Agilent 5800 ICP-OES

To analyze a sample via ICP-OES the sample must be in an aqueous form. These can be straight water samples or digested samples. All aqueous samples should be acidified to keep elements in solution. Nitric acid (HNO₃) is most often used. However, hydrochloric (HCl), sulfuric (H₂SO₄), hydrofluoric (HF), or combinations of acids can be used. If you’re using something other than 2-5% HNO₃ you must inform the GEAL Center (jriddle1@ua.edu). Failure to do so can cause precipitation of elements if mixing standards and sample matrixes, poor data, or even damaging the equipment. Always use trace metal/ultra-high purity grade acid when acidifying to avoid contamination.

If you are unsure of how to prepare your lab and samples for ICP-OES analysis, the GEAL Center can give guidance (e.g. labware cleaning methods, setting up laboratory reagent blanks, etc). However, it is up to each individual lab to determine their SOPs for your experimental method and lab setup.

Preservation of many sample types is needed. Due to samples needing a variety of preservation techniques, it is up to your lab to determine the requirements for your samples. Common ones include refrigerating, freezing, and/or chemical preservation. Please inform the GEAL Center which preservation method you are using, so that we can match with your samples in our lab.

All samples¹ must be filtered through at least 0.45µm filter to remove particulate matter prior to running samples on the ICP-OES. Failure to do so can cause interference from particles as well as the buildup of deposits in the spray chamber and torch.

Warning: Samples that are not filtered and run through the ICP-OES will incur a cleaning fee of $200 since the machine will have to be brought down for cleaning. Data quality cannot be guaranteed, and samples will have to be rerun at original run cost + second run.

Here at GEAL, we strive to provide the best quality we can and to ensure your data is with no error. These are the steps we take to provide that:

Calibration Standard (CAL) — A solution prepared from the primary dilution standard solution or stock standard solutions and the internal standards and surrogate analytes. The CAL solutions are used to calibrate the instrument response with respect to analyte concentration.

Calibration Blank (CB) — A volume of reagent water fortified with the same matrix as the calibration standards, but without the analytes, internal standards, or surrogate analytes.

Instrument Performance Check Solution/Internal Standard (IPC) — A solution of one or more method analytes, surrogates, internal standards, or other test substances used to evaluate the performance of the instrument system with respect to a defined set of criteria.

Linear Calibration Range (LCR) — The concentration range over which the instrument response is linear.

Quality Control Sample (QCS)(ICV and CCV) — A solution of method analytes of known concentrations that is used to fortify an aliquot of LRB or sample matrix. The QCS is obtained from a source external to the laboratory and different from the source of calibration standards. It is used to check laboratory performance with externally prepared test materials.

While GEAL works to ensure quality in our lab, it is important to ensure you have quality control in your lab. While we here cannot enforce what you or your students do, it is recommended you provide these samples to check the quality of work for your lab as well.

Field/Lab Duplicates (FD) — Two separate samples collected/processed at the same time and placed under identical circumstances and treated exactly the same throughout field and laboratory procedures. Analyses of field/lab duplicates indicate the precision associated with sample collection, preservation and storage, as well as with laboratory procedures.

Laboratory Fortified Blank (LFB) — An aliquot of reagent water or other blank matrices to which known quantities of the method analytes are added in the laboratory. The LFB is analyzed exactly like a sample, and its purpose is to determine whether the methodology is in control, and whether the laboratory is capable of making accurate and precise measurements.

Laboratory Fortified Sample Matrix (LFM) — An aliquot of a sample to which known quantities of the method analytes are added in the laboratory. The LFM is analyzed exactly like a sample, and its purpose is to determine whether the sample matrix contributes bias to the analytical results. The background concentrations of the analytes in the sample matrix must be determined in a separate aliquot and the measured values in the LFM corrected for background concentrations.

Laboratory Reagent Blank (LRB) — An aliquot of reagent water or other blank matrices that are treated exactly as a sample including exposure to all glassware, equipment, solvents, reagents, internal standards, and surrogates that are used with other samples. The LRB is used to determine if method analytes or other interferences are present in the laboratory environment, the reagents, or the apparatus.

Quality Control Sample (QCS) — A solution of method analytes of known concentrations that is used to fortify an aliquot of LRB or sample matrix. The QCS is obtained from a source external to the laboratory and different from the source of calibration standards. It is used to check laboratory performance with externally prepared test materials.