How are reporting limits determined?
How reliable are results just above the reporting limit?
Why do your reports suggest confirming positive results by GC/MS or HPLC/MS?
What are J values and should they be used for regulatory purposes?
Can I get lower reporting limits if I ask for drinking water methods on all matrices?
How long are samples routinely kept by North Coast Labs?
How far in advance should I order sample containers?
There are specific EPA procedures that a laboratory must follow in the determination of its reporting limits. Before the reporting limits (RL) can be set, the method detection limit (MDL) must be determined. The most common method of determining a method detection limit is a statistical process involving the analysis of seven low level spikes on a single matrix (usually distilled water). A Student’s T analysis is applied to the results and a concentration at which the laboratory is 99% certain that the actual analyte concentration is not zero is calculated. The upper limit of the confidence interval of this number is the minimum concentration the laboratory can report, and is called the method detection limit. The RL is the lowest level of analyte that can be reliably determined within specified limits of accuracy and precision during routine laboratory operating conditions. The RL should generally be below any regulatory limits, but notifying the lab of reporting limit requirements is highly recommended.
The relative uncertainty of an analytical measurement varies substantially as the measured value approaches both the RL and the MDL. The sample matrix may have a considerable effect on the sample preparation process and the ability of the instrument to detect an analyte at the usual RL, as well. Also, the method detection limit (MDL) is set so that there is only a 1 % chance of reporting a false positive on the matrix on which the method detection limit was determined. This says nothing about the reliability of the actual reported value compared to a theoretical true value, nor does it account for matrix effects.
While most positive values encountered during an analysis using a gas chromatograph are confirmed on a second column, it is always prudent to confirm a positive value using another detector. GC/MS or HPLC/MS is the preferred method of confirmation because the possibility of misidentification is greatly reduced.
A J qualifier is used to flag a value that is between the method detection limit (MDL) and the reporting limit (RL). There is considerable uncertainty associated with values between the MDL and the RL; therefore, these values should not be used for decision-making purposes.
Some regulatory agencies are now requiring the use of EPA methods that provide the lowest RL’s independent of the sample matrix. EPA 500 series methods were developed for the analysis of synthetic and volatile organic compounds in drinking water and yet some regulators are actually requiring that these methods be used on groundwater and surface water. Method proficiency is initially demonstrated by analyzing replicate spikes on deionized water and does not take into account the effects of different sample matrices on the MDL. If a sample other than drinking water is analyzed using a drinking water method, it is almost certain that the RLs will be much higher than those of a drinking water analyzed using the same method.
Our policy is to keep samples 30 days from the time we receive them. If you suspect that you may need additional analyses, it is important to request that your samples be held for possible additional analyses on your chain of custody. By doing this, your samples will stored under the proper conditions to maintain their integrity. Samples without this designation will be stored at room temperature following the completion of their analyses for thirty days.
We routinely keep a ready supply of sample containers on hand. If you know in advance that you will need sample containers it is wise to order them seven days in advance of the date that you would like to pick them up or have them delivered. With advance notice you are assured of having all of the requested containers ready when you need them.
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