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ISO/WD
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samples with a high chloride content, weigh a smaller test portion e.g. 5 g of
reconstituted or RTF product
.
7.3
Transfer 2,5 ml precipitating solution I (4.3) and 2,5 ml precipitating
solution II (4.4) into the tube. Complete to 50 ml with water. Mix well. If foam
impacts the constant volume, one or two drops of defoaming agent (3.12)
shall be used.
7.4
Centrifuge at 12 000
g
for 5 min at 4°C. Then equilibrate to room
temperature.
7.5
Accurately transfer either 10 ml supernatant from steps 7.2 to 7.4 or
weigh an appropriate aliquot of RTF or reconstituted powder (e.g. 25 g
accurate to 0,1 mg). For samples with a high chloride content, weigh a smaller
test portion e.g. 5 g of reconstituted or RTF product.
Into a 120 ml sample beaker or autosampler cup. Add 5 ml nitric acid solution (4.5), and 50 ml of
water before titration. Add a magnetic stirring rod (if the titrator does not have a build-in rod
stirrer). Place the autosampler cup or beaker onto a magnetic stirrer and stir until dissolved or
finely suspended.
7.6
The pH of the test solution shall be below 1,5. In case of any doubts,
check by means of a pH-meter and, if necessary, add a little more nitric acid
solution (4.5).
8
Instrument operating conditions
8.1
Check and maintenance of the combined silver electrode
Rinse electrode with deionized water and wipe before use. Renew the electrolyte 1 mol/l KNO
3
(4.9) periodically per manufacturer’s recommendations. If fat sticks to the electrodes during a
series of analyses, then eliminate it by briefly immersing the electrode in acetone. The silver
electrode shall be stored in 1 mol/l KNO
3
(4.9) or per manufacturer’s recommendations after
appropriate cleaning.
NOTE: In place of the combined silver electrode, separate silver and reference electrodes may also
be used.
8.2
Titration
Connect the combined silver electrode to the titration apparatus, according to the manufacturer's
indications. Ensure that the titration vessels are correctly placed on the autosampler and there are
enough reagents: both nitric acid solution (if added automatically) (4.5) and 0,1 mol/l AgNO
3
(3.7
or
[J-CTS5
]4.1). If no autosampler is available, then place the sample solutions manually under the
titration equipment.
Put the wash solution (4.6) in the washing position if an auto sampler used. Ensure that the volume
of wash solution is adequate.
Under continuous stirring and without touching the electrode, titrate the sample solution
automatically with 0,1 mol/l standardized silver nitrate solution (3.7 or
[J-CTS
6]4.1), up to the end
potential. The consumption of 0,1 mol/l of silver nitrate solution should be recorded automatically
and can be read from the titrator software, or documented in the titrator operating records. For
manual titration, using a burette add 0,1 mol/l standardized silver nitrate solution, until the end
potential has nearly been met. Then continue to titrate slowly until the end point is met as
observed by the two small (about 0,05 ml) silver nitrate solution.
Special case: determination of very low amounts of chloride
2016.03 (APRIL 2017) - MTE-01/03
MLT REPORT
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