ICP-OES Detector and Instrument Calibration

This Information Applies To: Agilent 5000 Series ICP-OES (5100, 5110, 5800, 5900)

Issue

How to calibrate the ICP-OES

ICP-OES calibration is a two-step procedure:

1. The detector calibration performs a dark current calibration to correct for detector and electronic background signals.
2. The instrument calibration uses a specified calibration solution to calibrate the wavelengths of the polychromator.

ICP-OES wavelength calibration solution is available as either Agilent ICP-OES wavelength calibration solution Ready to use (part number 6610030100) or Agilent ICP-OES wavelength calibration solution concentrate-dilute 1:10 before use (part number 6610030000). Alternatively, it can be prepared as per Agilent ICP-OES, Preparing the Instrument Calibration Solution.

Tips: An instrument calibration needs to be performed the first time the instrument is run, when new software is loaded, when drift correction lines are added or removed, and when the polychromator purge gas is changed. The gases that can be used for purge are either Ar or N2. It is recommended that an instrument calibration be performed monthly thereafter.

Detector calibration steps to follow

1. Turn off the plasma.

2. Turn on the water chiller. The calibration will not begin until the camera temperature is below -40 °C.

3. From the ICP-OES home page, select Instrument > Calibration and under the Detector heading click Calibrate (Figure 1).

   
   Figure 1. Detector Calibration

4. The Instrument Calibrate button will not be available until the detector calibration is completed.

Instrument calibration steps to follow

1. Complete a detector calibration before the instrument calibration.

2. Turn on the plasma, and allow to the temperature to stabilize. This step typically takes approximately 20 minutes, however if the instrument has been turned off for an extended time, it may take longer.

3. Purge the polychromator and the snout for about 20 minutes before starting the calibration and leave on during the instrument calibration. The purge can occur while the instrument temperature is stabilizing. From the ICP-OES home page, select Instrument > Status and under the Purge heading select check boxes Boost and Snout (Figure 2).

   
   Figure 2. Instrument Purge

4. Adapt systems configured with AVS 6/7, AVS 4, and autosampler for manual sample introduction. Replace the rinse/carrier supply tubing from the inlet end of the peristaltic pump tubing with tubing that can be immersed in the calibration solution.

   Tips: Manual sample introduction allows for continuous flow during the length of the calibration. AVS systems are optimized for sample throughput and may have insufficient sample measuring time.

5. Aspirate the calibration solution.

6. Determine the appropriate calibration mode:

   1. Default radial calibration. 

   2. Axial calibration. Use for VDV/SVDV configured instruments.

   3. Organic wavelength calibration. Use for wavelengths and settings specific to organic analysis.

7. Start the calibration: From the ICP-OES home page, select Instrument > Calibration and under the Instrument heading select the appropriate calibration mode check box, then select Calibrate.

   
   Figure 3. Instrument Calibration

8. The instrument will complete the calibration and report onscreen calibration results. Wavelengths that fail will be flagged. 

9. If calibration fails, follow these guidelines:

   1. Failure at low UV wavelengths (e.g. Al) may indicate that the polychromator and snout purge are off, or there has been insufficient purge time. Rerun the calibration after a longer purge time.

   2. Failure across a wide range of wavelengths may indicate problems with either:

      1. Sample introduction components. Check the sample introduction system and repeat the calibration.

      2. Calibration solution problems. Prepare a new calibration solution and repeat the calibration.

10. After the instrument has passed the calibration, aspirate rinse solution to thoroughly clean the sample introduction system.

11. Reattach the AVS 6/7, AVS 4, and autosampler, if applicable.

Tips: Agilent recommends performing the detector and instrument calibrations monthly.

Learn how to effectively maintain and operate your Agilent ICP-OES: ICPOES-EX-1100e - Agilent 5110 ICP Expert Software Part 1 (Ver. 7.4) ICPOES-EX-1130e - Agilent 5000 Series ICP-OES: Introduction to ICP Expert Software (Ver. 7.5) e-learning courses available from Agilent education