CH332 Lab 2: Lake and Drinking Water Analysis by ICP-OES

Part 2: ICP Protocols

The objective of this laboratory is to analyze lake water samples and drinking water samples using Inductively Coupled Plasma Spectroscopy based on standard ICP-OES procedures. This lab will familiarize you with the influence of forward RF power, plasma viewing height/length, sample flow rate, analytical wavelength, background correction, and argon flow rate on instrumental performance. You will prepare samples for analysis and will be responsible for calibrating the instrument and reporting metal concentrations in lake water and drinking water samples with the appropriate analytical uncertainties.

Remember: As with the plastic water collection bottles, all plastic ICP sample tubes must be cleaned using the 3%nitric acid, rinsed and dried before use. There is a jug for soaking the tubes under the hood in the PQ lab.

You will be designing your ICP run for both the lake water and the drinking water samples. At the end of every 5 samples, one check sample (250 ppb ICPMS 71A in 3% HNO3) and a 3% HNO3 blank are automatically completed (included in the instrument protocol). Therefore, you will use a series of 10 samples followed byseveral samples included for quality control: a duplicate sample, an internal standard (250 ppb ICPMS71A in 3% HNO3), anarsenic sample of unknown concentration and an As spike. By running the same sample twice (duplicate), we will ensure that our measurements are precise. Adding a known quantity (spike) to our sample will allow us to ensure the instrument is responding as predicted. Any error that is introduced due to sample contamination or variation in pipetting technique will becomeapparent.Be sure that the SAMPLE BLANK water samples are included in the run (the blanks that you set up as samples!!). Errors in the blank measurements will indicate contamination in the sampling method. After (or while) testing the samples, we will check for "flags" in the data, or values that stand out as being significantly higher than expected. These samples must be retested to ensure validity.

EPA Standards for Drinking Water

Contaminant / Maximum Contaminant Level Goal (not enforced) (mg/L) / Maximum Contaminant Level (enforced) (mg/L)
Cu / 1.3 / 1.3
Pb / 0 / 0.015
Fe / 0.3 / none
As / 0 / 0.010
Cl2 / 4.0 / 4.0
F- / 4.0 / 4.0
Hg / 0.002 / 0.002
Ca / not regulated
Mg / not regulated
Na / not regulated
P / not regulated

Add any for 2012??

Report Format

You will be designing your own report form. Please refer to the NEL report on the CH332 website. The template below (from 2010) mimics the NEL format listing each metal and including columns with the following headings:

Concentration
EPA "Safe" Range
Local Range (This would tell how their water compares to other local spots)
Detection Limit
Preparation Date/Time
Analysis Date/Time

Weshould have a comments section, just like on the NEL report. Weshould point out any irregular results(differ from the EPA standards or the local ranges). The instrument and the protocol should be included. The limitations of your work should be explained. Recommendations: all samples showing undesirable results should be retested by a certified laboratory (suggest one??).

We will use Excel (mail merge and label printing) to format the results into the report form. Careful correlation between the ICP data and the Excel formatting saves a lot of time and effort!

Please check that the information below is updated for elements tested and 2012 guidelines!!

Result Form
Parameter / Result / Unit / Detection Limit / EPA Safe limit / Method / Preparation
date/time / Analysis
date/time / Analyst
Copper / mg/L / 1.3
Lead / mg/L / 0.0015
Iron / mg/L / 0.3
Arsenic / mg/L / 0.01
Chlorine / mg/L / 4
Fluorine / mg/L / 4
Calcium / mg/L / 0.002
Magnesium / mg/L / NA
Sodium / mg/L / NA
Phosphorus / mg/L / NA
Add any for 2012??
Element
(Add any for 2012??) / Expected Concentration in Drinking Water (ppm)
Copper / 1.3
Lead / 0.015
Iron / 0.3
Arsenic / 0.010
Chlorine / <250
Fluorine / 2
Calcium / 3.4-131
Magnesium / 0.57-15
Sodium / 20
Phosphorus / <0.02