minutes to about 100 minutes, from about 3 minutes to about 95 minutes, from about 3 minutes to about 90 minutes, from about 3 minutes to about 85 minutes, from about 3 minutes to about 80 minutes, from about 3 minutes to about 75 minutes, from about 3 minutes to about 70 minutes, from about 3 minutes to about 65 minutes, from about 3 minutes to about 60 minutes, from about 3 minutes to about 55 minutes, from about 3 minutes to about 50 minutes, from about 3 minutes to about 45 minutes, from about 3 minutes to about 40 minutes, from about 3 minutes to about 35 minutes, from about 3 minutes to about 30 minutes, from about 3 minutes to about 25 minutes, from about 3 minutes to about 20 minutes, from about 3 minutes to about 15 minutes, from about 3 minutes to about 10 minutes, from about 3 minutes to about 5 minutes, or from about 3 minutes to about 4 minutes.

The second time period (T2) may be from about 4 minutes to about 100 minutes, from about 4 minutes to about 95 minutes, from about 4 minutes to about 90 minutes, from about 4 minutes to about 85 minutes, from about 4 minutes to about 80 minutes, from about 4 minutes to about 75 minutes, from about 4 minutes to about 70 minutes, from about 4 minutes to about 65 minutes, from about 4 minutes to about 60 minutes, from about 4 minutes to about 55 minutes, from about 4 minutes to about 50 minutes, from about 4 minutes to about 45 minutes, from about 4 minutes to about 40 minutes, from about 4 minutes to about 35 minutes, from about 4 minutes to about 30 minutes, from about 4 minutes to about 25 minutes, from about 4 minutes to about 20 minutes, from about 4 minutes to about 15 minutes, from about 4 minutes to about 10 minutes, or from about 4 minutes to about 5 minutes.

The second time period (T2) may be from about 5 minutes to about 100 minutes, from about 5 minutes to about 95 minutes, from about 5 minutes to about 90 minutes, from about 5 minutes to about 85 minutes, from about 5 minutes to about 80 minutes, from about 5 minutes to about 75 minutes, from about 5 minutes to about 70 minutes, from about 5 minutes to about 65 minutes, from about 5 minutes to about 60 minutes, from about 5 minutes to about 55 minutes, from about 5 minutes to about 50 minutes, from about 5 minutes to about 45 minutes, from about 5 minutes to about 40 minutes, from about 5 minutes to about 35 minutes, from about 5 minutes to about 30 minutes, from about 5 minutes to about 25 minutes, from about 5 minutes to about 20 minutes, from about 5 minutes to about 15 minutes, or from about 5 minutes to about 10 minutes.

The second time period (T2) may be from about 10 minutes to about 100 minutes, from about 10 minutes to about 95 minutes, from about 10 minutes to about minutes, from about 10 minutes to about 85 minutes, from about 10 minutes to about 80 minutes, from about 10 minutes to about 75 minutes, from about 10 minutes to about 70 minutes, from about 10 minutes to about 65 minutes, from about 10 minutes to about 60 minutes, from about 10 minutes to about 55 minutes, from about 10 minutes to about 50 minutes, from about 10 minutes to about 45 minutes, from about 10 minutes to about minutes, from about 10 minutes to about 35 minutes, from about 10 minutes to about 30 minutes, from about 10 minutes to about 25 minutes, from about 10 minutes to about 20 minutes, or from about 10 minutes to about 15 minutes.

The second time period (T2) may be from about 15 minutes to about 100 minutes, from about 15 minutes to about 95 minutes, from about 15 minutes to about 90 minutes, from about 15 minutes to about 85 minutes, from about 15 minutes to about 80 minutes, from about 15 minutes to about 75 minutes, from about 15 minutes to about 70 minutes, from about 15 minutes to about 65 minutes, from about 15 minutes to about 60 minutes, from about 15 minutes to about 55 minutes, from about 15 minutes to about 50 minutes, from about 15 minutes to about 45 minutes, from about 15 minutes to about minutes, from about 15 minutes to about 35 minutes, from about 15 minutes to about 30 minutes, from about 15 minutes to about 25 minutes, or from about 15 minutes to about 20 minutes.

The second time period (T2) may be from about 20 minutes to about 100 30 minutes, from about 20 minutes to about 95 minutes, from about 20 minutes to about 90 minutes, from about 20 minutes to about 85 minutes, from about 20 minutes to about minutes, from about 20 minutes to about 75 minutes, from about 20 minutes to about 70 minutes, from about 20 minutes to about 65 minutes, from about 20 minutes to about 60 minutes, from about 20 minutes to about 55 minutes, from about 20 minutes to about 50 minutes, from about 20 minutes to about 45 minutes, from about 20 minutes to about 40 minutes, from about 20 minutes to about 35 minutes, from about 20 minutes to about minutes, or from about 20 minutes to about 25 minutes.

The second time period (T2) may be from about 25 minutes to about 100 minutes, from about 25 minutes to about 95 minutes, from about 25 minutes to about 90 minutes, from about 25 minutes to about 85 minutes, from about 25 minutes to about 80 minutes, from about 25 minutes to about 75 minutes, from about 25 minutes to about minutes, from about 25 minutes to about 65 minutes, from about 25 minutes to about 60 minutes, from about 25 minutes to about 55 minutes, from about 25 minutes to about 50 minutes, from about 25 minutes to about 45 minutes, from about 25 minutes to about 40 minutes, from about 25 minutes to about 35 minutes, or from about 25 minutes to about 30 minutes.

The second time period (F2) may be from about 30 minutes to about 100 minutes, from about 30 minutes to about 95 minutes, from about 30 minutes to about 90 minutes, from about 30 minutes to about 85 minutes, from about 30 minutes to about 80 minutes, from about 30 minutes to about 75 minutes, from about 30 minutes to about 70 minutes, from about 30 minutes to about 65 minutes, from about 30 minutes to about 60 minutes, from about 30 minutes to about 55 minutes, from about 30 minutes to about 50 minutes, from about 30 minutes to about 45 minutes, from about 30 minutes to about 40 minutes, from about 30 minutes to about 35 minutes.

The second time period (T2) may be from about 35 minutes to about 100 minutes, from about 35 minutes to about 95 minutes, from about 35 minutes to about minutes, from about 35 minutes to about 85 minutes, from about 35 minutes to about 80 minutes, from about 35 minutes to about 75 minutes, from about 35 minutes to about 70 minutes, from about 35 minutes to about 65 minutes, from about 35 minutes to about 60 minutes, from about 35 minutes to about 55 minutes, from about 35 minutes to about 50 minutes, from about 35 minutes to about 45 minutes, or from about 35 minutes to about 40 minutes.

The second time period (T2) may be from about 40 minutes to about 100 minutes, from about 40 minutes to about 95 minutes, from about 40 minutes to about 90 minutes, from about 40 minutes to about 85 minutes, from about 40 minutes to about 80 minutes, from about 40 minutes to about 75 minutes, from about 40 minutes to about 70 minutes, from about 40 minutes to about 65 minutes, from about 40 minutes to about minutes, from about 40 minutes to about 55 minutes, from about 40 minutes to about 50 minutes, or from about 40 minutes to about 45 minutes.

The second time period (T2) may be from about 45 minutes to about 100 minutes, from about 45 minutes to about 95 minutes, from about 45 minutes to about 90 minutes, from about 45 minutes to about 85 minutes, from about 45 minutes to about minutes, from about 45 minutes to about 75 minutes, from about 45 minutes to about 70 minutes, from about 45 minutes to about 65 minutes, from about 45 minutes to about 60 minutes, from about 45 minutes to about 55 minutes, or from about 45 minutes to about 50 minutes.

The second time period (T2) may he from about 50 minutes to about 100 minutes, from about 50 minutes to about 95 minutes, from about 50 minutes to about 90 minutes, from about 50 minutes to about 85 minutes, from about 50 minutes to about 80 minutes, from about 50 minutes to about 75 minutes, from about 50 minutes to about 70 minutes, from about 50 minutes to about 65 minutes, from about 50 minutes to about 60 minutes, or from about 50 minutes to about 55 minutes.

The second time period (T2) may be from about 55 minutes to about 100 minutes, from about 55 minutes to about 95 minutes, from about 55 minutes to about 90 minutes, from about 55 minutes to about 85 minutes, from about 55 minutes to about 80 minutes, from about 55 minutes to about 75 minutes, from about 55 minutes to about 70 minutes, from about 55 minutes to about 65 minutes, or from about 55 minutes to about 60 minutes.

The second time period (T2) may be from about 60 minutes to about 100 minutes, from about 60 minutes to about 95 minutes, from about 60 minutes to about 90 minutes, from about 60 minutes to about 85 minutes, from about 60 minutes to about 80 minutes, from about 60 minutes to about 75 minutes, from about 60 minutes to about minutes, or from about 60 minutes to about 65 minutes.

The second time period (T2) may be from about 65 minutes to about 100 minutes, from about 65 minutes to about 95 minutes, from about 65 minutes to about 90 minutes, from about 65 minutes to about 85 minutes, from about 65 minutes to about 80 minutes, from about 65 minutes to about 75 minutes, or from about 65 minutes to about 70 minutes.

The second time period (T2) may be from about 70 minutes to about 100 minutes, from about 70 minutes to about 95 minutes, from about 70 minutes to about 90 minutes, from about 70 minutes to about 85 minutes, from about 70 minutes to about 80 minutes, or from about 70 minutes to about 75 minutes.

The second time period (T2) may be from about 75 minutes to about 100 minutes, from about 75 minutes to about 95 minutes, from about 75 minutes to about 90 minutes, from about 75 minutes to about 85 minutes, or from about 75 minutes to about 80 minutes.

The second time period (T2) may be from about 80 minutes to about 100 minutes, from about 80 minutes to about 95 minutes, from about 80 minutes to about minutes, or from about 80 minutes to about 85 minutes.

The second time period (T2) may be from about 85 minutes to about 100 minutes, from about 85 minutes to about 95 minutes, or from about 85 minutes to about 90 minutes.

The second time period (F2) may be from about 90 minutes to about 100 minutes, or from about 90 minutes to about 95 minutes.

The second time period (F2) may be from about 95 minutes to about 100 minutes.

The second time period (T2) may be about 0.1 minutes, about 0.2 minutes, about 0.3 minutes, about 0.4 minutes, about 0.5 minutes, about 1 minute, about 1.5 minutes, about 2.0 minutes, about 2.5 minutes, about 3.0 minutes, about 3.5 minutes, about 4.0 minutes, about 4.5 minutes, about 5.0 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or about 60 minutes.

The second time period (T2) may he at least about 0.1 minutes, about 0.2 minutes, about 0.3 minutes, about 0.4 minutes, about 0.5 minutes, about 1 minute, about 1.5 minutes, about 2.0 minutes, about 2.5 minutes, about 3.0 minutes, about 3.5 minutes, about 4.0 minutes, about 4.5 minutes, about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or at least about 60 minutes.

The second time period (T2) may be no more than about 0.1 minutes, about 0.2 minutes, about 0.3 minutes, about 0.4 minutes, about 0.5 minutes, about 1 minute, about 1.5 minutes, about 2.0 minutes, about 2.5 minutes, about 3.0 minutes, about 3.5 minutes, about 4.0 minutes, about 4.5 minutes, about 5 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or no more than about 60 minutes.

The first pressure, second pressure and third pressure may refer to a target pressure in the reaction vessel, and may be measured as the average pressure in the reaction vessel once a stable, or the target, pressure has been reached.

The method of the invention may include one or more additional steps. These may be performed before, simultaneously with, or after any of the above-mentioned 20 steps.

Alkalisation of the cocoa material takes place from the point of addition of the alkali solution to the reaction vessel to the point that the reaction is stopped (i.e., the reaction vessel is depressurised (to atmospheric pressure) and the alkalised cocoa powder is discharged from the reaction vessel).

Prior to step (a), the reaction vessel may be pre-heated. Advantageously, this prevents condensation forming on the interior surface of the reaction vessel during the first pressure step (step (c)) which would increase the drying time. The reaction vessel may be pre-heated to a jacket temperature greater than 100°C. The jacket temperature relates to the temperature of a reactor jacket which at least partially, preferably considerably, surrounds the reaction vessel and is therefore capable of heating (or cooling) the contents of the reaction vessel by permitting the uniform exchange of heat between the heating/cooling means in the jacket (for example, fluid circulating in the jacket) and the wall( s) of the reaction vessel.

The cocoa powder added to the reaction vessel in step (a) may he derived from the group consisting of: cocoa nib, for example ground cocoa nib, cocoa shell, partially alkalised cocoa powder, cocoa fibre, carob pod, carob pod pulp, roasted carob pod, and combinations thereof.

After step (a), but before step (b), the sample of cocoa powder in the reaction vessel may he mixed under heating. The sample of cocoa powder may be heated to a temperature of from about 50°C to about 100°C, from about 60°C to about 90°C, from about 70°C to about 80°C, or about 75°C. The temperature may refer to the target temperature of the cocoa powder, and may be measured as the average temperature of the cocoa powder once a stable temperature has been reached. The sample of cocoa powder in the reaction vessel may he mixed under heating for a period of at least 3 minutes, preferably about 3 to about 10 minutes. Advantageously, mixing and heating the sample of cocoa powder prevents, or at least significantly reduces, the formation of agglomerates of cocoa powder, the formation of which could have a detrimental effect on the efficiency of the alkalisation reaction.

The cocoa powder may be heated using any means available to the skilled person. For example, the cocoa powder may be heated by injection into the reaction vessel of hot air or steam, and/or through contact heating, e.g., with a heated reaction vessel jacket to transfer heat to the reaction vessel walls.

Step (b) may comprise mixing of the alkali solution and the cocoa powder under heating. The mixture of cocoa powder and alkali solution may be mixed under a temperature of from about 70°C to about 100°C, or from about 80°C to about 90°C.

Advantageously, mixing ensures that the alkali solution is well dispersed across the cocoa powder.

The mixing may be continuous mixing for the duration of the alkalisation reaction. The alkalisation reaction may begin at the point the alkali solution is added to the reaction vessel and, therefore, to the cocoa powder.

In step (c), the gas may be steam. Advantageously, steam increases the moisture content of the alkali solution and cocoa powder reaction mixture which facilitates the colour-producing reactions in the cocoa powder. Thus, the alkalisation reaction can produce an alkalised cocoa powder with a more intense, dark colour of cocoa powder.

Step (a), (b), (c), (d) and/or (e) may take place without a continuous air flow.

Step (a), (b), (c), (d) and/or (e) may take place with an air flow of less than about 15 rn3/hr, about 14 m3/hr, about 13 m'/hr, about 12 m3/hr, about 11 rn3/hr, about 10 m3/hr, about 9 m3/hr, about 8 m3/hr, about 7 m3/hr, about 6 m3/hr, about 5 m3/hr, about 4 m3/hr, about 3.5 m3/hr, about 3 m3/hr, about 2.5 m3/hr, about 2 m3/hr, about 1.5 m3/hr, about 1 m3/hr, about 0.5 m3/hr, less than about 0.2 m3/hr, or less than about 0.1 m3/hr.

By "continuous air flow" it is meant that air, or any other suitable gas (e.g., oxygen-enriched air or nitrogen), is able to enter and exit the reaction vessel. In the prior art, it is typical that substantially for the duration of the reaction (i.e., from the point of addition of the alkalizing agent), the reaction is carried out under continuous air flow at a substantially constant flow rate.

In step (d), the gas may be released from the reaction vessel by venting the gas out of the vessel such that the pressure (P2) in the reaction vessel is less than the first pressure (P1) and the third pressure (P3). The second pressure (P2) may he atmospheric pressure. Step (d) may he a reaction vessel depressurisation step.

Step (e) may be carried out under continuous air flow. The continuous air flow may he at a flow rate of from about 30 m3/hr to about 70 m3/hr, from about 35 m3/hr to about 65 m3/hr, from about 40 rn3/hr to about 60 m3/hr, from about 45 m3/hr to about 55 m3/1n, or about 50 rn3/hr.

The continuous air flow may be at a flow rate of from about 30 m3/hr to about 70 m3/hr, from about 30 m3/hr to about 65 m3/hr, from about 30 m3/hr to about 60 m3/hr, from about 30 m3/hr to about 55 m3/hr, from about 30 m3/hr to about 50 m3/hr, from about 30 m3/hr to about 45 m3/hr, from about 30 m3/hr to about 40 m3/hr, or from about 30 1113/hr to about 35 m3/hr.

The continuous air flow may be at a flow rate of from about 35 m3/hr to about 30 70 m3/hr, from about 35 tn3/hr to about 65 m3/hr, from about 35 m3/hr to about 60 m3/hr, from about 35 m3/hr to about 55 m3/hr, from about 35 m3/hr to about 50 m3/hr, from about 35 m3/hr to about 45 m3/hr, or from about 35 m3/hr to about 40 m3/hr.

The continuous air flow may be at a flow rate of from about 40 m3/hr to about 70 m3/hr, from about 40 m3/hr to about 65 m3/hr, from about 40 m3/hr to about 60 m3/hr, 5 from about 40 m3/hr to about 55 m3/hr, from about 40 m3/hr to about 50 m3/hr, or from about 40 m3/hr to about 45 m3/hr.

The continuous air flow may be at a flow rate of from about 45 m3/hr to about 70 m3/hr, from about 45 m3/hr to about 65 m3/hr, from about 45 m3/hr to about 60 m3/hr, from about 45 m3/hr to about 55 m3/hr, or from about 45 m3/hr to about 50 m3/hr.

The continuous air flow may be at a flow rate of from about 50 m3/hr to about m3/hr, from about 50 m3/hr to about 65 m3/hr, from about 50 m3/hr to about 60 m3/hr, or from about 50 m3fhr to about 55 m3fhr.

The continuous air flow may be at a flow rate of from about 55 m3/hr to about 70 m3/hr, from about 55 m3/hr to about 65 m3/hr, or from about 55 m3/hr to about 60 15 m3/hr.

The continuous air flow may be at a flow rate of from about 60 m3/hr to about 70 m3/hr, or from about 60 m3/hr to about 65 m3/hr.

The continuous air flow may be at a flow rate of from about 65 m3/hr to about 70 m3/hr.

The continuous air flow may be at a flow rate of about 1.0 m3/hr, about 1.5 m3/hr, about 2 m3/hr, about 2.5 m3/hr, about 3.0 m3/hr, about 3.5 m3/hr, about 4.0 m3/hr, about 4.5 m3/hr, about 5.0 m3/hr, about 5.5 m3/hr, about 6.0 m3/hr, about 6.5 m3/hr, about 7.0 m3/hr, about 7.5 m3/hr, about 8.0 m3/hr, about 8.5 m3/hr, about 9.0 m3/hr, about 9.5 m3/hr, or about 10.0 m3/hr.

The continuous air flow may be at a flow rate of less than about 1.0 m3/hr, about 1.5 m3/hr, about 2 m3/hr, about 2.5 m3/hr, about 3.0 m3/hr, about 3.5 m3/hr, about 4.0 m3/hr, about 4.5 m3/hr, about 5.0 m3/hr, about 5.5 m3/hr, about 6.0 m3/hr, about 6.5 m3/hr. about 7.0 m3/hr. about 7.5 m3/hr, about 8.0 m3/hr, about 8.5 m3/hr, about 9.0 m3/hr, about 9.5 m3/hr, or less than about 10.0 m3/hr.

The continuous air flow may he at a flow rate of from about 1.0 m3/hr to about 10.0 m3/hr, from about 3.0 m3/hr to about 7.0 m3/hr, or about 5.0 rn3/hr.

The continuous air flow may be at a flow rate of from about 1 m3/hr to about 10.0 m3/hr, from about 1.0 m3/hr to about 9.0 m3/hr, from about 1.0 m3/hr to about 8.0 m3/hr, from about 1.0 m3/hr to about 7.0 m3/hr, from about 1.0 rn3/hr to about 6.0 rn3/hr, from about 1.0 m3/hr to about 5.0 m3/hr, from about 1.0 m3/hr to about 4.0 m3/hr, from about 1.0 m3/hr to about 3.0 m3/hr, or from about 1.0 m3/hr to about 2.0 m3/hr.

The continuous air flow may be at a flow rate of from about 2.0 m3/hr to about 10.0 m3/hr, from about 2.0 m3/hr to about 9.0 m3/hr, from about 2.0 m3/hr to about 8.0 m3/hr, from about 2.0 m3/hr to about 7.0 m3/hr, from about 2.0 m3/hr to about 6.0 m3/hr, from about 2.0 m3/hr to about 5.0 m3/hr, from about 2.0 m3/hr to about 4.0 m3/hr, or from about 2.0 m3/hr to about 3.0 m3/hr.

The continuous air flow may be at a flow rate of from about 3.0 m3/hr to about 10.0 m3/hr, from about 3.0 m3/hr to about 9.0 m3/hr, from about 3.0 m3/hr to about 8.0 m3/hr, from about 3.0 m3/hr to about 7.0 m3/hr, from about 3.0 m3/hr to about 6.0 m3/hr, from about 3.0 m3/hr to about 5.0 m3/hr, or from about 3.0 m3/hr to about 4.0 m3/hr.

The continuous air flow may be at a flow rate of from about 4.0 m3/hr to about 10.0 m3/hr, from about 4.0 m3/hr to about 9.0 m3/hr, from about 4.0 m3/hr to about 8.0 m3/hr, from about 4.0 m3/hr to about 7.0 m3/hr, from about 4.0 m3/hr to about 6.0 m3/hr. 20 or from about 4.0 m3/hr to about 5.0 m3/hr.

The continuous air flow may be at a flow rate of from about 5.0 m3/hr to about 10.0 m3/hr, from about 5.0 m3/hr to about 9.0 m3/hr, from about 5.0 m3/hr to about 8.0 m3/hr, from about 5.0 rn3/hr to about 7.0 m3/hr, or from about 5.0 rn3/hr to about 6.0 m3/hr.

The continuous air flow may be at a flow rate of from about 6.0 m3/hr to about 10.0 m3/hr, from about 6.0 m3/hr to about 9.0 m3/hr, from about 6.0 m3/hr to about 8.0 m3/hr, or from about 6.0 m3/hr to about 7.0 m3/hr.

The continuous air flow may be at a flow rate of from about 7.0 m3/hr to about 10.0 m3/hr, from about 7.0 m3/hr to about 9.0 m3/hr, or from about 7.0 m3/hr to about 8.0 m3/hr.

The continuous air flow may he at a flow rate of from about 8.0m3/hr to about 10.0 m3/hr, or from about 8.0 m3/hr to about 9.0 m3/hr.

The continuous air flow may be at a flow rate of from about 9.0 m3/hr to about 10.0 m3/hr.

Advantageously, it has been found that a flow rate of from about 1.0 m3/hr to about 10.0 rn3/hr or 30 m3/hr to about 70 m3/hr can favourably impact the colour of the alkalised cocoa powder to produce a darker-coloured alkalised cocoa powder. Advantageously, it is believed that carrying out step (e) under continuous air flow produces a suitably dark-coloured alkalised cocoa powder with intense flavour, and relatively low pH. As such, these properties of an alkalised cocoa powder can be produced without requiring the entirety of the alkalisation reaction to be carried out under continuous air flow or for a higher concentration of alkali agent to be used.

After step (e). the method may comprise a further step, step (f). Step (f) may comprise venting air out of the reaction vessel to return the pressure in the reaction vessel to atmospheric pressure.

After step (f), the method may comprise a further step, step (g). Step (g) may comprise applying a vacuum to the reaction vessel. Advantageously, the vacuum may remove moisture in the reaction vessel. The vacuum may he discontinued, and a sample of alkalised cocoa powder taken by an operator to measure the moisture content of the alkalised cocoa powder. If the moisture content is too high (for example, above 5% moisture content), the operator may reapply the vacuum to remove further moisture. When applying the vacuum, it is favourable to apply a slow ramp step to prevent particles of alkalised cocoa powder being drawn into vent lines, or similar, of the reaction vessel.

Step (g) may comprise applying a vacuum to the reaction vessel to reduce the moisture content in the alkalised cocoa powder to no more than about 5 wt.%, about 4 wt.%, about 3 wt.%, about 2 wt.%, or no more than about 1 wt.%, based on the weight of the alkalised cocoa powder.

Step (g) may comprise applying a vacuum to the reaction vessel to reduce the moisture content in the alkalised cocoa powder to from about 1 wt.% to about 5 wt.%, from about 1 wt.% to about 4 wt.%, from about 1 wt.% to about 3 wt.%, from about 1 wt.% to about 2 wt.%, based on the weight of the alkalised cocoa powder.

Step (g) may comprise applying a vacuum to the reaction vessel to reduce the moisture content in the alkalised cocoa powder to from about 2 wt.% to about 5 wt.%, 5 from about 2 wt.% to about 4 wt.%, or from about 2 wt.% to about 3 wt.%, based on the weight of the alkalised cocoa powder.

Step (g) may comprise applying a vacuum to the reaction vessel to reduce the moisture content in the alkalised cocoa powder to from about 3 wt.% to about 5 wt.%, or from about 3 wt.% to about 4 wt.%, based on the weight of the alkalised cocoa 10 powder.

Step (g) may comprise applying a vacuum to the reaction vessel to reduce the moisture content in the alkalised cocoa powder to from about 4 wt.% to about 5 wt.%, based on the weight of the alkalised cocoa powder.

After step (g), the method may comprise a further step, step (h). Step (h) may comprise cooling the alkalised cocoa powder by passing cool water through a reactor jacket at least partially, preferably considerably, surrounding the reaction vessel. Advantageously, this prevents the risk of discharging the alkalised cocoa powder at an elevated temperature which may cause harm to the operator.

After step (h), the method may comprise a further step, step (i). Step (i) may comprise discharging or emptying the reaction vessel of the alkalised cocoa powder.

The alkalised cocoa powder may be in a compacted form. As such, after step (i), the method may comprise a further step, step (j). Step (j) may comprise grinding (or milling) the compacted alkalised cocoa powder to reduce the particle size of the alkalised cocoa powder. A classifying mill, for example a jet mill or other dry mill, may be used to grind, or mill, the compacted alkalised cocoa powder.

Advantageously, the alkalised cocoa powder of the present invention may be used in the manufacture of food and beverage compositions.

Thus, according to a third aspect of the invention, there is provided a food or beverage composition comprising the alkalised cocoa powder of the first aspect.

The food or beverage composition may he a food or beverage product. The food or beverage product may be selected from the group consisting of: milk, dark, and white chocolate and compound compositions (for use, amongst others, in confectionary, as bars, in truffles and pralines, or as inclusions, coatings, or fillings), drinking chocolate, flavoured milks (dairy and non-dairy), flavoured syrups, a baked products, a farinaceous product diet bars and meal substitutes, sports and infant nutrition, ice-cream products, dairy products, puddings, mousses, sauces, breakfast cereals or any combination thereof.

The baked product. may be selected from the group consisting of: a cookie, a biscuit, a pie, a cake, bread, pastry or any combination thereof.

The farinaceous product may be selected from the group consisting of: a baked product as defined hereinabove, dough, batter or any combination thereof.

The invention according to any aspect may include any of the features, optional or otherwise, of the invention according to any other aspect.

Detailed Description of the Invention

hi order that the invention may be more clearly understood one or more embodiments thereof will now he described, by way of example only, with reference to the accompanying drawings, of which: Figure 1 is a schematic block diagram of a process according to an embodiment of the present invention; and Figure 2 is a graph showing the pressure in the reaction vessel against time for a method for preparing an alkalised cocoa powder according to an embodiment of the present invention.

Referring to the Figures, a sample of cocoa powder 1 may be initially selected.

In this embodiment, the sample of cocoa powder is natural cocoa powder obtained from cocoa nib.

The sample of cocoa powder 1 may be added to a bulk handling system 101.

An alkali agent 2 may then be selected. In this embodiment, the alkali agent is potassium carbonate. A quantity of water 3 may be added to the alkali agent 2 to form an alkali solution. In this embodiment, the alkali solution comprises the alkali agent 2 in a concentration of from 4 wt.% to 5 wt.%. The alkali solution may be added to an alkali solution tank 102.

At step 201, a reaction vessel 200 may he pre-heated to a temperature of greater than 100°C.

At step 202, the cocoa powder 1 may be added to the reaction vessel 200 by transferring the cocoa powder 1 from the bulk handling system 101 to the reaction vessel 200. In the reaction vessel 200, the cocoa powder 1 may be mixed whilst under heating. The cocoa powder 1 may be mixed for a period of from about 3 minutes to about 10 minutes under heating to a temperature of about 75°C.

At step 203, the alkali solution may be added to the reaction vessel 200 from the alkali solution tank 102 to begin alkalisation of the cocoa powder. In this embodiment, once the alkali solution is added to the reaction vessel 200, the cocoa powder and alkali solution mixture comprises cocoa powder in an amount of about 80 wt.%, potassium carbonate in an amount of about 5 wt.%, and water in an amount of about 15 wt.%, each based on the total weight of the cocoa powder and alkali solution mixture. The mixture may be mixed under heating to a temperature of from about 80°C to about 90°C.

At step 204, steam 4 may be injected into the reaction vessel 200. An amount. of steam 4 sufficient to increase the pressure in the reaction vessel 200 to a first pressure (P1) of from approximately 6.0 bara to approximately 7.0 bara may be injected into the reaction vessel 200. The pressure may be increased from approximately atmospheric pressure to the first pressure (P1) over the course of about 18 minutes. The first pressure (P1) may be held for a first time period (T1) of about 30 minutes.

At step 205, the reaction vessel 200 may be depressurised from the first pressure (P1) to a second pressure (P2). In this embodiment, the second pressure (P2) is from approximately 1.0 bara to approximately 1.5 barn. The pressure in the reaction vessel may he decreased from the first pressure (P1) to the second pressure (P2) over the course of about 40 minutes.

Depressurisation of the reaction vessel 200 may include ejection of steam and volatile components 304 from the reaction vessel 200.

At step 206, air 5 may he injected into the reaction vessel 200 to aerate the reaction vessel 200. Aeration of the reaction vessel 200 may increase the pressure in the reaction vessel 200 to a third pressure (P3). An amount of air 5 may be injected into the reaction vessel 200 to increase the pressure to a third pressure (P3) of from about 3.0 Kara to about 4.0 Kara. The pressure may be increased from the second pressure (P2) to the third pressure (P3) over the course of about 10 minutes. The third pressure (P3) may be held for a third time period (T3) of about 60 minutes.

In this embodiment, step 206 is carried out under continuous air flow. The continuous air flow may be at a rate of from about 40 m3/hr to about 60 m3/hr.

The first pressure (P1) may he about two times the third pressure (P3).

At step 207, the reaction vessel 200 may be depressurised from the third pressure (P3) to a vacuum. The pressure in the reaction vessel 200 may be decreased from the third pressure (P3) to the vacuum over the course of about 10 minutes.

Depressurisation of the reaction vessel 200 may include ejection of water, air and volatile components 306 from the reaction vessel 200 and, upon application of the vacuum, water and volatile components 307 may he ejected from the reaction vessel into a vacuum system. The alkalised cocoa powder may be dried, under vacuum, for 30 to 50 minutes.

At step 208, the reaction vessel may he cooled by passing cold water through a reactor jacket surrounding, or at least partially surrounding, the reaction vessel 200. At step 208, the mixture within the reaction vessel (i.e., the alkalised cocoa powder) may be cooled to a temperature of below 80°C.

Steps 202, 203, 204, 205, 206, 207 and 208 may be carried out under continuous At step 209, alkalised cocoa powder 308 may he discharged from the reaction vessel 200. The alkalised cocoa powder 308 may be in a compacted and abrasive form.

At step 210, the alkalised cocoa powder 308 may be ground to reduce the particle size of the alkalised cocoa powder 308. In this embodiment, an air classifier mill may be used to grind the compacted alkalised cocoa powder 308. The resultant alkalised cocoa powder 308 may he an alkalised cocoa powder according to the invention.

The one or more embodiments are described above by way of example only. Many variations are possible without departing from the scope of protection afforded 10 by the appended claims.

Examples

Three Examples of alkalised cocoa powder were prepared.

In Example 1, an alkalised cocoa powder was prepared representing a small-scale batch and using a 100 wt.% solution of potassium carbonate.

In Example 2, an alkalised cocoa powder was prepared representing a small-scale batch and using a 50 wt.% solution of potassium carbonate.

In Example 3, an alkalised cocoa powder was prepared representing a large-scale batch and using a 50 wt.% solution of potassium carbonate.

The respective quantities of cocoa powder, potassium carbonate and water used in the described Examples are provided in Tables 1-3.

Table 1 -Example 1

Ingredient Recipe Initial solution Quantities to Final solution Added water concentration add needed ratio Unit 1%1 [%] [kg] [kg] [%] Cocoa 79.37% - 25.00 - -Potassium carbonate from initial solution (100%) 4.76% 100.00% 1.50 6.50 23% Water from initial solution (0%) 15.87% 0.00% Water - 5.00 77% Total 100.00% 100.00% 31.50 6.50 100.00%

Table 2 -Example 2

Ingredient Recipe Initial solution Quantities to Final solution Added water concentration add needed ratio Unit [%] [%] [kg] [kg] [%] Cocoa 79.37% 25.00 Potassium carbonate from initial solution (50%) 4.76% 50.00% 3.00 6.50 46% Water from initial solution (50%) 15.87% 50.00% Water 3.50 54% Total 100.00% 100.00% 31.50 6.50 100,00%

Table 3 -Example 3

Ingredient Recipe Initial solution Quantities to Final solution Added water concentration add needed ratio Unit [Yo] [%] [kg] [kg] [%] Cocoa 79.37% 300.00 Potassium carbonate from initial solution (50%) 4.76% 50.00% 36.00 78.00 46% Water from initial solution (50%) 15.87% 50.00% Water 42.00 54% Total t\-) 10031p% 100.00% 5 378.00 78.00v, 100.00% c The operating parameters in respect of each of Examples 1 -3 are specified in Table 4, below.

Table 4

Pre-heat jacket temperature 161°C Time to first pressure 18 minutes First pressure approximately 6.0 -7.0 bara Duration at first pressure 30 minutes Time to second pressure 40 minutes Second pressure approximately 1.0 -1.5 bara Duration at second pressure 1.0 minute Time to third pressure 18 minutes Third pressure approximately 3.0 -4.0 bara Duration at third pressure 60 minutes Air flow during third pressure 5.0 m3/hr Time to vacuum 10 minutes Alkalised cocoa powders according to the invention were prepared by following the method detailed below and in Table 4.

A reaction vessel was pm-heated to 161°C by supplying steam to a pipe network within a jacket surrounding considerably all of the reaction vessel. Once the pre-heat temperature was reached, a sample of cocoa powder was added from a bulk handling system to the reaction vessel. The cocoa powder was stirred (60 rpm) in the reaction vessel and the pre-heat temperature maintained.

Separately, an alkali solution was formed by adding a solution of potassium carbonate to water. The concentration of potassium carbonate in the alkali solution was 4.76 % (total potassium carbonate equivalent in grams (% fat free dry matter). The alkali solution was obtained from Brenntag SE, based in Germany.

A solution of potassium carbonate (23.08 wt.%) was added to the reaction vessel under continuous stirring (60 rpm). The reaction vessel was then closed and pressurised using steam (about 159°C) injected into the reaction vessel to initiate a first pressure of 6.0 bara. The pressure in the reaction vessel was increased from atmospheric pressure to 6.0 bara over the course of 18 minutes. The pressure of 6.0 bara was maintained, notwithstanding relatively minor fluctuations, for 30 minutes. During this time, the temperature of the cocoa powder and alkali solution mixture increased to approximately 160°C.

The reaction vessel was then depressurised by ejecting (or venting) steam and volatile components out of the reaction vessel. The start of the depressurisation of the reaction vessel indicated the completion of the duration of the first pressure. The reaction vessel was depressurised to a second pressure of 1.5 bara over the course of 40 minutes, during which the temperature of the reaction vessel jacket was reduced to approximately 120°C. The pressure was held at 1.5 bara for 1 minute.

The reaction vessel was then pressurised using compressed air, to initiate a third pressure of 3.0 bara, and the temperature of the reaction vessel jacket decreased to about 95°C. The pressure in the reaction vessel was increased from 1.5 bara to 3.0 bara over the course of 18 minutes. The pressure of 3.0 bara was maintained, notwithstanding relatively minor fluctuations, for 60 minutes. When the increase of pressure to the third pressure was initiated, an air flow was introduced into the reaction vessel. The air flow was continued for the duration of the 60-minute period at which the pressure in the reaction vessel was at 3.0 bara. The air flow was at a rate of 5.0 m3/hr.

The reaction vessel was then depressurised by applying a vacuum to the reaction vessel, indicating the completion of the period of the third pressure and completion of the alkalisation reaction. Water, air and volatile components were ejected (or vented) out of the reaction vessel into a vacuum system. The reaction vessel was depressurised from the pressure of 3.0 bara to a vacuum (approximately -1.0 bara) over the course of 10 minutes. Application of the vacuum removed moisture from the alkalised cocoa powder and, therefore, dried the alkalised cocoa powder. The alkalised cocoa powder was dried, under vacuum, for 40 minutes.

The cocoa powder and alkali solution mixture was continuously stirred (or mixed) throughout the alkalisation reaction.

Once the vacuum was released, cold water was passed through the reactor jacket to cool the alkalised cocoa powder to no more than 75°C.

The alkalised cocoa powder was then discharged from the reaction vessel. The alkalised cocoa powder was in the form of a hard, compacted cake and so was ground using a classifying mill to reduce its particle size.

The colour L-value, pl-I, D90, ash content, sodium content and potassium content were measured as described herein, and the results shown in Table 5.

I0 Table 5

Colour pH fat fineness D90 ash Sodium Potassium (*L wt.% (% < 75pm, sieve) (pm) wt.% (mg/100g) (mg/100g) GRTM307) 21.3 -26.0 6.10 10 - 99.5 35 14 32 4590 - 12 6.65 Further Examples of alkalised cocoa powder were prepared.

The operating parameters in respect of each of Examples 4 -II are specified in Table 6, below.

Alkalised cocoa powders according to the invention were prepared by following the method detailed below and in Table 6.

A reaction vessel was pre-heated by supplying steam to a pipe network within a jacket surrounding considerably all of the reaction vessel. Once the pre-heat jacket temperature was reached, a sample of cocoa powder was added from a bulk handling system to the reaction vessel. Stirring was then initiated (60 rpm) and the pre-heat temperature maintained.

Separately, an alkali solution was formed by adding a solution of potassium carbonate to water. The alkali solution was obtained from Brenntag SE, based in Germany, and this solution was diluted to give a solution of potassium carbonate having a potassium carbonate concentration of 23.08%.

The alkali solution was added to the reaction vessel under continuous stirring (60 rpm). The reaction vessel was then closed and pressurised using steam injected into the reaction vessel to initiate a first pressure. The pressure in the reaction vessel was increased from atmospheric pressure to the first pressure over the course of a 'time to first pressure', as indicated for each Example in Table 6. The first pressure was maintained, notwithstanding relatively minor fluctuations, for a 'duration at first pressure', as indicated for each Example in Table 6.

The reaction vessel was then depressurised by ejecting (or venting) steam and volatile components out of the reaction vessel. The start of the depressurisation of the reaction vessel indicated the completion of the duration of the first pressure. The reaction vessel was depressurised to a second pressure of 1.5 tiara over the course of a time to second pressure', as indicated in Table 6, during which the temperature of the reaction vessel jacket was reduced to approximately 120°C. The second pressure was held at 1.5 ban for 1 minute The reaction vessel was then pressurised, over the course of a 'time to third pressure' as indicated in Table 6, using compressed air (at a 'temperature of air added for P3' as indicated in Table 6) to initiate a third pressure. The temperature of the reaction vessel jacket was decreased to a 'jacket temperature at P3' as indicated in Table 6. The third pressure was maintained, notwithstanding relatively minor fluctuations, for a 'duration at third pressure', as indicated in Table 6. When the increase of pressure to the third pressure was initiated, an air flow was introduced into the reaction vessel.

The air flow was maintained for the 'duration at third pressure'.

The reaction vessel was then depressurised by applying a vacuum to the reaction vessel, indicating the completion of the period of the third pressure and completion of the alkalisation reaction. Water, air and volatile components were ejected (or vented) out of the reaction vessel into a vacuum system. The reaction vessel was depressurised from the third pressure to a vacuum (approximately -1.0 tiara) over the course of about minutes. Application of the vacuum removed moisture from the alkalised cocoa powder and, therefore, dried the alkalised cocoa powder. The alkalised cocoa powder was dried, under vacuum, for a 'time at vacuum after third pressure', as indicated in Table 6.

The alkalised cocoa powder was then discharged from the reaction vessel. The 10 alkalised cocoa powder was in the form of a hard, compacted cake and so was ground using a classifying mill to reduce its particle size.

Table 6

Example Added Fat content Batch size (kg) Alkali Water K2CO3 (g) K2CO3 Total K2CO3 K2CO3 cocoa (%) batch (g) batch (g) Equivalent solution (%) powder (kg) in g (% FFDM) 4 25.00 11.0 25.0 Potassium 5000.0 600.0 1500.0 6.94 23.08 carbonate 25.00 11.0 25.0 Potassium 5000.0 600.0 1500.0 6.94 23.08 carbonate 6 25.00 11.0 25.0 Potassium 5000.0 600.0 1500.0 6.94 23.08 carbonate 7 10.00 11.0 10.0 Potassium 2000.0 600.0 600.0 6.94 23.08 carbonate 8 10.00 11.0 10.0 Potassium 2000.0 600.0 600.0 6.94 23.08 carbonate 9 10.00 11.0 10.0 Potassium 2000.0 600.0 600.0 6.94 23.08 carbonate 10.00 11.0 10.0 Potassium 2000.0 600.0 600.0 6.94 23.08 carbonate 11 10.00 11.0 10.0 Potassium 2000.0 600.0 600.0 6.94 23.08 carbonate

C

Table 6

Example Pre-heat Temperature Time to First Duration Time to Second Duration at jacket of steam first pressure at first second pressure second temperat added for P1 pressure (bara) pressure pressure (bara) pressure ure (°C) (°C) (min) (minutes) (minutes) (minutes) 4 166.0 158.9 7.0 6.00 15.0 7.0 1.50 1.0 166.0 158.9 7.0 6.00 15.0 7.0 1.50 1.0 6 165.9 158.9 7.0 6.00 15.0 7.0 1.50 1.0 7 165.9 158.9 7.0 6.00 15.0 7.0 1.50 1.0 8 165.9 158.9 7.0 6.00 15.0 7.0 1.50 1.0 9 166.0 158.9 7.0 6.00 45.0 7.0 1.50 1.0 166.0 158.9 7.0 6.00 15.0 7.0 1.50 1.0 11 166.0 158.9 7.0 6.00 15.0 7.0 1.50 1.0

C

N..) U)

C

Table 6

Example Time to Jacket Temperature Third Duration at Air flow Time at pH of Colour L-value Sodium third temperat of air added pressure third pressure during third vacuum after alkalised (mg/100 pressure ure at P3 for P3 (°C) (bara) (minutes) pressure third pressure cocoa g) (minutes) (°C) (m3/hr) (minutes) powder 4 16.0 95.0 100.0 5.00 60.0 5.0 30.0 6.60 26.42 19.10 16.0 95.0 125.0 5.50 30.0 5.0 44.0 6.50 26.04 11.20 6 16.0 95.0 100.0 5.00 60.0 5.0 30.0 6.65 26.04 11.20 7 16.0 95.0 100.0 5.00 60.0 4.5 30.0 6.65 24.10 20.45 8 16.0 95.0 100.0 5.00 60.0 3.0 30.0 6.60 23.70 15.25 9 16.0 95.0 150.0 4.00 60.0 >1.5 30.0 6.50 24.12 25.65 16.0 95.0 125.0 5.00 60.0 >1.5 30.0 6.50 24.95 17.90 11 16.0 95.0 100.0 6.00 30.0 5.0 30.0 6.35 25.16 26.55 Added water (g)' refers to the quantity of water added in a 10kg hatch equivalent.

Water batch (g)' refers to the actual quantity of water added for the respective hatch size.

'K2CO3 (g)' refers to the quantity of potassium carbonate added in a 10kg batch equivalent.

K2CO3 batch (g)' refers to the actual quantity of potassium carbonate added for the respective batch size.

Surprisingly, it has been found that the method for preparing an alkalised cocoa powder according to the invention produces an alkalised cocoa powder having a pH of from 6.10 to 6.65, which is relatively low (i.e., not as alkaline) compared to the pH of known alkalised cocoa powders.

Notably, the alkalised cocoa powder does not exhibit an undesirable powdery taste and mouthfeel as is common with alkalised cocoa powders having a pH of above about 6.65, for example pH 6.70 or above, as is found in the prior art. Further, the alkalised cocoa powder of the invention does not possess an unpleasant alkali flavour or odour due to it having a pH of from about 6.10 to about 6.65.

Notably, as shown in the Examples, the alkalised cocoa powder may have a colour L-value such that the alkalised cocoa powder has a darker colour.

Advantageously, the alkalised cocoa powder of the invention is therefore suitable for producing a food or beverage product having a tailored, dark colour profile without providing an undesirable alkaline flavour profile.

Thus, it is notable that the alkalised cocoa powder of the present invention may he used on its own or mixed with other cocoa powders, for example non-alkalised cocoa powders, to produce food and beverage products with tailored colour and flavour profiles. Advantageously, the alkalised cocoa powder can be used to decrease costs or increase cost margins, since smaller quantities of the alkalised cocoa powder can be used to achieve the same colour impact as larger quantities of standard, non-alkalised cocoa powders.

As shown in Examples 1-3, it is advantageous that the alkalised cocoa powder of the invention has a D90 value of less than about 50 pm (i.e., 35 pm). This is because the alkalised cocoa powder therefore comprises particles which are easily solubilised by a fluid, for example water, for example when the alkalised cocoa powder is being used to form a cocoa beverage or cocoa butter. As such, the resultant product (for example a cocoa beverage or cocoa butter) does not provide undesirable 'sandy' texture and taste properties which are objectionable to the consumer.

Notably, the alkalised cocoa powder of Examples 1-3 has an ash content of about 14 wt.%, which is a relatively low ash content compared to alkalised cocoa powders of the prior art. As such, the alkalised cocoa powder of the invention may comprise a relatively low concentration of minerals and, therefore, a higher concentration of cocoa. Further, the ash content of the alkalised cocoa powder is such that the alkalised cocoa powder is not 'over-alkalised' which may result in a detrimental and off-putting flavour and texture for a consumer. Instead, advantageously, the ash content of the invention provides for a stronger cocoa flavour of the alkalised cocoa powder which is favourable to a consumer.

Notably, the potassium content and sodium content of the alkalised cocoa powder of the invention as shown in the Examples 1-3, and Examples 4-11 in respect of sodium content, provide individual and synergistic health benefits to the consumer.

Advantageously, the potassium content of 4590 mg/1008 and sodium content of 32 mg/100g can result in a product which provides health benefits to a consumer compared to a product formed of a cocoa powder having a sodium content of greater than 150 mg/100g or a product of low potassium content.

Surprisingly, as shown with the Examples, the method of the invention provides a desirable alkalised cocoa powder which comprises a sodium content no greater, or at least not significantly greater, than the sodium content of natural cocoa. Advantageously, therefore, the alkalised cocoa powder does not require the addition of sodium to provide desirable flavour notes to the consumer. This is particularly advantageous with respect to marketing the alkalised cocoa powder as it can be labelled and marketed as having no sodium added to it, making the product more appealing to consumers.

Further, the Examples of the alkalised cocoa powder of the invention are prepared using one or more alkalis which do not comprise ammonia-based alkalis which are commonly used in the prior art. As such, the alkalised cocoa powder of the invention may avoid the toxic and volatile properties associated with ammonia-based compounds used in preparing known alkalised cocoa powders, while exhibiting a darker colour as is desired.

Surprisingly, the present invention provides for an alkalised cocoa powder having a relatively low pH, which is sufficiently alkalised to provide desirable colour and flavour profiles, without the use of relatively strong ammonium-based alkalis, and without the use of large quantities of a sodium-based alkali, for example sodium hydroxide, which is often used in the prior art as a substitute for strong ammonium-based alkalis, or to supplement strong ammonium-based alkalis.

Notably, the alkalised cocoa powder of the invention may be prepared without the need to use ammonia-based alkalis and without requiring significant quantities of comparatively weaker alkalis, such as sodium-based alkalis, for example sodium hydroxide. As such, the method of preparing the alkalised cocoa powder may avoid the toxic and volatile properties of ammonia-based alkalis which are disadvantageous for the environment and disadvantageous for operator handling in respect of the preparation of the alkalised cocoa powder. Moreover, the method of preparing the alkalised cocoa powder of the invention may avoid using weaker alkalis, such as sodium-based alkalis, for example sodium hydroxide, in significant quantities, as is common in the art. Such methods employing significant quantities of comparably weaker alkalis are disadvantageous in terms of the cost of manufacture and the handling and processing of such large quantities of alkali, and in respect of the subsequent difficulties faced by operators in obtaining desired flavour and organoleptic profiles of the alkalised cocoa powder.

Further, it is advantageous that the method parameters of the invention, in particular the first pressure value and the third pressure value, can he adjusted, as required, to produce an alkalised cocoa powder with tailored properties in respect of colour L-value, pH, sodium content and D90 value, as desired.

Beneficially, as shown in the Examples, such favourable, tailored alkalised cocoa powders may be produced without the aforementioned disadvantageous properties associated with using ammonia-based alkalis. As such, the alkalised cocoa powders find particular benefit as its own product or mixed with other cocoa powders, for example non-alkalised cocoa powders, to produce food and beverage products with tailored colour and flavour profiles. Advantageously, the alkalised cocoa powder may therefore be used to decrease costs or increase cost marains_ since smaller quantities of the alkalised cocoa powder can he used to achieve the same, or at least similar, colour impact as larger quantities of standard, non-alkalised cocoa powders.

It should he noted that adjusting the first pressure value and/or third pressure value of the method of the invention may be carried out simply and at minimal cost to the overall method of preparing an alkalised cocoa powder. Thus, advantageously, properties of the alkalised cocoa powder produced by the method of the invention, such as colour L value, sodium content, pH and D90 value, can be tailored, as desired, with relative ease and at minimal cost. In comparison, disadvantageously, known methods of the prior art typically require wholesale changes to the method for producing alkalised cocoa powder, including use of different alkali or combinations of alkali, use of significantly greater quantities of alkali, or significant changes to temperature and periods of pressure, in order to tailor the properties of the resultant alkalised cocoa powder.

It can be concluded that a method for preparing the alkalised cocoa powder of the invention, as described in the claims, produces a suitably dark-coloured alkalised cocoa powder with intense flavour, and relatively low pH, therefore providing the atbrementioned advantages of the alkalised cocoa powder and of its method of preparation.

Claims

CLAIMS1. An alkalised cocoa powder having a pH of from 6.10 to 6.65.
2. An alkalised cocoa powder according to claim 1, wherein the alkalised cocoa powder has a pH of from 6.20 to 6.60.
3. An alkalised cocoa powder according to claim 1 or 2, wherein the alkalised cocoa powder has a pH of from 6.20 to 6.50.
4. An alkalised cocoa powder according to any of claims 1 to 3, wherein the alkalised cocoa powder has a pH of from 6.25 to 6.45.
5. An alkalised cocoa powder according to any preceding claim, wherein the alkalised cocoa powder has a D90 value of less than 50 Rm.
6. An alkalised cocoa powder according to any preceding claim, wherein the alkalised cocoa powder has an ash content of less than 15 wt.%.
7. An alkalised cocoa powder according to any preceding claim, wherein the alkalised cocoa powder has a potassium content of at least 3500 mg/100g, and/or wherein the alkalised cocoa powder has a sodium content of less than mg/100g.
8. An alkalised cocoa powder according to any preceding claim, wherein the alkalised cocoa powder has a colour L-value as measured by the While diluent method of from 17.0 to 26.0.
9. A method for preparing an alkalised cocoa powder according to any preceding claim, the method comprising the steps: a. Adding a sample of cocoa powder to a reaction vessel; b. Adding an alkali solution to the reaction vessel; c. After step (b), adding a gas to the reaction vessel such that the pressure in the reaction vessel reaches a first pressure (P1); d. After step (c), releasing at least a portion of the gas from the reaction vessel to reduce the pressure in the reaction vessel to a second pressure (P2); e. After step (d), adding a gas to the reaction vessel such that the pressure in the reaction vessel reaches a third pressure (P3); wherein P1 is greater than 3 0 bara, P3 is greater than 2.5 bara, and P2 is less than P1 and P3.
10. A method according to claim 9, wherein P1 is greater than P3.
11. A method according to claim 9, wherein P1 is greater than 4.0 bara.
12. A method according to any of claims 9 to 11, wherein P3 is greater than 3.5 bara.
13. A method according to any of claims 9 to 12, wherein the first pressure (P1) is from 4.0 bara to 8.0 bara.
14. A method according to claim 13, wherein the first pressure (P1) is from 5.0 bara to 7.0 ham.
15. A method according to any of claims 9 to 14, wherein the method comprises increasing the pressure in the reaction vessel from atmospheric pressure to the first pressure over the course of from 1 minute to 10 minutes, preferably from 5 minutes to 9 minutes, preferably about 7 minutes.
16. A method according to any of claims 9 to 15, wherein the second pressure is no greater than 1.5 bara.
17. A method according to any of claims 9 to 16, wherein the third pressure is no greater than 6.0 bara.
18. A method according to any of claims 9 to 17, wherein the first pressure is held for a first time period, and wherein the first time period is from 10 minutes to 50 minutes, preferably from 14 minutes to 46 minutes, more preferably from 15 minutes to 35 minutes.
19. A method according to any of claims 9 to 18, wherein the third pressure is held for a third time period, and wherein the third time period is from 25 minutes to 90 minutes, preferably from 28 minutes to 65 minutes.
20. A method according to any of claims 9 to 19, wherein the method comprises decreasing the pressure in the reaction vessel from the first pressure to the second pressure over the course of from 1 minute to 20 minutes, preferably from minutes to 10 minutes, more preferably about 7 minutes. 21. 22. 23. 24. 25.A method according to any of claims 9 to 20, wherein there is no significant air flow, or at least an air flow of less than 1.5 m3/hr, into the reaction vessel when the reaction vessel is at the first pressure.A method according to any of claims 9 to 21, wherein there is a continuous air flow through the reaction vessel when the reaction vessel is at the third pressure, optionally wherein the continuous air flow is at a rate of from 1.5 m-'/hr to 6 ml/hr, preferably about 5 m3/hr.A method according to any of claims 9 to 22, wherein the alkali agent is one or more compounds selected from the group consisting of: magnesium carbonate, sodium carbonate, potassium carbonate, magnesium hydrogen carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, sodium sesquicarbonate, potassium sesquicarbonate, magnesium hydroxide, sodium hydroxide, potassium hydroxide, and combinations thereof A food or beverage product comprising the alkalised cocoa powder of any of claims 1 to 8.A beverage product according to claim 24, wherein the beverage is chocolate milk.