Alkalinity notes

advertisement
Alkalinity notes
1. Setup instrument
 Turn on titrator on back of instrument
 Turn on carousel
 Open Titramaster 85 software Login: uc merced Password: titration
 Supervisor mode needs to be initiated for changing certain parameters when performing setup.
You can keep instrument in supervisor mode but you can change back to working mode if you
do not want anyone messing with instrument properties.
o Highlight working mode > hold down STOP button > enter password (test) > exit
o Highlight Return in mode > enter to change > confirm
 Changing reagents
o Install reagent > new reagent > bottle exchange > calibrate reagent
 Make sure a cup is in place to catch reagent flowing out!
 Hit stop to stop reagent from coming out after a few ml have been dispensed
 Reagent recipe 0.01M HCl. HCl is stored in acid storage in lab. Look for bottle
with Conklin label.
 Install new electrode (if needed)
o Disconnect old electrode, connect new electrode, or replace electrode
 Calibrate electrode
o > Run calibration. Pour buffer solutions into sample cups (pH 4, in position 1, pH 7 pos.
2, pH 10 pos. 3). Sequence will start with 2 rinse cycles in position 19-20, then to each
buffer.
o Calibration will automatically be updated after pH 10 cycle has completed.
 Instrument is ready to run if all face icons on titrator are smiling
o If you have gone through this procedure, and instrument is not displaying happy face,
try calibrating reagent and/or installing new electrode again. Keep doing one or the
other until instrument is happy 
2. To change method (if needed, not typically necessary to change method)
 Highlight working mode, hit enter
 > Method
 Select method > Gran_Alk is the method used for low alkalinity and has been programmed into
the instrument
 Change Working mode back to SAC Sequence.
3. To run samples
 Sequence is set up to run 18 individual samples, 6 samples x 3 reps = 18
 Sample prep
o Filter samples 0.45 um for alkalinity, non-filtered for acid neutralizing capacity
o





Measure out 25 ml volume. If a precise balance is available, you can measure out 25 g to get
ml.
o Run each sample in triplicate
o Place sample cups in carousel
To change # of samples or sequence Sequence/Sample Stack > Edit sequence > highlight # of
samples and enter change
Position 19 and 20 are always DI! These are the electrode rinse cups.
To run sequence > Run “Sequence SAC”; make sure SAMPLE CHANGER IS ON or you will get a
communication failure!
Test will initialize (5 min stirring time) before starting analysis. This allows pH sensor to
equilibrate.
Samples will take about 10-15 min per cup, dispensing 0.4 ml of titrant until pH gets to 3.
4. Titramaster software readout
 As samples are running, you can see the pH/volume titration curve
 Once the endpoint has been reached, you can export your data to the Master titration excel
spreadsheet located on the computer desktop or on the digital library.
https://eng.ucmerced.edu/snsjho/files/MHWG/Laboratory/Alkalinity?sort_on=id&sort_dir=asc
 Open up titration curve > right click on curve plot > export to Excel > save to folder on desktop
5. Alkalinity/ ANC calculation
 The Gran alk method is used in this spreadsheet since results are typically very low for Sierra
mountain water samples.
 Open alkalinity titration template spreadsheet: “Master Alkalinity Template”. Located on DL or
desktop of titration computer.
 Copy and paste pH and vol data into template, save as. Copy and paste all 3 replicates into one
spreadsheet using different tabs.
 Once the data has been input to the spreadsheet, an alkalinity value is calculated for you! Do
this to all 3 replicates and calculated an average and standard deviation.
Download