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Agilent 5800 ICP-OES
Agilent 5800 ICP-OES
Staff Contact: Rachel Alvelais (ralvelais@lbl.gov)
Instrument Location: 67-4203B
Most Important Principles
Most Important Principles
You must be authorized to work under the "Work on 4th Floor" (MF-0001), "Strong Acids" (MF- ), and "ICP-OES" (MF-0010) WPC activities to operate the instrument.
There can be NO AMOUNT OF FLUORINE in your sample or standards. This is a very strict policy to protect the glass components of the ICP.
Use extreme caution when handling ICP standards and samples. Though the acid content is typically only 2-5% acid, the solutions still have a pH of 1 and can burn skin and damage clothing.
You must inform the staff contact of the elemental composition of your samples, not just the analyte of interest, prior to running your samples.
Your samples must be acidified to 2-5% acid (hydrochloric or nitric acid) for the instrument.
You must send the staff contact photographs of the peristaltic tubing, waste stream tubing, and the glass of the torch, PRIOR to turning the instrument on. Each time.
Your data is only as trustworthy and quantitative as your sample preparation and data treatment! Pay attention to signal-to-noise ratio, RSD, and replicates!
Our new instrument is extremely sensitive and reliable compared to our old one. We encourage everyone to run Quality Control checks during their experimental analysis in order to track precision and accuracy of the instrument. We suggest running QC checks at LEAST TWICE: once, right after your calibration standards finish but before you start running your samples, and then once at the end of your run. IDEALLY you should run QC after every 6-12 samples. Unless you are following EPA protocols, this isn’t necessary but it’s still helpful.
Standard Operating Procedure
Standard Operating Procedure
This video explains how to use the ICP-OES located at the Molecular Foundry. It focuses on instrument and software set-up, including an auto-sampler, but does not describe sample preparation. This instrument uses a 5% nitric acid wash solution and radial + axial view argon torch, and the operating methods described here include tricks we've learned to deal with the quirks of our software package.
5800 New ICP Instrument Manual.pdfA new video guide is coming soon!
For those analyzing for lithium, sodium, potassium:
For those analyzing for lithium, sodium, potassium:
Lithium is a big "Easily Ionizable Element," as are other alkali metals. In order to mitigate the easily ionizable element effect and get accurate quantification of Lithium as well as your other elements, there will be an added step to sample preparation. It helps if you have read (a little bit) about the "EIE" effect on ICP-OES. You don't need to become an expert on it, just understand why it's important to mitigate the EIE effect with cesium in your samples.
We have received a concentrated cesium ionization buffer solution! In order for the Cs ionization buffer to work, you MUST put the SAME concentration of Cs in EVERY standard and EVERY sample. The buffer only works if it is IN VAST EXCESS of the other alkali metals in solution (Na, K, Li, Mg). If you have <100ppm Li or Na in solution, then 500 ppm of Cs MAY be enough. But if you have higher concentrations in your samples, then you need a greater excess of Cs! This paper illustrates that Li concentration readings stabilize in their accuracy when Cs is added in excess of 1000 ppm!
Good starting places:
A major non-spectral interference in ICP-OES is due to easily ionizable elements, particularly group I and group II elements . In ICP-OES the goals is to provide sufficient energy to excite an electron. If more energy is supplied, however, the electron may be completely dislodged, resulting in a cation. As there is no emission of electromagnetic radiation during this process, each atom that is ionized is lost from detection. The net result is a decrease in the intensity of emission lines for that element, resulting in an observed concentration lower than actual. Another major type of non-spectral interference occurs when there is a shift in the equilibrium of the system. This equilibrium exists between the ground state atoms, excited atoms, and ions. The overabundance of an element may shift this equilibrium, affecting the intensity of emission. For example, an overabundance of potassium (K) may cause a reduction in the apparent concentration of sodium (Na). The large number of K atoms may collide with the Na atoms, resulting in an increased signal when compared to a standard solution with a considerably lower concentration of K atoms. (Source.)
And:
The result of the study on elemental combinations clearly shows that the occurrence of ionization interference can be presumed from the magnitude of ionization potentials. After examining the methods for adding low ionization potential elements to both sample solution and standard solution, it was confirmed that ionization interference could be successfully suppressed by adding low ionization potential elements, especially excessive amounts of cesium. (Source)
Information on the EIE effect (for lithium): https://www.tandfonline.com/doi/full/10.1080/00387010701293245
COMMON QUESTIONS
COMMON QUESTIONS
Q: The chiller is alarming!
Q: The chiller is alarming!
A: The chiller is likely alarming for ambient air temperature. Silence the alarm, then make sure the black floor fan beside the chiller is on and pointed out from underneath the lab bench. If there is not enough air flow from under the bench with the chiller and the rest of the room, the chiller alarms at 88°F. If the chiller continues to alarm, silence it again and pull it out from under the bench so that it has more airflow to the rest of the room. If it continues to alarm, call the staff member in charge.
Q: I have a little tiny itty bitty amount of fluorine in my samples. I know I cleaned it well, so is it okay to measure it on the ICP now?
Q: I have a little tiny itty bitty amount of fluorine in my samples. I know I cleaned it well, so is it okay to measure it on the ICP now?
A: NO AMOUNT OF FLUORINE is allowed to be run in the ICP. This includes LiPF6, LiPFSI, etc. Even minor amounts react with your acid to form HF, which eats away at the nebulizer and torch. A nebulizer costs over $1,000.
Q: My samples won't digest/will precipitate in acid, can I dilute them with pure water? With base?
Q: My samples won't digest/will precipitate in acid, can I dilute them with pure water? With base?
A: NO. Your samples MUST be 2-5% acid to be run in the ICP. If your sample is precipitating, it may require a different acid digestion method, or it may be incompatible. Contact the listed staff member to discuss solutions.
Q: Can I leave my standards next to the ICP? I might want to use them again next week.
Q: Can I leave my standards next to the ICP? I might want to use them again next week.
A: Nope! Do not leave samples or standards next to the instrument. Dispose of your samples when you're done in our waste bottle, or take them with you.
Q: Someone is on the instrument but my name is reserved on the calendar. What do I do?
Q: Someone is on the instrument but my name is reserved on the calendar. What do I do?
A: If you are on the calendar then you have the right to use the tool. It's okay to remind people of this rule and ask them to leave... or ask one of the staff to step in. We don't mind enforcing the rules! :-)
Q: Solvent is not flowing through my tubing when I rinse. How can I fix this?
Q: Solvent is not flowing through my tubing when I rinse. How can I fix this?
A: You may have put the tubing on the pump backwards. Double check it or ask for help. In addition, the tubing goes flat over time. Forgetting to dry the tubing causes problems as well as leaving the clamps connected (not releasing tubing pressure) after running the instrument. Unfortunately, if the tubing is flat that means the inside has collapsed and sealed off the opening, which prevents solvent flow. The only fix is to replace the tubing with a new one found in the second drawer under the autosampler.
Q: What do I do when the torch shuts itself off mid-run?
Q: What do I do when the torch shuts itself off mid-run?
A: This happens on occasion. Check that your chiller and gas flow are okay and restart the torch. Let the torch stabilize for 20 minutes, then start again. If it shuts off on its own a second time, contact the staff member in charge of the tool. It's possible you have too much organic content in your samples, or that the torch is clogged and needs replacement and recalibration.
Sample Prep Guides
Sample Prep Guides
General Shared Copy of ICP Sample Prep.pdfICP WASTE INSTRUCTIONS.pdfOLD 720 INSTRUCTIONS
OLD 720 INSTRUCTIONS
ICP manual.docxICP standards spreadsheet instructions.docICP standard form_UPDATED 2021.xlsPage updated
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