Leeman Labs Prodigy ICP Brief Directions

Department of Chemistry, TuftsUniversity

Leeman Labs Prodigy ICP Brief Directions

These directions cover only the bare minimum. For further information refer to the Prodigy Operations Manual, particularly Chapter 3, “Quick Start Tutorial”.

There are two frames in the Salsa ICP software window. The left frame (Navigation Panel) has three tabs- , , and that control method parameters, Autosampler use, and Data acquisition respectively. When the tab is selected, the right hand frame (Detail Panel) has additional tabs;

The sequence of events is:

Check and address and issues→Ignite Plasma →Open or Create Method→ Autoalign Hg Lamp→ Align other lines→ Position Plasma→ Run Standards for Calibration→Run Samples→Print Report

Turn on Procedure

Turn on Argon. Confirm pressureis 80 psi. Argon may be from compressed gas tank or liquid argon dewar.

Check that nitrogen for camera purge is on, about 80psi.

Turn on water circulator under the bench(cools the coil).

Clamp the pump tubing down on the peristaltic pump. Don't turn the knobs

Check that the blast gate above the fume extractor is open (It is normally kept open)

Turn on the instrument, if not already on (it is normally left on, with low purge). If the instrument was OFF for more than an hour, it must be powered ON for at least 2 hours before proceeding.

Turn on computer and, monitor if not already on

Check that Spray Chamber drain and Rinse Drain have sufficient free volume available

Select the icon to start the ICP software.

Open Method

Select Method/Open from the menu, or create new method as described below.

Go to Analysis tab. Select Analysis/New from the main menu. Enter a name for the analysis. Select

Creating a new Method

Methods are created and edited from the Method tab in the left hand frame. Select File/New from menu. Enter method name and analysis name

Instrument Control

This tab is used for direct control of the instrument, for example starting the plasma, and for setting pump and rf parameters. The default Plasma, Pump, and RF parameters should work in most cases. Consult the manual before changing. The Axial view is more sensitive, but more prone to interference. Most analyses in ppm range can use radial.

Element Selection

Select element, then select line, usually the one labeled best. Select Add Line button. Always include Mn (257.61) for peaking. Note that elements can be displayed in periodic table or alphabetic order. When element selection is complete, select each element in the Navigation panel list, and select axial or radial in the tab.

Standards/MSA

Select . Enter name, concentration and units (mg/l, ppm, ppb), and number of integrations(usually 3). Select . You should have at least three standards; Blank, low standard (e.g. 1ppm), High Standard (e.g. 10 ppm).

Internal Standards

For optional internal standards (see manual)

Quality Control Checks

Define check standards, if used

QC Automation

Setup calibration standards and check standards if using the autosampler.

Analytical Parameters

This is where you set exposure times, rinse times, number of integrations (usually 3). For high S/B lines and concentration in ppm range, 1 sec exposures will usually be OK. Software allows exposures up to 300sec.

Summaries

This tab contains line fit parameters of most the recent calibration of this method.

General

General information about method; Name, creator, date created, etc

Starting the plasma

Before starting the plasma, confirm that the pump is working. Insert sipper into DI water. In Instrument Controlpage,select pump ON. In about 1 min you will see alternating bands of water and air in the drain tube. DO NOT PROCEED UNTIL PUMP IS WORKING PROPERLY.

In Instrument Controlpage,select. Gas will flow for 60-90 sec before plasma ignites to clear air out of lines.

Autoalign Hg Lamp

Select the Autoalign icon.

Confirm that or Hg Ref is checked.

Select

Select when alignment is complete

Align other wavelengths

Use a sample containing about 10ppm of the element or elements to be aligned.Insert the sipper tube into standard. WAIT 40 sec for uptake. Select the Autoalign icon,. You will need to repeat the Hg Ref alignment.

Check other lines to align. Select .Select when alignment is complete. Values of dx, dy should be no more than +/-2. If 3 or more, and repeat. If still 3 or more contact Dave Wilbur.

Position Plasma

Insert sipper into 10ppm Mn solution. WAIT 40 sec for uptake. From the Instrument Control page, select .When the Position Source window appears, Select the Mn 257.610 line. Select . When the operation is finished, the display will look like the figure at right. When everything was new peak intensities were near 400,000 radial, 2,000,000 axial for 10ppm Mn.

Run Standards for Calibration

Insert the sipper tube into standard. Select Standard icon from toolbar. Select the standard to run, number of integrations, and whether to delay 40 sec for uptake. Select .

The information in the and tabs will update with each standard.

When all standards have been run select to accept the new calibration.

Run Samples

Insert the sipper tube into sample. Select Sample icon from toolbar. Enter a name, Select .The information in the tabs will update with each sample.

Print Report

Select the Tab. Select the Analysis Chapter. Select items to be reported. Select or to create report. Select Output, either , or that can be opened in Excel. For CSV file, enter the file name and select .

Qualitative Analysis

Select the Full Frame icon from the toolbar. Enter a sample name, select .

Select in the section, select the image from the data list. Select to generate a list of likely elements.

Shutdown Procedure

Aspirate dilute nitric acid or DI water for 5 minutes

Click on the button on the Instrument control page to extinguish torch.

Release the pump tubing clamps.

Turn OFFthe water circulator (under the bench).

Turn off Argon at tank, DO NOT turn off nitrogen purge.

Sign log book

Tidy up.

Using the autosampler

Click on the Air button on the Autosampler portion of the Instrument Control page. Insert the sipper tube so the angled portion is just below the lower guide. Tighten the holding screws. Confirm that the autosampler has a 14 tube standards rack in the left position and 44 tube sample racks in the center and right position.

Go to the Instrument Control page. Check the box, and enter a delay of 5 min. This will extinguish the torch at the end of the autosampler run.

Select the tab on the Navigation Panel. Positions on the Standards rack will already be labeled with the names of the standards defined in the method. Put Standard and sample tubes in the racks. Enter Sample ID and Extended ID information in the table for each sample.Select the button to start the autosampler run.

The autosampler can also be used as a sample rack during manual operation. In this case use the Instrument Control page, autosampler section to move the sipper tube to the appropriate position before selecting the Standard or Sample icon from toolbar.

Revised 09/23/2016D. Wilbur Page 1 of 4