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Perkin Elmer ICP-OES calibration curve issue

Discussions about GC-MS, LC-MS, LC-FTIR, and other "coupled" analytical techniques.

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Hello all,

I'm operating Perkin Elmer ICP-OES optima 4300 and I have an issue with calibration curves.

After running the calibration standards, the curves were not shown on the software as I kept getting this message "no calibration curve because standard intensity and concentration values are not in the same order".
We bought the used instrument from this vendor and they sent us the technicians for the installation. This message was not on when they were running the instrument with the calibration standard that I prepared.

I've been testing the instrument on my own and the intensities and concentrations of standards and known samples were always inaccurate. I have requested a service visit from the vendor but they charge me a ridiculous price, and thus, prefer to solve this on my own.

Has anyone on this forum had a similar issue with the ICP-OES? Please share with me how you resolved the issue if you had.

Also, does anyone know a forum for mass spectrometry? I'm aware this forum is for liquid chromatography, so I would like to join if there's a forum for ICP users.

Thank you in advance for your help :)
The lab where I work just got an OES but it's taking forever to get it setup. So I can only make a wild guess. The AA it's replacing would have trouble calibrating sodium and gave a message "Standard number not applied. No calibration because the signs of absorbance and concentration may differ". That would happen it the blank signal was too low. I had to add a small amount of sodium to our calibration blank - well below the reporting limit. Only about 0.1 ppm. Could it be something like that with OES?
I used a PE 4300 for years and I may be able to help, but I'd need more information.

Did the vendor teach you the basics of operation?

- does the plasma look okay?
- is the sample uptake okay?
- are the nebulizer and spray chamber clean?
- have the torch and injector been cleaned?

You can also tell a lot from the data. Is there a way you can upload and link the .txt datafile from an attempted calibration? A .txt version of the method wouldn't hurt either. There should be an option in the software to save the method as text. I'm assuming you're using Winlab32? Alternatively you can send me your email address in a private message.

Just a note: You asked about a forum for Mass Spec. What you're using isn't a mass spectral technique. ICP-OES is optical emission spectrometry. It detects the wavelengths of light emitted from the species in the plasma. ICP-MS is a mass spectral technique but that's a different instrument.
Hello anionman,

I would expect the blank signal to be low as I use it as a washing solution before introducing samples after standards and between samples. But I will try your method by adding an aliquot of interested element solution to the blank. Thank you for your suggestion.



Hello MichaelVW,

Thank you for offering help on this. To answer your questions,

1. The vendor went through a very brief basic of operation. However, I have enough experience operating ICP-MS and used ICP-OES a few times. I’m using Winlab32 software, and I have no problem setting up methods and sample lists.
2. The plasma looks okay.
3. The sample uptake is okay but I’m considering increasing the sample uptake time. It is suggested that I’m getting the error message because not enough sample reaches the plasma. I’m going to test this by increasing the sample uptake time so that enough sample volume can be introduced to the plasma.
4. I found the droplets were building up during the analysis and some residues in the spray chamber. I took out the chamber and cleaned it with the detergent. I confirmed that now it’s aerosols that are introduced to the plasma. I used 2% nitric acid as a washing solution and rinsed the nebulizer for an hour.
5. I couldn’t check the torch and injector by myself but when the technicians came over for the installation, they should have checked those. I will check it on my own to make sure they are clean.

I was trying to send you a private message, but nothing appears after clicking “Contact MichaselVW” on your profile. My email address is j.kang@li-metal.com. It’d be great if you could send me an email and I can share the ICP data. Thank you for your help.
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