Hanna Instruments HI 903 - Manual (Page 191)

Method ID: HI8301EN
Moisture Determination in Solvent with 5 mg/mL Titrant (One-Comp.)
for external dissolution or extraction
Titrator Application Methods: General Methods - r. 0.4
Description:
Method for the determination of moisture in
extraction/dissolution solvent using 5 mg/mL One-
Component Titrant. The results are expressed in %
mass and should be less than 0.1%.
Electrode:

HI 76320 Double Platinum Pin Electrode
Reagents:

5 mg/mL One-Component KF Volumetric Titrant

Dry Methanol
Other Accessories:

A clean, dry 1-mL syringe

A clean, dry 22-gauge , 6” non-coring septum
penetration needle

GL 45-Thread Solvent Bottle
Titration Procedure:

Setup titrator according to the instruction manual.
 Press “Select Method” from the main screen. Use
t
he arrow keys to highlight ‘HI8301EN Solvent w/
5mg/mL 1-comp. ’ and press “Select”.

Install a 5-mL burette filled with 5 mg/mL One-
Component KF Volumetric Titrant and verify that
no air bubbles are present in the burette or tubing.
If necessary prime until all air has been removed
completely.
For the determination of the exact concentration of
the titrant, follow HI8001EN 5.0 mg/mL Titrant
Standardization using Liquid Water Standard.

Connect the solvent bottle top assembly to the
bottle of methanol according to the manual.

Prepare the titration vessel according to the
manual. Dispense enough solvent from the solvent
bottle t
o fill the vessel to the “min” line (about 50
mL).
 Press “Start/Stop” to pre-titrate the solvent and the
titration vessel moisture. Allow the background
drift rate to stabilize before proceeding to the next
step.

Stop stirring the solvent in the extraction/
dissolution bottle.

Fill the syringe and needle with the
extraction/dissolution solvent.

Weigh the syringe, needle and solvent.
 Press “Start Analysis”. You will be prompted to
enter the sample size.

Dispense 0.7500 g to 1.0000 g of solvent into the
titration vessel through the septum using the
needle. Pay attention not to get any solvent on
the electrode or beaker walls. If necessary swirl
the titration vessel by hand.

Clear the needle of residual solvent by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of solvent is seen on the end of the
needle, dip the end of the needle briefly in the
titration solvent.

Remove the needle from the titration vessel and
weigh the syringe again in order to determine the
added sample mass (by difference of the two
measurements.)

Use the numeric keypad to enter the exact weight
and press “Enter” to start the analysis.
 At the end of the titration the “Sample Analysis
Result
” screen is displayed. The results are
expressed in % mass of water. Record this value
as the “External Solvent Concentration”.
Method Parameters:
Name: Solvent w/ 5mg/mL 1-comp.
Method Revision: 1.0
Type: Sample Analysis
Predispensing Amount: None
Pre-Analysis Stir Time: 0 Sec
Stirring Speed: 900 RPM
Stirbar Type: Medium
Drift Entry: Automatic
Solvent: Methanol
Sample Parameters:
Sample Determ.: Normal
Sample Name: Solvent
Sample Type: Mass
Sample Size: 1.0000 g
Titrant: Composite 5
Titrant Type: One Component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.: 5.0000 mg/mL
Date/Time: Jan 1, 2011 12:00
Titrant Age Reminder: 2d:00h:00m
Control Parameters:
Start Mode: Cautious
Standby Mode: Enabled
Standby Duration: 720 minutes
Imposed Current: 20 uA
Minimum Dose: 0.2500 uL
Maximum Dose: 5.0000 uL
Timed Increment: 1 second
End Point Value: 180.0 mV
Signal Averaging: 3 Readings
Flow Rate: 10.0 mL/min
Termination Parameters:
Maximum Duration: 600 sec
Maximum Titrant Volume: 5.0000 mL
Term. Criterion: Relative Drift
Relative Drift: 10.0 ug/min
Result Unit: %
Calculations:
Titrant units: mg/mL
Titrant volume consumed: V (mL)
Final results units: % Mass
Titrant concentration: 5.0000 mg/mL
Sample mass: 1.0000 g