I would like to know what would be a good method development for the analysis, as my previous method has resulted in no results appearing for the Mg analysis.
Hi did you check APHA method ? APHA chapter 3120 - Metals by Plasma Emission Spectroscopy, Method B - Inductively Coupled Plasma (ICP) Method.
Here is the link, hope it helps.
https://law.resource.org/pub/us/cfr/ibr/002/apha.method.3120.1992.pdf
In ICP-OES 2100DV Perkin Elmer
I use for Ca 317.933 nm wavelenght and for Mg 285.213 nm! Plasma view Attn Axial.
Twister Spray Chamber with Helix 50 ml cyclonic.
Plasma 15 L/min
Aux 0.2 L/min
Neb 0.65 L/min
Power(watts) 1300
Sample flow rate 1.5 ml
My results for QC VKI DWB
http://www.eurofins.dk/media/2837/dwb-16-8_9-0510_uk.pdf
G'day Andreea,
I'll start from the start, forgive me if you've already done these. Sample introduction is the main area where problems occur. Check and/or replace the pump tubes and look to see if you're getting spray into the spray chamber. Instrument parameters can be obtained from the manufacturer initially. For axial, analysing surface and groundwaters, you could try:
Power - 1.20 kW
Plasma flow rate - 15 L/min
Auxillary flow rate - 1.5 L/min
Nebuliser flow rate - 0.9 L/min
Replicate read time - 10 s
Instrument stabilisation time - 25 s
Sample uptake delay - 40 s
Pump rate - 15 rev/min
Rinse time - 45 s
Measurement repeats - 3
Use at least 2 lines per element, for Ca and Mg you could use:
Ca - 317.933 and 315.887
Mg - 279.800 and 285.213
Troubleshoot and check the instrument with undigested samples, to rule out the digestion as a source of error. When you're sure the ICP is giving what you should be getting by analysing some known samples eg. preparing known standards and/or external CRMs or RMs, then there are plenty of sources of information on the method development process. I hope this helps and good luck.
Cheers,
Adam
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