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2.5.4 PHMB (as raw material) test

PHMB dosing method by UV spectrum

Method Nickel-Nioxime
For a 15g tablet of ABREUVAL TABLETS

Principle

This dosage technique is based on the ability of PHMB to get complexed with iron
cations.

Measuring equipment scaling

Needed reactives and equipment

It is needed a visible spectrophotometre that can set 2 successive wave lengths in the
same sample.

Necessary reactives to the preparation of the different solutions used in that dosage :
- Concentrated ammonia,
- Nickel (II) chloride hexahydrated,
- Nioxime (cyclohexane-1,2-dione-dioxime),
- Vantocil IB (aquous solution at 20% PHMB = the active ingredient used in
ABREUVAL TABLETS),
- Distilled water.

Procedure

Solutions preparation :
- Nickel solution : in a 100 mLflask, 0.04 gr of NICL2.6H2O are dissolved with with
50 mL of distilled water to which are added 15 mL of concentrated ammonia.
The the solution is completed to 100ml with distilled water. The obtained
concentration is 100g/mL Ni2+.
- Nioxime solution : dissolve 0.1 g of Nioxime in 100 mL of distilled water.
- PHMB solution : take 0.50 g of Vantocil IB and dissolve in 1L of distilled water.
The obtained solution is at 500 ppm Vantocil IB and consequently at 100 ppm
PHMB. This is the solution A.

Remark : It is compulsory to use distilled water because tap water does not give
good results.

Scaling preparation :
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The range ismade of 4 solutions with the following concentrations : 5, 10, 15 & 20
ppm of PHMB. In 5 measuring flasks of 100 ml, sample the volumes of solution A
given in the following board and complete up tp 100ml withdistilled water. Obtained
PHMB final concentrations are precised on the second line of the board.

Flask number 1 2 3 4 5
Solution A volume(ml) 2 5 10 15 20
PHMB final conc. 2 5 10 15 20

Then sample 50 mL of each solution to which you should add 1ml of nickel solution.
Homogenise well the solution & wait for 3 minutes. Then add Nioxime solution (1 mL),
as precedently and shake the solution well. After this step the solution is getting
coloured. The resting time between the addition of nioxime solution and the UV
spectrum must be the same for all samples. It can be chosen by the operator but
must be above one minute.
Solution must be UV screened under 2 different length waves : 550 nm that is the
maximum absorption peak and 620 nm that enable to make a correction that is
necessary to get exploitable results and also to get a good repeatability.

Remark : a mixing at 0 ppm in PHMB with only Nickel & Nioxime solutions should
not be done because it is not usage for dosing because of the non homogeneous
colouration.

Sample analysis

Dissolve a tablet of 15g (5.34% in weight of PHMB) in a flask of 1 L. Fill until

the line of gauge with distilled water. A tablet, being planned to dissolve in 1000L,
it
’st husnec es saryt o mi xf r
om 15 t o 30 mi nut est he s
olut
ion wi
th a magnet ic
mixer. to dissolve it to the maximum. Nevertheless there are particles in
suspension, it is thus necessary to filter the solution.
The obtained filtered solution being at 800 ppm, what is outside the range of
the right of calibration, it is necessary to dilute it by 100.
For that purpose, take 5 mL of the filtered solution and dilute them in the phial
of 500 mL. Fill until the line of gauge with distilled water.

Take 50 mL of this solution, activate the chronometer during the addition of 1

mL of Nickel solution. Shake a few seconds.
After three minutes, add 1 mL of Nioxime solution. Shake a few seconds. Two
minutes after this last addition, launch the UV analysis.
It is very important to respect the released time between every addition.

It is preferable that the product quantity allows to make the analysis at least
three times.

Remark: in case the analysis of the product would not require preliminary dilution, if
the presence of water not distilled in its composition is too important, it cannot be
analyzed.