
Aqueous Metal Sampling and Sample Preservation
The following guidelines are taken from "Standard Methods for the Examination
of Water and Wastewater", 19th Ed., 1995, A.D. Eaton, L.S. Clesceri, and A.E.
Greenberg, ed.
1. General Precautions and Procedures
- Rinse container 2-3 times with the sample to be collected
- fill the container full, leaving approximately 1% of the volume empty to allow for
possible thermal expansion
- determine how much concentrated nitric acid is required to bring the sample to a pH <
2 on a separate sample first
- use the same bottle of acid throughout the analysis in order to obtain a reliable blank
- if sampling a stream, collect the sample at mid-stream and at mid-depth
- use a sample bottle with a polytetrafluoroethylene (TFE or Teflon) liner
2. Sample Containers
- Sample containers should be composed of quartz or tetrafluoroethylene (Teflon). Cheaper
alternatives are composed of polypropylene or linear polyethylene with a polyethylene cap.
Borosilicate glass can be used, but avoid "soft glass" containers if the sample
concentration is in the microgram/L range (ppb).
- Containers and filters need to be cleansed as follows. Thoroughly clean the sample
containers with a metal-free non-ionic detergent solution, rinse with tap water, soak in
acid, and then rinse with metal-free water. For quartz, TFE, or glass materials, use 1+1
HNO3, 1+1 HCl, or aqua regia (3 parts conc. HCl + 1 part conc. HNO3)
for soaking. For plastic material, use 1+1 HNO3 or 1+1 HCl. Reliable soaking
conditions are 24 hr at 70 oC.
3. Preservation
- Acidify immediately after sampling with concentrated nitric acid to a pH < 2 (usually
1.5 mL conc HNO3 /L sample). High purity commercial acid such as provided by
J.T. Baker is preferred.
- After acidification, refrigerate at 4 oC. Samples with metal concentrations
in the ppm range will stay stable for up to 6 months; concentrations in the ppb range need
to be sampled as soon as possible.
Direct suggestions, comments, and questions about this page to
Pete Poston, postonp@wou.edu

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Copyright © 1997 Western Oregon University