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ISO 14900 2017 Hydroxyl Count

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ISO 14900 2017 Hydroxyl Count

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INTERNATIONAL ISO
STANDARD 14900

Second edition
2017-03

Plastics — Polyols for use in the


production of polyurethane —
Determination of hydroxyl number
Plastiques — Polyols pour la production du polyuréthanne —
Détermination de l’indice d’hydroxyle

Reference number
ISO 14900:2017(E)

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ISO 14900:2017(E)


COPYRIGHT PROTECTED DOCUMENT


© ISO 2017, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
[email protected]
www.iso.org

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Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 1
4 Principle......................................................................................................................................................................................................................... 2
5 Interferences............................................................................................................................................................................................................. 2
6 Reagents......................................................................................................................................................................................................................... 2
7 Apparatus...................................................................................................................................................................................................................... 4
8 Method A — Acetylation................................................................................................................................................................................ 5
8.1 Procedure..................................................................................................................................................................................................... 5
8.2 Expression of results........................................................................................................................................................................... 7
8.3 Precision and bias................................................................................................................................................................................. 7
8.4 Test report.................................................................................................................................................................................................... 8
9 Method B — Phthalation............................................................................................................................................................................... 8
9.1 Procedure..................................................................................................................................................................................................... 8
9.2 Expression of results........................................................................................................................................................................... 9
9.3 Precision and bias.............................................................................................................................................................................. 10
9.4 Test report................................................................................................................................................................................................. 10
Bibliography.............................................................................................................................................................................................................................. 12

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ISO 14900:2017(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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www​.iso​.org/​directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www​.iso​.org/​patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment,
as well as information about ISO’s adherence to the World Trade Organization (WTO) principles in the
Technical Barriers to Trade (TBT) see the following URL: www​.iso​.org/​iso/​foreword​.html.
This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12,
Thermosetting materials.
This second edition cancels and replaces the first edition (ISO 14900:2001), of which it constitutes a
minor revision. It also incorporates the Technical Corrigendum ISO 14900:2001/Cor. 1:2005. The
changes compared to the previous edition are as follows:
— in Clause 2, the normative references have been updated;
— in Clause 4, it has been clarified that Method A refers to “acetylation” and Method B refers to
“phthalation”.

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Introduction
International Standards have been published which deal with the determination of hydroxyl values of
unsaturated-polyester resins (ISO 2554), non-ionic surface active agents (ISO 4326, ISO 4327), binders
for paints and varnishes [ISO 4629 (all parts)] and industrial polyglycols (ISO 6796). The two methods
in this document are improved versions of imidazole-catalyzed procedures specifically tailored to the
determination of the hydroxyl number of many types of polyol, including those used in the production of
polyurethanes. Method A is especially suited to the determination of the hydroxyl number of polyether
polyols that may have steric hindrance, or are otherwise difficult to determine by phthalation. Method B
is a general method based on phthalation and is applicable to a wide range of polyol types. Both of these
methods are similar to procedures found in ASTM D4274.

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INTERNATIONAL STANDARD ISO 14900:2017(E)

Plastics — Polyols for use in the production of


polyurethane — Determination of hydroxyl number
WARNING — Persons using this document should be familiar with normal laboratory practice.
This document does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices and to
ensure compliance with any national regulatory conditions.

1 Scope
This document specifies two methods for the measurement of the hydroxyl number of polyols used
as polyurethane raw materials. It is necessary to know the hydroxyl content of polyols to properly
formulate polyurethane systems. Method A is primarily applicable to readily esterified polyether
polyols. It is also intended for polyols which have significant steric hindrance, such as those based on
sugars. Method B is intended for polyether polyols, polymer polyols and amine-initiated polyols, but
may give low results for sterically hindered polyols. Other polyols can be analysed by these methods
if precautions are taken to verify applicability. These methods can be used for research and for quality
control and specification purposes.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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 385, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 760, Determination of water — Karl Fischer method (General method)
ISO 835, Laboratory glassware — Graduated pipettes
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 4788, Laboratory glassware — Graduated measuring cylinders
ISO 6353-1, Reagents for chemical analysis — Part 1: General test methods
ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series
ISO 6353-3, Reagents for chemical analysis — Part 3: Specifications — Second series

3 Terms and definitions


For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://​w ww​.electropedia​.org/​
— ISO Online browsing platform: available at http://​w ww​.iso​.org/​obp

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3.1
polyurethane
polymer prepared by the reaction of an organic di- or polyisocyanate with compounds containing two
or more hydroxyl groups
3.2
hydroxyl number
hydroxyl value
number of milligrams of potassium hydroxide equivalent to the hydroxyl content of 1 g of a test portion

4 Principle

4.1 Method A (Acetylation): A test portion is refluxed in a solution of acetic anhydride in pyridine
to acetylate the hydroxyl groups present; the reaction is catalyzed by imidazole. The excess reagent
is hydrolyzed with water and the resulting acetic acid is titrated with standardized sodium hydroxide
solution. The hydroxyl content is calculated from the difference in titration of the test portion and a blank
solution.

CAUTION — Acetic anhydride and pyridine are toxic and flammable. In addition, acetic anhydride
is corrosive. Take proper precautions when handling these reagents.

4.2 Method B (Phthalation): The hydroxyl groups in a test portion are esterified by refluxing with a
solution of phthalic anhydride in pyridine; the reaction is catalyzed by imidazole. The excess anhydride
is hydrolyzed with water and the phthalic acid formed is titrated with standardized sodium hydroxide
solution. The hydroxyl content is calculated from the difference in titration of the test portion and a blank
solution.

5 Interferences

5.1 Excess water will interfere by destroying part of the esterification reagent. If the sample contains
more than 0,2 % water, dry the sample with a reagent that will not add acidity or basicity to the sample.

5.2 Primary and secondary amines and long-chain fatty acids react with the reagent to form stable
compounds that will be included in the result.

6 Reagents
Reagent-grade chemicals shall be used in all determinations. Unless otherwise indicated, it is intended
that all reagents conform to the specifications of ISO 6353-1, ISO 6353-2 and ISO 6353-3, although other
grades may be used provided that it is first determined that the reagent is of sufficiently high purity to
permit its use without lessening the accuracy of the determination.
Unless otherwise indicated, references to water shall be understood to mean grade 2 reagent water as
defined by ISO 3696.

6.1 Acetylation reagent (for method A).

Mix 127 ml of acetic anhydride with 1 000 ml of dry pyridine (6.7). Add 16 g of imidazole (6.3) and swirl
carefully to dissolve. Prepare the reagent fresh daily and keep it in a dark bottle. Do not use it if it is
darker than pale yellow.
NOTE Some laboratories have reported that dark, resinous solids have formed when the mixture of pyridine
and esterification reagent is heated. In that event, it has been found that preparing the acetylation reagent with
the addition of 0,4 % water in the pyridine (6.8) will correct the problem. However, care has to be taken that
sufficient reagent is present to complete the reaction quantitatively. See also 8.1.2.

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CAUTION — Acetic anhydride and pyridine are eye, skin, and respiratory irritants. Avoid bodily
contact with these reagents and use only in a well-ventilated area.

6.2 Phthalation reagent (for method B).

Weigh 116 g of phthalic anhydride into a 1 l brown bottle. Add 700 ml of pyridine (6.7) and shake
vigorously until dissolved. Add 16 g of imidazole and swirl carefully to dissolve. The reagent shall stand
overnight before use. Avoid prolonged exposure of the reagent to moisture in the air. Discard reagent
that develops a colour. In the blank titration as described in the procedure for method B, exactly 25 ml
of this reagent shall consume between 95 ml and 100 ml of 0,500 mol/l sodium hydroxide.

6.3 Imidazole, reagent grade or equivalent.

6.4 Hydrochloric acid, standard solution, 0,1 mol/l.

Prepare and standardize to four significant figures in accordance with good practice, using potassium
acid phthalate (6.6) as a primary standard. Determine and record the temperature at which the
standardization was performed. The concentration of the solution shall be corrected to the temperature
at which the determination is performed, as described in 6.9. This solution is required only if a
correction is to be applied for the presence of strong base in the sample being analysed.

6.5 Phenolphthalein indicator solution, 10 g/l.

Prepare a solution of 1 g of phenolphthalein in 100 ml of pyridine (6.7).

6.6 Potassium acid phthalate.

Use a certified primary standard.

6.7 Pyridine, reagent grade, containing less than 0,1 % water.

If purification is required, distil from phthalic anhydride, discarding the fraction boiling below 114 °C
to 115 °C.

6.8 Pyridine, containing from 0,30 % to 0,45 % water (used for special cases: see the note to 6.1).

Determine the water content of the pyridine using ISO 760. Add the required amount of water. The
required volume of water to add per litre of pyridine may be calculated as follows:
Water to add, in ml = 4,0 − 9A

where A is the percent water already in the pyridine.

6.9 Sodium hydroxide, standard solution, 0,5 mol/l.

Prepare and standardize to four significant figures in accordance with good practice. Determine and
record the temperature at which the standardization was performed. The factor for thermal expansion
of this solution is 0,000 14. For calculation of the hydroxyl content, the concentration of the solution
shall be corrected to the temperature at which the determination was performed by the following:
cθ2 = cθ1 + F(θ1 − θ2)

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where

cθ1 is the concentration of the solution when standardized, in mol/l;

cθ2 is the concentration during analysis of samples, in mol/l;

θ1 is the temperature of the solution during standardization, in °C;

θ2 is the temperature of the solution during analysis of samples, in °C;

F is the factor to correct for thermal expansion of the solution.

7 Apparatus

7.1 Potentiometric titrator or pH-meter, accurate to 0,1 mV or better, equipped with a pair of
electrodes or a combination glass-calomel electrode and a piston burette having a 100 ml capacity or
capability for multiple automatic refilling.

7.2 Syringes, 2 ml, 5 ml and 10 ml, with an orifice suitable for handling viscous polyols.

7.3 Magnetic stirrer.

7.4 Analytical balance, accurate to 0,1 mg.

7.5 Volumetric pipette, 20 ml, conforming to ISO 648.

7.6 Measuring pipette, 1 ml, conforming to ISO 835.

7.7 Graduated cylinder, 100 ml, conforming to ISO 4788.

7.8 Beakers, 250 ml, 500 ml.

7.9 Burette (for colorimetric titration), 100 ml total capacity, range of graduated portion 50 ml, with
0,1 ml graduations, and conforming to ISO 385. If a 100 ml burette is not available, the first 50 ml of
titrant may be added by pipette and the titration completed with a 50 ml burette.

7.10 Conical flasks, 300 ml, with standard taper 24/40 joint.

7.11 Condenser, West type, 400 mm, drip-tip, standard taper 24/40 joint with cooling extending to
the joint.

7.12 Oil bath, maintained at 115 °C ± 2 °C.

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8 Method A — Acetylation

8.1 Procedure

8.1.1 If the sample does not contain an appreciable amount of water, determine the test portion size
required using one of the following formulae:

561 × 0, 98
Test portion size, in g =
Expected hydroxyl number
or

0, 009 8 × Mr
Test portion size, in g =
n
where

Mr is the molecular mass of the hydroxyl-containing compound;

n is the number of hydroxyl groups in the molecule.


NOTE In each case, the calculation is based on the assumption that a maximum of 9,8 meq of hydroxyl is
present.

Since the calculated test portion size will be near the maximum permitted by the method, adhere
closely to the amount calculated.
If the sample contains an appreciable amount of water, the test portion size shall be adjusted to
accommodate this interference. In this case, determine the test portion size using one of the following
formulae:

0, 170 1 × 0, 98
Test portion size, in g =
0, 009 4 R + [0, 01 S × (n × 17, 01) / Mr ]
or

550
Test portion size, in g =
Expected hydroxyl number + (31, 2 × R )
where

R is the water in the sample, in mass %;

S is the purity of the sample, in mass %;

Mr is the molecular mass of the hydroxyl-containing compound;

n is the number of hydroxyl groups present in the molecule.


Precision and accuracy may be decreased when appreciable amounts of water are present because of
the required decrease in test portion size.

8.1.2 Having calculated the appropriate size, weigh the test portion into a clean, dry conical flask (7.10).

8.1.3 Pipette 25,0 ml of the acetylation reagent (6.1) into each flask (7.10) used for test portion and
blank determinations, using a uniform drainage time for all aliquots. If necessary, swirl the test portion
flask to dissolve the test portion. Connect each flask to a condenser (7.11) (if the surrounding atmosphere

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is humid, connect the condenser to a drying trap containing 2-mesh, indicating-type calcium chloride),
seal the joint with 1 or 2 drops of pyridine, and place on a hotplate. Heat at the reflux temperature for
30 min, regulating the hotplate so that the vapours condense gently near the bottom of the condenser.
Note that for some polyol types, a longer period of reflux may be necessary. Check that the time used is
sufficient to reach a constant value for the hydroxyl number.

8.1.4 After the reflux period, allow the flask to cool, then rinse the condenser with 25 ml of water.
Remove the condenser and rinse the joint of the condenser and the flask with water, collecting the
rinsings in the flask.

8.1.5 Titrate the solution by one of the following two procedures:

8.1.5.1 Potentiometric titration

Quantitatively transfer the solution to a 250 ml beaker, rinsing the flask with a small portion of water.
Place on the automatic titrimeter (7.1) and stir with a magnetic stirrer (7.3).
Immerse the titrimeter electrodes in the solution and titrate with 0,5 mol/l sodium hydroxide solution
(6.9) until the equivalence point is reached. If the volume of 0,5 mol/l NaOH solution required for the
titration of the test portion is less than 80 % of that required for the blank, the test portion was too
large and the analysis shall be repeated with a smaller test portion.
Record the temperature of the 0,5 mol/l NaOH solution.

8.1.5.2 Colorimetric titration

Add 0,5 ml of phenolphthalein indicator solution (6.5) and a magnetic stirrer bar to the test portion
solution.
Titrate, while stirring, with 0,5 mol/l sodium hydroxide solution to the first faint pink end point that is
permanent for 15 s.
Read the volume to 0,02 ml. If the volume of 0,5 mol/l NaOH solution required for the titration of the
test portion is less than 80 % of that required for the blank, the test portion was too large and the
analysis shall be repeated with a smaller test portion.
Record the temperature of the 0,5 mol/l NaOH solution.

8.1.6 If the sample contains significant acidity or alkalinity, correct the result as follows:

8.1.6.1 Weigh into a 300 ml conical flask the same amount of sample used for the hydroxyl
determination. Add to the flask 75 ml of pyridine (6.7), 75 ml of water, and 0,5 ml of phenolphthalein
indicator solution.

8.1.6.2 Acidity correction: If the solution in 8.1.6.1 is colourless, titrate with standard 0,1 mol/l NaOH
using potentiometric or colorimetric end point detection. Conduct a blank determination on the reagent
mixture described in 8.1.6.1, leaving out the test portion. The acidity correction, in milligrams of KOH per
gram, is calculated as follows:

(V1 − V2 ) c × 56, 1
Acidity correction =
m
where

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V1 is the volume of NaOH solution required for titration of the test portion, in ml;

V2 is the volume of NaOH solution required for titration of the blank, in ml;

c is the concentration of the NaOH solution, in mol/l;

m is the mass of the test portion, in g.

8.1.6.3 Alkalinity correction: If the solution in 8.1.6.1 is pink, titrate potentiometrically to the
equivalence point (or, if colorimetric end point determination is used, titrate to the disappearance of the
pink colour), using 0,1 mol/l HCl. Then add 1,0 ml excess of 0,1 mol/l HCl. Back-titrate with standard
0,1 mol/l NaOH to the equivalence point (or, if colorimetric, to a pink end point that persists for at least
15 s). Using standard 0,1 mol/l NaOH, titrate a blank containing exactly the same total amount of added
0,1 mol/l HCl and the reagent mixture used previously, but omitting the test portion. The alkalinity
correction, in milligrams of KOH per gram, is calculated as follows:

(V2 − V1 ) c × 56, 1
Alkalinity correction =
m
in which the symbols are as defined in 8.1.6.2.

8.2 Expression of results

8.2.1 Calculate the hydroxyl number, in milligrams of KOH per gram of sample, as follows:

(V 4 − V3 ) c × 56, 1
Hydroxyl number =
m
where

V3 is the volume of NaOH solution required in 8.1.5.1 or 8.1.5.2 for titration of the test portion, in ml;

V4 is the volume of NaOH solution required in 8.1.5.1 or 8.1.5.2 for titration of the blank, in ml;

c is the concentration of the NaOH solution, in mol/l;

m is the mass of the test portion, in g.

8.2.2 If the sample contains free acidity or alkalinity as measured in 8.1.6, correct the result as follows:

Hydroxyl number (corrected) = Hydroxyl number + acidity


or
Hydroxyl number (corrected) = Hydroxyl number − alkalinity

8.3 Precision and bias

8.3.1 Precision data were determined from round-robin tests conducted by laboratories associated
with the Polyurethane Raw Materials Analysis Committee (PURMAC) in the US. ASTM E180 was used to
calculate precision values. Data from the round robin may be obtained from ASTM Committee D-20 or
from the PURMAC committee of the American Plastics Council.

Use the criteria given in 8.3.2 and 8.3.3 to judge the acceptability of results.

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8.3.2 Repeatability (single analyst): Duplicate results obtained by the same analyst using the same
equipment on the same day should only be considered suspect if they differ by more than the value of r
shown in Table 1 for the same, or similar, material.

8.3.3 Reproducibility (multilaboratory): Results, each the mean of duplicates, obtained in separate
laboratories should only be considered different if they differ by more than the value of R shown in
Table 1 for the same, or similar, material.

Table 1 — Precision data for hydroxyl number by acetylation


Mean value of
Test material sr sR r R
OH number
PTME glycol 111 0,7 2,8 2,0 7,8
Glycerine-based polyol, p.o./e.o. capped 33,4 0,3 0,7 0,8 2,0
Glycerine-based polyol, p.o./e.o. capped 54,5 0,6 2,8 1,7 7,8
Sucrose/glycerine-based propoxylat- 492,6 1,5 3,9 4,2 10,9
ed polyol
sr   is the within-laboratory standard deviation of replicates;
sR   is the between-laboratory standard deviation of averages of duplicates;
r    is the within-laboratory repeatability limit (2,8 × sr);
R   is the between-laboratory reproducibility limit (2,8 × sR).

8.3.4 Bias: The bias for this test method has not been determined.

8.4 Test report


The test report shall include the following:
a) a reference to this document, i.e. ISO 14900;
b) the corrected hydroxyl number, to the nearest 0,1;
c) all details necessary to identify the product analysed (such as manufacturer, product type, lot or
notebook numbers, date of manufacture, as required);
d) the method of titration used (potentiometric autotitrator or colorimetric);
e) any incident or detail not stipulated in this document which may have influenced the result;
f) the date of the analysis.

9 Method B — Phthalation

9.1 Procedure

9.1.1 Weigh into a conical flask (7.10), using a syringe (7.2) or other suitable equipment, an amount of
sample calculated as follows:

561
Test portion size, in g =
Expected hydroxyl number
No material shall be allowed to touch the neck of the flask.
Record the test portion size to the nearest milligram.

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Since the calculated mass will be near the maximum permitted by the method, adhere closely to the
mass calculated.

9.1.2 Accurately pipette 25 ml of the phthalation reagent (6.2) into each flask used for test portion
and blank determinations. Swirl the test portion flask to dissolve the test portion. Connect each flask to a
condenser (7.11) and place the flasks in the oil bath (7.12), maintained at 115 °C ± 2 °C, for 30 min.

Some laboratories prefer to maintain the oil bath at 100 °C ± 2 °C. This variation may be used if it is
demonstrated that quantitative reaction is obtained with the particular product being tested.

9.1.3 After the heating period, remove the assembly from the bath and cool to room temperature.
Wash down the condenser with 30 ml of pyridine and remove the condenser. Quantitatively transfer the
solution to a 250 ml beaker using 20 ml of pyridine to rinse the flask.

9.1.4 Titrate the solution by one of the following two procedures:

9.1.4.1 Potentiometric titration

Place on the automatic titrimeter (7.1) and stir with a magnetic stirrer (7.3).
Immerse the titrimeter electrodes in the solution and titrate with 0,5 mol/l sodium hydroxide solution
(6.9) until the equivalence point is reached. If the volume of 0,5 mol/l NaOH solution required for the
titration of the test portion is less than 80 % of that required for the blank, the test portion was too
large and the analysis shall be repeated with a smaller test portion.
Record the temperature of the 0,5 mol/l NaOH solution.

9.1.4.2 Colorimetric titration

Add 0,5 ml of phenolphthalein indicator solution (6.5) and a magnetic stirrer bar to the test portion
solution.
Titrate, while stirring, with 0,5 mol/l sodium hydroxide solution to the first faint pink end point that is
permanent for 15 s.
Read the volume to 0,02 ml. If the volume of 0,5 mol/l NaOH solution required for the titration of the
test portion is less than 80 % of that required for the blank, the test portion was too large and the
analysis shall be repeated with a smaller test portion.
Record the temperature of the 0,5 mol/l NaOH solution.

9.1.5 If the sample contains significant acidity or alkalinity, correct the result as described in 8.1.6.

9.2 Expression of results

9.2.1 Calculate the hydroxyl number, in milligrams of KOH per gram of sample, as follows:

(V 4 − V3 ) c × 56, 1
Hydroxyl number =
m
where

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V3 is the volume of NaOH solution required in 9.1.4.1 or 9.1.4.2 for titration of the test portion, in ml;

V4 is the volume of NaOH solution required in 9.1.4.1 or 9.1.4.2 for titration of the blank, in ml;

c is the concentration of the NaOH solution, in mol/l;

m is the mass of the test portion, in g.

9.2.2 If the sample contains free acidity or alkalinity as measured in 8.1.6, correct the result as follows:

Hydroxyl number (corrected) = Hydroxyl number + acidity


or
Hydroxyl number (corrected) = Hydroxyl number − alkalinity

9.3 Precision and bias

9.3.1 Precision data were determined from round-robin tests conducted by laboratories associated
with the Polyurethane Raw Materials Analysis Committee (PURMAC) in the US. ASTM E180 was used to
calculate precision values. Data from the round robin may be obtained from ASTM Committee D-20 or
from the PURMAC committee of the American Plastics Council.

Use the criteria given in 9.3.2 and 9.3.3 to judge the acceptability of results.

9.3.2 Repeatability (single analyst): Duplicate results obtained by the same analyst using the same
equipment on the same day should only be considered suspect if they differ by more than the value of r
shown in Table 2 for the same, or similar, material.

9.3.3 Reproducibility (multilaboratory): Results, each the mean of duplicates, obtained in separate
laboratories should only be considered different if they differ by more than the value of R shown in
Table 2 for the same, or similar, material.

Table 2 — Precision data for hydroxyl number by phthalation


Mean value of
Test material sr sR r R
OH number
PTME glycol 112 0,4 1,7 1,1 4,8
Glycerine-based polyol, p.o./e.o. capped 34,0 0,1 0,5 0,3 1,4
Glycerine-based polyol, p.o./e.o. capped 56,1 0,3 1,7 0,8 4,8
Sucrose/glycerine-based propoxylat-
492 1,4 3,9 3,9 10,9
ed polyol
sr   is the within-laboratory standard deviation of replicates;
sR   is the between-laboratory standard deviation of averages of duplicates;
r   is the within-laboratory repeatability limit (2,8 × sr );
R   is the between-laboratory reproducibility limit (2,8 × sR).

9.3.4 Bias: The bias for this test method has not been determined.

9.4 Test report


The test report shall include the following:
a) a reference to this document, i.e. ISO 14900;
b) the corrected hydroxyl number, to the nearest 0,1;

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c) all details necessary to identify the product analysed (such as manufacturer, product type, lot or
notebook numbers, date of manufacture, as required);
d) the method of titration used (potentiometric autotitrator or colorimetric);
e) any incident or detail not stipulated in this document which may have influenced the result;
f) the date of the analysis.

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Bibliography

[1] ISO 2554, Plastics — Unsaturated polyester resins — Determination of hydroxyl value
[2] ISO 4326, Non-ionic surface active agents — Polyethoxylated derivatives — Determination of
hydroxyl value — Acetic anhydride method
[3] ISO 4327, Non-ionic surface active agents — Polyalkoxylated derivatives — Determination of
hydroxyl value — Phthalic anhydride method
[4] ISO 4629 (all parts), Binders for paints and varnishes — Determination of hydroxyl value
[5] ISO 6796, Polyglycols for industrial use — Determination of hydroxyl number — Phthalic anhydride
esterification method
[6] ASTM D4274, Standard Test Methods for Testing Polyurethane Raw Materials — Determination of
Hydroxyl Numbers of Polyols
[7] ASTM E180, Standard Practice for Determining the Precision of ASTM Methods for Analysis and
Testing of Industrial and Specialty Chemicals

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ISO 14900:2017(E)


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