The components of the OI Analytical Flow Solution IV Automated Ion Analyzer are an X-Y-Z random access autosampler (RA Sampler), a Model 502 multichannel peristalic pump, a two channel Expanded Range (ER) Detector, a Power Base, a Windows compatible computer with WinFLOW V4 software and a printer. The FS-IV segmented flow analysis is a process by which a quantity of analyte is measured in a continuously flowing stream of sample that has bubbles injected consistently throughout, ensuring complete mixing and minimizing dispersion. The SFA configuration introduces successive samples into a path where reagents are added, mixed and heated to generate a measurable photometric reaction.
II) Manifold Installation
A) Select the appropriate cartridge for the method to be analyzed.
B) Install the appropriate interference filter.
C) Verify that the analytical cartridge is configured as illustrated in the flow diagram.
D) Connect the appropriate pump tubes to the cartridge, their appropriate reagent containers, the ER detector and the waste container.
E) Connect the autosampler rinse pump tubes to deliver deionized water through the wash reservoir and then to waste.
III) Instrument Setup
A) Switch ON the master power strip for the autosampler, pump, ER detector, computer, and printer. Power ON autosampler, power base and computer.
B) Power ON heater, if indicated. Allow 15 minutes for temperature stabilization.
C) Open the WinFLOW V4 software program.
1) Select the appropriate Method. Verify that all settings are correct.
2) Select the appropriate Sample Table. Edit the table as needed.
3) Select Data Collect.
4) Enter an Operator identification and password.
5) Create a filename as C:\FLOW_4\year\month\YYMMDD.rst
D) Load the pump tubes and platens onto pump rollers, ensuring that the platen latches are properly engaged. Power on pump at 40% speed.
E) Clean the system by pumping the appropriate cleaning solutions through the sample line and reagent pump tubes.
F) Stabilize the instrument by pumping start-up solution through the appropriate reagent pump tube and deionized water through the sample line and other reagent lines for 10 minutes.
Select Play to initiate data display and monitor the baseline. Verify that the baseline is stable.
NOTE: A stable baseline absorbance is less than 100 uAU for vertical noise and less than 200 uAU/300 seconds for drift. Sharp fluctuations or consistent drifting in the baseline are signs of bubbles in the flowcell. Force start-up solution through the flowcell to clear out any bubbles.
G) Place reagents on line and pump for 10 minutes. Verify that the baseline is stable.
H) If a cartridge with an Open Tube Cadmium Reactor is in use, turn pump off and place the OTCR in line. Pump reagent for 5 minutes. Verify that the baseline is stable..
Note: Never pump air through an OTCR.
IV) Calibration Procedure
A) Calibrate with standards that bracket the sample concentrations.
B) Review calibration.
1) Select Calibration Plot to view graph. Select Calibration Results Table. Correlation coefficient should be greater than or equal to 0.990.
2) Clear calibration level(s), if necessary, by replacing C (Calibration standard) with U (Unknown) as the Type.
3) Recalibrate one or all levels, if necessary.
4) Print Calibration Results Table.
5) Confirm calibration with accuracy and precision controls.
C) Check calibration curve for drift, accuracy and precision with standards and controls every 20 samples.
B) Verify that all reagents are on-line and that the baseline is stable. Autozero the baseline.
C) Load sample tray with calibrants, samples, blanks and controls according to tray information.
1) Cup: Autosampler cup location
2) Name: Name of standard, sample, control and blank
3) Type: Sample Type (C=Calibrant, U=Unknown, Blank, RB=Read Baseline, CO=Carryover)
4) R: Number of Replicates
5) Dil: Dilution factor of sample
D) Select the Fast Forward icon to initiate the sequential analysis of samples.
NOTE: The SYNC peak initiates the peak recognition process.
G) Select Stop at any time to manually terminate the run. Save previously displayed data, if indicated. Select Rewind to reset. Select Play and Fast Forward to reinitiate data display and sample analysis.
H) Select Pause to modify the active portion of the Sample Tray Editor. Press Play to continue analytical run.
I) Modify the inactive portion of the Sample Tray Editor with additional standards, samples, controls and blanks as needed. Load sample tray appropriately. Close and save the Sample Tray Editor
NOTE: The analytical run will pause if the Sample Tray Editor is open and all samples from the active tray have been analyzed.
J) The analytical run will automatically stop if the Sample Tray Editor is closed and all samples have been analyzed.
B) If an Open Tube Cadmium Reactor is in use; turn off the pump, take the OTCR off-line and restart the pump.
C) Pump start-up solution through the appropriate reagent pump tube and deionized water through the sample line and other reagent lines for 10 minutes.
D) Stop the pump. Release tension on all pump tubes.
E) Close all files in the WinFLOW software. Exit Windows. Turn OFF computer.
F) Power OFF the system.
KIOWA CHEMISTRY LABORATORY Procedure Manual
Last Rev. 08 May 2007 by: Chris Seibold