Government of Canada Gouvernement du Canada

HPB Method MFHPB-03

February 2003

HEALTH PRODUCTS AND FOOD BRANCH

OTTAWA

DETERMINATION OF THE PH OF FOODS

INCLUDING FOODS IN HERMETICALLY SEALED CONTAINERS

Dev C. Nundy
Food Section
Ottawa Laboratory (Carling)
Canadian Food Inspection Agency
Ottawa, Ontario, K1A 0C6

e-mail: [email protected]

with Carol Crawford (CFIA, Vancouver), Donna Douey (CFIA, Calgary),

and Yvon-Louis Trottier (CFIA, St.-Hyacinthe).

1. APPLICATION

This method is designed to measure the equilibrium pH of foods, including thermally processed and foods
in other hermetically sealed containers. This revised method replaces MFHPB-25H, dated October 1991.

2. PRINCIPLE

This method is based upon the determination of the hydrogen ion concentration of food by direct
immersion of a single (combination) electrode into the food or a prepared sample of the food that has been
blended to paste consistency. This determination is recorded in terms of pH. Modern instrumentation and
availability of wide variety of electrode types and styles have made the measurement of pH simple and
convenient with very low maintenance.

3. DEFINITION OF TERMS

See Appendix A of Volume 2.

4. COLLECTION OF SAMPLES

See Appendix B of Volume 2.

5. MATERIALS AND SPECIAL EQUIPMENT

1) pH Meter

2) Combination electrode with Ag/Agcl Reference or Solid State Combination pH Electrode

Published on the Food Directorate’s (Health Canada's) website at http://www.hc-sc.gc.ca/food-aliment.

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3) Sieve or strainer

4) Buffer solutions, pH 3, 4, 5, 7, 10

5) Lab Blender, homogenizer or mixer

6) Lab Stomacher

7) Distilled water, recently boiled (CO2 free)

8) Separatory funnel or centrifuge

6. PROCEDURE

6.1 Handling and Preparation of sample units

6.1.1 Store perishable foods in the refrigerator (4/C) until day of analysis. Store non-perishable,
canned (normal or flat) or low moisture foods at room temperature. Store frozen foods at
-20/C.

6.1.2 Samples must be at room temperature before testing the pH. Thaw frozen samples at
refrigeration temperatures and then bring to room temperature before analysis.

6.1.3 For food in containers (such as canned), follow MFHPB-01 for the identification of the
container, removal and identification of the label, opening of the container, and mixing the
contents, as appropriate.
.
6.1.4 For other foods, handle as for other analysis, keeping in mind that many samples will
be undergoing microbiological testing and therefore must be handled
appropriately. Use aseptic technique and sterile equipment and avoid cross
contamination with other products, as appropriate.

6.2 Preparation of the food samples

The amount or weight of sample tested will depend on the amount of sample available. For
homogenized products, weigh a representative portion of the sample, in an appropriate amount
(approximately 100 g). Smaller amounts may be used in cases where the amount of sample
available is insufficient to test 100 g.

NOTE: A small amount of added water will not alter the pH of most food products, but
caution must be exercised concerning poorly buffered foods. When adding water
to a food matrix, the amount specified (i.e., 50 mL of water to 100 g of sample) is a
guideline only. Use as little water as possible to obtain the proper consistency.
This is particularly important with poorly buffered foods.

Some food products may consist of a mixture of liquid and solid components that differ in acidity.
Other food products may be semisolid in character. The following methods of sample preparation
should be used for pH testing, as appropriate.

6.2.1 Solids

Blend the sample to a paste consistency and determine the pH. Where more fluidity is
required add a small amount of recently-boiled distilled water to facilitate the blending. No
more than 50 mL of distilled water should be added to each 100 g of the product.

6.2.2 Liquid and solid component mixtures

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Mixtures of solids and liquids can be tested either by blending the mixture to a paste
consistency and measuring the pH directly or by separating the solid and liquid portions,
and testing each portion separately.

If separating the solid and liquid portions, drain the contents of the container by using a
suitable strainer or sieve. Standard sieve sizes of 8 to 20 are available for this procedure
and will be dependant on the particle size of the sample. Retain and test each portion
separately, preparing the solid component as in 6.2.1.

If the liquid portion contains sufficient oil to cause electrode fouling, separate the phases
with a separatory funnel or centrifuge and retain the aqueous phase for pH determination.
The oil phase may be discarded. See 7.4.1 regarding fouling of the electrode caused by
excessive oil.

6.2.3 Marinated oil products

Separate the oil from the solid product by using a suitable strainer or sieve, and discard
the oil. Blend the solid to a paste consistency and determine the pH. Where more fluidity
is required add a small amount of recently-boiled distilled water to facilitate the blending.
No more than 50 mL of distilled water should be added to each 100 g of the product. See
7.4.1 regarding fouling of the electrode caused by excessive oil.

6.2.4 Semisolid products

Food products of a semisolid consistency such as puddings, potato salad, etc., may be
blended to a paste consistency, and the pH determined on the prepared paste. Where
more fluidity is required add a small amount of recently-boiled distilled water to facilitate
the blending. No more than 50 mL of distilled water should be added to each 100 g of the
product.

6.2.5 Special product mixtures

For special product mixtures such as antipasto, pour off the oil, blend the remaining
product to a paste consistency and determine the pH. Where more fluidity is required add
a small amount of recently-boiled distilled water to facilitate the blending. No more than
50 mL of distilled water should be added to each 100 g of the product. See 7.4.1
regarding fouling of the electrode caused by excessive oil.

6.2.6 Meat and meat products

For unhomogenized products of a firm consistency, make a hole in the sample for each
measuring point, so that the glass electrode may be introduced into it without breakage.
Alternatively, a piercing type of electrode may be used to obtain a reading. If sample
integrity must be maintained for further microbiological testing, or if the sample
consistency does not allow this direct measurement, use the appropriate meat sample
preparation technique outlined below.

6.2.6.1 Meat and meat products other than dry and fermented meats
Process these meats as in 6.2.1 (solids).

6.2.6.2 Fermented meat products (Dry and Semi-Dry Sausages)

Mince a representative portion of the sample and homogenize to a paste
consistency with up to twice its weight of water (1:2), and determine the pH. No
more than 200 mL of distilled water should be added to each 100 g of the product.

6.2.6.3 Dried meats (Jerkies)

Mince a representative portion of the sample and homogenize to a paste
consistency with up to an equal mass of water (1:1), and determine the pH. No
more than 100 mL of distilled water should be added to each 100 g of the product.
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7. DETERMINATION OF PH OF SAMPLES

7.1 Ensure that the instrument is switched on and that all electronic components are warmed up
before proceeding.

7.2 The pH meter used should have a minimum accuracy of 0.1 pH unit, and reproducibility should be
± 0.05 pH unit or less. To obtain accurate results, a uniform temperature should be maintained for
the electrodes, the standard buffer solutions and the sample.

7.3 Instrument and Electrode Standardization

Standardization shall be accomplished using prepared standard buffers having a pH close to that
of the food to be tested. Refer to the pH meter operator’s manual for standardization procedures.
The buffer solutions should be at room temperature (21/C to 26/C).

7.4 The temperature of the sample should be at room temperature (21/C to 26/C). With some
expanded scale instruments, the sample temperature must be the same as the temperature of the
buffer solution used for the standardization. Other pH meters have temperature compensator
controls if the sample is not between 21/C and 26/C. Refer to the manufacturers’ manual.

7.4.1 Rinse and blot the electrode. Immerse the electrode in the sample and take the pH
reading, allowing one minute for the meter to stabilize (or with some models, whenever
the instrument signals, either by an audible “beep” or some other means, that equilibrium
has been reached). Rinse with distilled H20 and blot the electrode. Repeat on a fresh
portion of the sample. Oil and grease from the samples may coat the electrode, so it is
advisable to clean and standardize the instrument frequently. When oily samples cause
fouling problems, it may become necessary to rinse the electrode with 95% ethyl alcohol.
Make the measurement using the procedure appropriate to the pH meter and
electrode used. Read the pH directly from the scale or digital readout to the
nearest 0.05 pH unit, when a constant value has been reached. Record the pH
measurement to two decimal places.

For care and use of electrodes refer to manufacturers manual.

7.5 A surface or probe type of pH combination electrode can be used for pH determination of solid or
liquid samples.

8 DETERMINATION OF PH RESULTS

8.1 Record all measurements and/or observation for each representative sample. Summary tables
are recommended.

8.2 Non-destructive measurements (no mixing or homogenization of the sample)

At each point tested take two pH measurements to the nearest 0.05 pH unit. Repeat the
measurement at various points, if appropriate. The number of test points is a function of the
nature and the size of the sample.

For samples of 10 cm2 or less, measure the pH at two points, taking duplicate readings at each
point, with the mean recorded. The reported value is the average of the means, rounded to one
decimal point.

For a larger sample unit (greater than 10 cm2 ) measure the pH at one test point for every 10 cm2
unit area, with a minimum of three test points for the whole sample (duplicate readings at each
point). The reported value is the average of the means of all points tested, rounded to one
decimal point

8.3 Homogenized product measurements

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Take two pH determinations of the well mixed sample to the nearest 0.05 pH unit. The difference
between the values resulting from the two measurements shall not exceed 0.15 pH unit for
homogenized samples. If the difference is greater than 0.15 pH units, repeat the homogenization
or mixing procedure and repeat the pH determinations. Average the two pH determinations to
determine the pH result, rounded to one decimal point. This is the reported value. When more
than one sample unit is involved, report all values or the range of values (lowest and highest), as
appropriate.

9. REFERENCES

9.1 APHA. 2001. Compendium of methods for the microbiological examination of foods, 4th ed., F.P.
Downes and K. Ito (eds.). American Public Health Association, Washington, D.C.

9.2 Fisher Scientific. 1999. Accumet Electrochemistry Handbook, Bulletin No. 2823. Pittsburg, PA,
USA.

9.3 Fisher Scientific, Electrode Handbook, 5th Edition, Pennsylvania USA.

9.4 Australian New Zealand Food Authority (ANZFA). Food Standards Code. Standard 1.6.2 available
at http://www.anzfa.gov.au/foodstandardscodecontents/standard16/standard162.cfm

9.5 Koniecko, E.S., 1979. Handbook for Meat Analysis. 2nd edition. Avery Publishers, Group Wayne,
N.J. pp 103-104.

9.6 International Standrads Organization (ISO). 1974. Meat and Meat Products - Measurement of pH.
International Standard.
ISO 2917:1974.

9.7 ISO. 1999. Meat and Meat Products - Measurement of pH. International Standard
ISO 2917:1999.