Introduction

Preparing Reagents, Standards and Samples

Reagents

Dosino Reservoir:

DI water

Suppressor Rinse Solution:

0.1% methanol in DI water

• • 1 mL methanol to 1 L DI water

Suppressor Regenerant Solution:

0.05 M sulfuric acid solution

• • 2.7 mL sulfuric acid to 1 L DI water

Anions Eluent:

3.2 mM sodium carbonate/1.0 mM sodium bicarbonate solution

• Metrohm “A Supp 5 Eluent Snips”
  • pour contents into a 1 L volumetric flask
  • rinse the tube with DI water, adding to the flask
  • bring flask to volume

Cations Eluent:

1.7 mM nitric acid/1.7 mM PDCA (pyridine-2,6-dicarboxylic acid)

• dissolve 0.248 g PDCA in DI water in a 1 L flask
• add 106 µL concentrated trace metals grade nitric acid
• bring flask to volume with DI water.

To make a carboy’s worth:

• in a 2 L volumetric flask, mix 872 µL nitric acid, 2.272 g PDCA with DI water and bring to volume. 
• This may involve using a stir plate with a stir bar in the flask. Pour into the carboy.
• Add three more 2 L flasks filled with DI water.  

Standards

Prepare a standard curve, 10 mL per level, in IC vials:

• • Make sure that the vials are vortexed before analysis.

To add/edit standards, select the METHOD panel and Standards in the Evaluation window. Here you can also add/edit check standards information.

Samples

All samples are diluted 1:100 with DI water.

• • Make sure that the vials are vortexed before analysis.

Instrument Operation

Startup

1. Load a method (sets instrument’s operational parameters).
   • Select METHOD icon in left panel. 
   • Select File -> Open -> select the method. 
     • You can then save the method with a new name for the current Expedition (File -> Save As).

2. Make a new database for the Expedition (saves results in a central Expedition database)

• • • Select DATABASE icon in the left panel. 
    • Select File -> Database Manager. 
      • Select Edit pulldown then New. 
      • Type in a new name.
    • Here you can also make a database backup. 
      • Select Database Manager again and Backup, giving a unique Expedition name.
    • Go back to the METHOD panel. 
      • In the Evaluation window, click on Results icon. 
      • Select the Database tab. 
      • Double-click on the Name Database field and select your database name for the Expedition.

3. Go back to the WORKPLACE icon in the left panel.

• • Select the method that you want the instrument parameters to be set at (Equilibrium tab).

4. Confirm all reagent reservoirs are filled, peristaltic pump tubes are in good shape and their platens are engaged.

5. To start the instrument, select Equilibration tab > Start HW button.

• To shut down the instrument, select the Stop HW button.

 6. Monitor instrument conditions (Watch window) for ~ 60 min before starting a sequence.

• • • The anions baseline should be ~ 1 µS/cm. Suppressor may cause a small peak every 10 min or so. 
      • The anion pump pressure should be around 6.5 – 7.0 MPa.
    • The cations baseline should be ~ 870 µS/cm. 
      • The cation pump pressure should be around 4 – 4.5 Mpa.
    • The column thermostat display appears red until reaching 45°C. 
      • Allow the columns to come to temperature before starting sequence.

Sequences

1. To set up a sequence, select the WORKPLACE panel and Determination Series tab.

2. To create a new sample table, use the dropdown menu Sample Table -> New.

• • Go to Sample Table drop-down and select Properties. 
  • In the Display tab, make sure that the Value 1 radio button is checked. 
  • Now go to the Edit tab and make sure that the Value 1  radio button is checked.
  • Double click the first row to start populating the sample/sequence table. 

The table should follow a basic guideline as follows (see Figure 1). 

• • • The calibration standards will come first.
    • Followed by the blank(DI used as a sample).
    • A check standard.
    • Then the samples.
    • Checks every ten samples or so.

Figure 1 : Sample/sequence table example

Evaluating Results

LIMS

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