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 by several samples included for quality control: a duplicate sample, an internal standard
(250 ppb ICPMS71A in 3% HNO3), an arsenic 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
become apparent. 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
Cu
Pb
Fe
As
Cl2
FHg
Ca
Mg
Na
P
Maximum Contaminant Level Goal (not
enforced) (mg/L)
1.3
0
0.3
0
4.0
4.0
0.002
not regulated
not regulated
not regulated
not regulated
Maximum Contaminant Level
(enforced) (mg/L)
1.3
0.015
none
0.010
4.0
4.0
0.002
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
We should have a comments section, just like on the NEL report. We should 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
Copper
Lead
Iron
Arsenic
Chlorine
Fluorine
Calcium
Magnesium
Sodium
Phosphorus
Add any for 2012??
Result Unit Detection Limit
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
mg/L
EPA Safe
limit
1.3
0.0015
0.3
0.01
4
4
0.002
NA
NA
NA
Method
Preparation Analysis
Analyst
date/time date/time
Element
(Add any for
2012??)
Copper
Lead
Iron
Arsenic
Chlorine
Fluorine
Calcium
Magnesium
Sodium
Phosphorus
Expected Concentration in Drinking Water
(ppm)
1.3
0.015
0.3
0.010
<250
2
3.4-131
0.57-15
20
<0.02