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9-8
METHODS OPTIMIZATION
9.2.4
Liquid Samples
The water contained in liquid samples must be available to react with the KF reagent. It is
important to select a reagent or co-solvent with which the sample is miscible.
Liquids are typically added through the septum in the sample port via a syringe and needle
using the following steps:
1. Attach a long needle (approximately 6” long, 21-gauge) to a syringe large enough
to hold at least one complete sample volume.
2. Rinse the syringe and needle with sample several times by drawing in a small
portion of sample, fully extending the plunger, shaking to coat the syringe interior
and expelling the sample into a waste collection container.
3. Draw enough sample into the syringe for at least one titration.
4. Dry the outside of the needle with a lint free wipe or tissue.
5. Determine the mass of the syringe and sample.
6. Initiate a titration from standby mode by pressing the ‘start analysis’ option key.
7. Insert the needle through the septum in the sample port. Push the syringe through
the septum until the end of the needle is approximately 1 cm from the surface of
the solvent.
8. Steadily dispense the contents of the syringe ensuring that the sample is introduced
directly into the solvent and does not splash or spatter onto the wall of the titration
vessel electrode or dispensing tip.
9. Draw a small amount of air from inside the cell into the syringe to ensure that no
sample drops remain on the tip of the needle.
10. Remove the syringe and needle from the septum taking care to not touch the
needle to the solvent or other internal cell components.
11. Determine the mass of the syringe and needle.
12. Calculate the mass of the sample added to the titration cell (subtract the mass of
the syringe after the sample has been added from the mass of the syringe before
sample addition).
13. Enter the calculated mass of the sample into the
HI 904
.
14. Start titration using the option key ‘start analysis’ from the add sample screen.
As indicated above, when adding a liquid sample with a needle and syringe, it is important
that the sample is introduced directly into the solvent. Sample that is deposited on the sides
of the vessel or other internal components of the cell may not be titrated with the rest of the sample.
It is equally important that no drops remain on the tip of the needle. ‘Hanging drops’ will end
up on the bottom of the septum. This will result in false low results for the determination.
Liquid samples with high viscosity may be careful warmed to improve the flow through the
needle.
In some cases liquid samples may require one of the additional preparatory steps listed in
the sections that follow. Specific sample preparation instructions are included with each
standard method.
Summary of Contents for HI 904
Page 1: ...1 QUICK START GUIDE HI 904 KARL FISCHER COULOMETRIC TITRATOR Revision 1 0 www hannainst com...
Page 4: ...4 QUICK START GUIDE...
Page 7: ...7 QUICK START GUIDE TITRATOR CONNECTIONS Front View Rear View...
Page 17: ...1 INSTRUCTION MANUAL HI 904 KARL FISCHER COULOMETRIC TITRATOR Revision 1 00 www hannainst com...
Page 20: ...4...
Page 22: ...1 2 INTRODUCTION...
Page 24: ...2 2 SETUP...
Page 27: ...2 5 SETUP 2 3 Installation 2 3 1 Titrator Top View...
Page 28: ...2 6 SETUP 2 3 2 Titrator Rear View 2 3 3 Titrator Left side View...
Page 38: ...3 2 USER INTERFACE...
Page 46: ...3 10 USER INTERFACE...
Page 48: ...4 2 GENERAL OPTIONS...
Page 82: ...5 24 METHODS...
Page 84: ...6 2 TITRATION...
Page 94: ...6 12 TITRATION...
Page 96: ...7 2 AUXILIARY FUNCTIONS...
Page 104: ...8 2 MAINTENANCE PERIPHERALS...
Page 112: ...8 10 MAINTENANCE PERIPHERALS...
Page 124: ...9 12 METHODS OPTIMIZATION...
Page 125: ...A3 2 APPENDIX 3...
Page 126: ...A3 6 APPENDIX 3 MAN HI904 09 13...
Page 127: ...A1 1 APPENDIX 1 Appendix 1 Contents A1 TECHNICAL SPECIFICATIONS A1 3...
Page 128: ...A1 2 APPENDIX 1...
Page 132: ...A2 2 APPENDIX 2...
Page 134: ...A2 4 APPENDIX 2...
Page 135: ...A3 1 APPENDIX 3 Appendix 3 Accessories A3 TITRATOR COMPONENTS A3 3...
Page 136: ...A3 2 APPENDIX 3...
Page 140: ...A3 6 APPENDIX 3 MAN HI904 09 13...
Page 141: ...1 GENERAL APPLICATIONS BROCHURE HI 904 KARL FISCHER COULOMETRIC TITRATOR www hannainst com...
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Page 144: ......
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Page 150: ...2 TITRATION THEORY...
Page 166: ...18 TITRATION THEORY A B Figure 8 Potential glass electrode mV C...