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Generally, the slope is ~59 mV at 25°C. Slope is determined during calibration.
The function F, when plotted as a function of the volume of acid added (v), is linear when sufficiently removed from the equivalence point. We measure mV instead of pH to determine the endpoint because this method offers better precision. The optimum range of millivolts for linearity is 220–240 mV. The value of v at F = 0 is the equivalence point from which the alkalinity is evaluated.
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Before an electrode can be used, it must be calibrated against pH buffers in the range expected in samples. Generally, calibration at pH 4, 7 and 10 covers the necessary range. Make sure the gray side-hole plug for the electrode is unplugged before starting a measurement.
- Make sure the water bath temperature is set to 25°C. Ensure no air bubbles are present in the acid dispensing line. Press DOS on the body of the titrator to push acid through the line to remove potential air bubbles. Select Calibrate Electrodes from the Main instrument panel.
- Enter your range of buffers (4, 7, 10).
- Select your Drift Span. The default drift span is 30.
- Place 3 mL of the first buffer solution in the vessel. Add stir bar. Remove the electrode from the storage solution, rinse with DI water, and blot dry with a Kimwipe. Do not rub the electrode, as this can cause a static charge. Insert the electrode tip into the titration vessel (not touching the bottom of the cup or the stir bar). Confirm that the frit is in the solution.
- Select Cal 1 and then Start. Measure until the drift gets close to 0.0. Usually approximately 500 seconds will be adequate. Select Stop when satisfied with measurement.
- When finished, clean vessel and the electrode.
- Repeat steps 4–6 with each calibration buffer, selecting Cal2 and Cal3 when appropriate.
- When all three buffers have been run, the slope value of the regression curve should be close to –59 pH/mV. Select OK-Save to save the calibration.
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The rate at which the titrator dispenses acid into the sample can be adjusted according to the expected alkalinity value. Higher alkalinities may require faster dispensing rates. The dispensing rate can be selected from a list of predetermined programs or a new dispensing rate program can be created.
Select Edit Rates from the Main instrument panel.
To create a new rate program:
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Make sure to select a correct dispensing rate program for the standard in question. You can access the rates by selecting Edit Rates from the Main instrument panel.
Before any measurement, press the red STOP/FILL button on the titrator itself. This will fill the syringe pump and ensure you will not run out of acid during the titration.
To start creating a standard ratio correction, select STANDARDS from STANDARD from the Main instrument panel.
- Place 3 ml of standard in vessel. Add stir bar and immerse electrode in vessel. Confirm that the frit is in the solution.
- Select Continue.
- Click START.
- Insert the acid dispensing probe when prompted.
- When finished, clean vessel and electrode. Repeat steps 1–4 until you have at least three consistent measurements per standard.
Now go to the STND Manager, selected from the Main instrument panel.
- Select the three measurements you want to average and click Average.
- The window to the right shows the next step in which you can save the new standard ratio correction or replace an old one. Usually we save as a new ratio (e.g. 371_13august). The window showing the name creation is not shown.
- Click Done.
To select a standard ratio correction for subsequent measurements go to Setup in the main alkalinity interface.
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Before any measurement, press the red STOP/FILL button on the titrator itself. This will fill the syringe pump and ensure you will not run out of acid during the titration.
Select SAMPLE from the Main instrument panel.
Select the sample (IWS) from LIMS tree. Alternatively, type or scan in a Text_ID. If you use a Filter Code IWS, the software will only bring up the IWS sample, which can be handy if your IW has a lot of children.
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The Gran-Method window appears with the results of the titration. Write the pH and the Alkalinity Cor value in the blue book. This is the result with the standard ratio correction applied to it. Click Ok/Save. This will upload the result to LIMS assuming the MUT uploader is active.
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