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Textiles - Determination of PH PDF

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INTERNATIONAL ISO

STANDARD 3071

Third edition
2005-06-15

Textiles — Determination of pH
of aqueous extract
Textiles — Détermination du pH de l'extrait aqueux

Reference number
ISO 3071:2005(E)

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Contents Page

Foreword............................................................................................................................................................ iv
Introduction ........................................................................................................................................................ v
1 Scope ..................................................................................................................................................... 1
2 Normative references ........................................................................................................................... 1
3 Terms and definitions........................................................................................................................... 1
4 Principle ................................................................................................................................................. 1
5 Reagents ................................................................................................................................................ 1
6 Apparatus .............................................................................................................................................. 2
7 Preparation of test samples................................................................................................................. 2
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8 Procedure .............................................................................................................................................. 2
8.1 Preparation of the aqueous extract .................................................................................................... 2
8.2 Measurement of the pH of the aqueous extract ................................................................................ 2
9 Calculation............................................................................................................................................. 3
10 Precision ................................................................................................................................................ 3
11 Test report ............................................................................................................................................. 3
Annex A (informative) Preparation of standard buffer solutions .................................................................. 4

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ISO 3071:2005(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

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International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 3071 was prepared by Technical Committee ISO/TC 38, Textiles.

This third edition cancels and replaces the second edition (ISO 3071:1980), which has been technically
revised.

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Introduction
The pH-value of the aqueous extract of a textile affords a useful index to its processing history. In addition, it is
becoming more common to demand that the textile, in its various forms, conforms to certain limits in respect of
its acidity or alkalinity, often expressed in terms of the pH-value of the aqueous extract.
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INTERNATIONAL STANDARD ISO 3071:2005(E)

Textiles — Determination of pH of aqueous extract

1 Scope
This International Standard specifies a method for determining the pH of the aqueous extract of textiles. The
method is applicable to textiles in any form.

2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

3 Terms and definitions


For the purposes of this document, the following terms and definitions apply.

3.1
pH
co-logarithm of the hydrogen ion concentration in an aqueous extract

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4 Principle
The pH-value of an aqueous extract of a textile is measured electrometrically at room temperature by means
of a glass electrode.

5 Reagents
All reagents used shall be of recognized analytical grade.

5.1 Distilled or deionized water, of at least grade 3 as defined in ISO 3696, having a pH between 5,0
and 7,5.

The pH shall be verified the first time the water is used. If it is not within the specified range, the water shall be
redistilled using chemically resistant glassware. Acid or organic matter can be removed by distilling water from
a solution of 1 g/l potassium permanganate and 4 g/l sodium hydroxide. Alkalinity (e.g. the presence of
ammonia) can be removed by distilling the water from a solution of dilute sulfuric acid. If the distilled water is
not grade 3, boil 100 ml of distilled water in a beaker at a moderate rate for (10 ± 1) min and allow the covered
beaker to cool to room temperature.

5.2 Potassium chloride solution, 0,1 mol/l, prepared using distilled or deionized water (5.1).

5.3 Buffer solutions, which may be prepared as specified in Annex A, having a pH similar to that being
determined, for calibration of the pH-meter before measurement. Buffer solutions having a pH around 4, 7 or 9
are recommended.

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6 Apparatus
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6.1 Stoppered glass or polypropylene flasks, chemically resistant, for preparation of the aqueous extract.

NOTE It is recommended that the glassware used for this test be set aside for this purpose only and filled with
distilled water between tests.

6.2 Mechanical shaker, providing rotational or reciprocating movement sufficient to obtain a ready
exchange of liquid between the interior of the textile material and the solution used in preparing the extract. A
to-and-fro movement at a rate of 60 min−1 or a rotational frequency of 30 min−1 has been found satisfactory.

6.3 Beakers, chemically resistant, with a capacity of 150 ml (see Note to 6.1).

6.4 Rods, chemically resistant (see Note to 6.1).

6.5 pH-meter, with a glass electrode, capable of measuring to at least 0,1 pH-units.

6.6 Balance, accurate to 0,01 g.

6.7 1 l volumetric flasks, of grade A quality.

7 Preparation of test samples


7.1 Take a laboratory sample representative of the bulk of the textile material and sufficient to provide all
the test samples required. Cut the laboratory sample into pieces having approximately 5 mm sides or of such
a size as to allow the test samples to wet out rapidly.

7.2 To avoid contamination, handle the material as little as possible. Take from the laboratory sample three
test samples of (2,00 ± 0,05) g each.

8 Procedure

8.1 Preparation of the aqueous extract

Prepare the extract in triplicate at room temperature, as follows:

Place each test sample and 100 ml of extracting solution [either water (5.1) or potassium chloride solution
(5.2)] into a stoppered flask (6.1). Agitate the flask for a short period by hand to ensure that the textile material
is properly wetted out, then shake it mechanically for 2 h ± 5 min.

Record the temperature of the extracting solution used.

8.2 Measurement of the pH of the aqueous extract

Calibrate the pH-meter at the temperature of the extract to be measured. Check the calibration of the
pH-meter using two buffer solutions.

Immerse the electrode several times in the same solution (water or KCl solution) used to prepare the extract
until the indicated pH-value stabilizes.

Decant the first extract into a beaker, immediately immerse the electrode to a depth of at least 10 mm and stir
gently with a rod until the pH-value stabilizes (do not record the pH-value of this solution).

Decant the second extract into another beaker, immediately immerse the electrode, without washing, in the
beaker to a depth of at least 10 mm and allow to stand without stirring until the pH-value stabilizes. Record
this value.

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Decant the third extract into another beaker, immediately immerse the electrode, without washing, in the
beaker to a depth of at least 10 mm and allow to stand without stirring until the pH-value stabilizes. Record
this value.

Record the pH-values of the second and third extracts as the first and second measurements.

9 Calculation
If the difference between the two pH-values, expressed to the nearest 0,1 pH-units, is greater than 0,2, repeat
the procedure with other test samples. When two valid measurements have been obtained, calculate the
mean value.

10 Precision
Interlaboratory trials were carried out between nine laboratories measuring seven samples. Statistical analysis
was carried out and the following results were obtained:
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Using water (5.1) as the extracting solution: Reproducibility limit R = 1,7 pH-units;

Using KCl solution (5.2) as the extracting solution: Reproducibility limit R = 1,1 pH-units.

NOTE The statistical analysis was carried out in accordance with ISO 5725-2, Accuracy (trueness and precision) of
measurement methods and results — Part 2: Basic method for the determination of repeatability and reproducibility of a
standard measurement method.

11 Test report
The test report shall include the following information:

a) a reference to this International Standard, i.e. ISO 3071;

b) the mean pH-value, to the nearest 0,1 pH-units;

c) the type of solution used (water or KCl solution);

d) the pH of the extracting solution;

e) the temperature of the extracting solution;

f) any factor likely to have had an effect on the results, including any resistance to wetting out of the test
samples

g) the date of the determination.

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Annex A
(informative)

Preparation of standard buffer solutions

A.1 General
Use only reagents of recognized analytical reagent grade. Prepare the buffer solutions using water of at least
grade 3 as defined in ISO 3696 and renew them at least once a month.

A.2 pH 4,0 potassium hydrogen phthalate solution (0,05 mol/l)


Dissolve 10,21 g of potassium hydrogen phthalate (KHC8H4O4) in distilled or deionized water in a 1 l
volumetric flask and dilute to the mark. The pH of this solution is 4,00 at 20 °C and 4,01 at 25 °C.

A.3 pH 6,9 potassium dihydrogen orthophosphate and disodium hydrogen


orthophosphate solution (0,08 mol/l)
Dissolve 3,9 g of potassium dihydrogen orthophosphate (KH2PO4) and 3,54 g of disodium hydrogen
orthophosphate (Na2HPO4) in distilled or deionized water in a 1 l volumetric flask and dilute to the mark.

The pH of this solution is 6,87 at 20 °C and 6,86 at 25 °C.

A.4 pH 9,2 disodium tetraborate solution (0,01 mol/l)

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Dissolve 3,80 g of disodium tetraborate decahydrate (Na2B407 ⋅10H2O) in distilled or deionized water in a 1 l
volumetric flask and dilute to the mark. The pH of this solution is 9,23 at 20 °C and 9,18 at 25 °C.

4
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ISO 3071:2005(E)
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