Method detection limit (MDL) is defined as “…the minimum measured
concentration of a substance that can be reported with 99% confidence
that the measured concentration is distinguishable from method blank
results” (EPA 2016). This information is applicable to determining the
presence of contaminants in a water sample. But it is not useful for
quantifying the precision of concentrations reported for naturally
occurring solutes, particularly at levels near the MDL. A limit of
quantification (LOQ) can be used to determine the minimum
concentration that can be reported with some level of precision. This
is sometimes taken as three times the MDL, although methods for
setting this limit are not well standardized. We define the LOQ as the
value above which analytical variability is within 10% of the measured
value, as determined by standard solutions run as unknowns. For values
above the LOQ, concentrations may be reported and interpreted with two
significant figures. For values between the MDL and the LOQ, analyses
are not repeatable within 10%, and could vary by 50% or greater.
Concentrations below the LOQ are best interpreted to one significant
figure. For calculation of solute fluxes, samples with concentrations
less than MDL are assigned a value equal to ½ of the MDL. Samples with
concentrations between the MDL and LOQ are assigned the measured
value. Solute fluxes based on calculations where a substantial number
of samples have concentrations less than the LOQ should be reported to
only one significant figure and variations should be interpreted with
caution.
Values of MDL and LOQ will vary as methods or analytical instruments
are changed. There are also minor fluctuations year to year from minor
variations in laboratory operating conditions. The limits documented
here generally apply to water samples analyzed in the Durham lab
starting June 1, 2010. Starting on June 1, 2013, the Durham lab took
over analysis of the weekly precipitation and streamwater samples from
the Hubbard Brook Experimental Forest. So this document applies to the
long-term Hubbard Brook streamwater and precipitation chemistry
datasets starting on that date. For QA/QC parameters of the earlier
part of the Hubbard Brook long-term dataset, see Buso et al. 1999.
In the future, when major changes to procedures or instrumentation at
the Durham lab alter MDL or LOQ, this data packaged will be updated to
include revised values.
Buso, D. C, Gene E Likens, and J. S Eaton. 2000. Chemistry of
Precipitation, Stream Water And Lake Water From The Hubbard Brook
Ecosystem Study: A Record Of Sampling Protocols And Analytical
Procedures. Newtown Square, PA: USDA Forest Service, Northeastern
Research Station. General Technical Report NE-275.
EPA 2016. Definition and Procedure for the Determination of the Method
Detection Limit, Revision 2. EPA 821-R-16-006.