ISO 4629-1:2016 pdf free download.Binders for paints and varnishes Determination of hydroxyl value Part 1:Titrimetric method without using a catalyst
Liants pour peintures et vernis — Determination de l’indice d’hydroxyle — Partie 1: Méthode titrimétrique sans catalyseur.
8.3 Determination
Add 5 ml of ethyl acetate (52) to the contents of the conical flask and shake, if necessary, with gentle warming, until the test portion (LZ) is dissolved.
If the test portion is not soluble in ethyl acetate, another solvent may be used.
Allow to cool to room temperature, add (5,00 ± 0,02) ml (see Note 1) of the acetylating reagent (5) by means of the microburette or pipette () and fit the reflux condenser (2) on the conical flask.
Heat the flask in the heating apparatus (), maintained at (50 ± 1) °C, for 20 mm, shaking every 5 mm.
Cool the contents of the flask to room temperature, remove the condenser, add 2 ml of water, replace the condenser and vigorously shake the flask. Add 10 ml of the pyridine/water mixture (&4) from the top of the condenser so as to rinse down the condenser tube. Mix the contents of the flask and allow to stand for 5 mm at room temperature. Add 30 ml of the toluene/butanol mixture (5) from the top of the condenser and use a further 30 ml of the toluene/butanol mixture to rinse the condenser/flask joint.
Titrate with potassium hydroxide solution ()
— either in the presence of a colour indicator (see Note 2), a few drops of phenolphthalein solution (52) or mixed-indicator solution (5), or
— determining the end point potentiometrically (see Note 3), using the potentiometric titration apparatus (f).
NOTE 1 The tolerance of 0,02 ml on the volume of the acetylating reagent is necessary to obtain the required precision of the test result.
NOTE 2 The colour changes are as follows:
— phenolphthalein: colourless (acid)/red (alkaline);
— mixed indicator: yellow (acid)/blue (alkaline).
NOTE 3 For hydroxyl values below 10 or dark-coloured solutions, potentiometric determination of the end point is desirable.
8.4 Blank test
Carry out a blank test, following the same procedure and using (5,00 ± 0,02) ml of the acetylating reagent (5S), but omitting the test portion.
8.5 Determination of acid value
Determine the acid value in accordance with ISO 2114:2000, Method A.
9 Expression of results
Calculate the hydroxyl value HV, in milligrams of KOH per gram of the product, using Formula (2):ISO 4629-1:2016 pdf free download.
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