Section 149.46. Handling of samples.

 

(1)   Sample collection .

(a) The laboratory shall retain records supplied by the collector to allow the laboratory to evaluate collection procedures against the laboratory's sample acceptance policy.

(b) When the laboratory provides containers and preservatives for sample collection, including bulk sampling containers such as "carboys", the laboratory shall have standard operating procedures in place which address concerns that the containers are adequately cleaned and not contributing to contamination of samples, do not contain analytes of interest at levels which will affect sample determinations and that the preservatives used are sufficiently pure to maintain the validity of reported results. Containers supplied by the laboratory for sample collection shall allow collecting a sufficient amount of sample to perform all required or requested determinations at the required or desired sensitivity.

(2)   Sample acceptance policy.

(a) The laboratory shall have and follow a written policy that clearly outlines the conditions under which samples will be accepted or rejected for analysis, or under which associated reported results will be qualified.

1. Drinking water samples received beyond holding time, improperly preserved, in inappropriate containers or showing evidence that they have not been collected according to approved or accepted protocols shall be rejected for analysis, unless the laboratory can document that it has been instructed by the client to proceed with analyses, and all associated results are accompanied by a disclaimer attesting that results may not be used to determine or evaluate compliance with the safe drinking water act.

2. The results of samples that are not drinking waters shall be appropriately qualified if the samples are received improperly preserved, in inappropriate containers, beyond holding time, with insufficient volume to complete requested analyses, or if the laboratory has evidence that the samples have not been collected according to approved or accepted protocols. Alternatively, the laboratory may reject the samples for analysis.

(b) When samples received do not conform to the descriptions provided by a collector, the laboratory shall consult with the collector or sample originator to determine the processing or disposition of the samples.

(3)   Sample handling protocols.

(a) The laboratory shall establish and follow procedures for identifying samples uniquely. The procedures shall ensure that the identity of samples cannot be confused physically or when referenced in records or other documents.

1. Samples received by a laboratory for analysis shall be assigned a unique identification code.

2. The unique identification code shall be placed on a sample container as a durable label.

3. The unique identification code shall be used as a link to associate samples with their complete history, including treatment and analysis, while in the laboratory's possession.

(b) Chain-of-custody documentation shall be required for those facilities that do not perform their own sample collection, transport and analysis.

(c) The laboratory shall apply evidentiary chain of custody procedures when it receives samples that support regulatory investigations or when required to do so in accordance with a written agreement between the laboratory and the client.

(4)   Sample preservation and holding time.

(a) Laboratories shall follow the sample preservation procedures and holding times required by state and federal regulations. If the sample preservation procedures and holding times are not required by state or federal regulations, laboratories shall follow the sample preservation procedures and holding times established in the analytical method. If the analytical method does not establish sample preservation procedures or holding times, laboratories shall follow the procedures in the authoritative sources specified in Appendix III of this chapter.

(b) Samples requiring preservation at 6ºC under this section shall be considered preserved if they are received at a temperature from above their freezing point to 6ºC or if they are received surrounded by ice. If the samples are not received on ice, the laboratory shall record one of the following at the time of receipt:

1. The temperature of an actual sample.

2. The temperature of a temperature blank shipped with the samples.

3. The temperature of the melt water in the shipping container.

(c) When multiple samples requiring thermal preservation at 6 o C are received in the same cooler or holding container, the entire set of samples shall be considered preserved if the temperature of a blank or a sample is determined to be from above freezing to 6 o C, or if there is ice remaining in the shipment container.

(d) Samples to be analyzed for whole effluent toxicity shall be considered preserved if their temperature on receipt is above freezing and does not exceed 10 o C.

(e) Except as specified in pars. (b) to (d) , samples requiring thermal preservation at a temperature other than 6 o C shall be considered preserved if their temperature on receipt is within plus or minus 2 degrees of the required preservation temperature.

(5)   Sample receipt documentation . The laboratory shall document the receipt and condition of all samples in chronological hard copy or electronic records. The records may be maintained in any format that retains the following information:

(a) The identity of the client or entity submitting samples, or the project associated with the received samples.

(b) The dates of sample collection and laboratory receipt.

(c) The times of sample collection and laboratory receipt for samples to be analyzed for tests with holding times equal to or less than 48 hours.

(d) The unique sample identification code assigned by the laboratory.

(e) Documentation of sample preservation status and other sample conditions on receipt.

(f) An unequivocal link between the sample identification code assigned by the laboratory and the field collection identification code assigned by the collector.

(g) The requested analyses, unless the laboratory collects and analyzes its own samples and analyses are directed by permit.

(h) The reference to requested test methods, when the collector or sample originator specifies them.

(i) Any comments resulting from the inspection undertaken to determine whether samples meet the policy in sub. (2) .

(6)   Storage of samples.

(a) The laboratory shall have procedures and appropriate facilities for avoiding deterioration, contamination, loss or damage of samples during storage.

(b) Samples requiring thermal preservation at temperatures other than 6 o C shall be stored under refrigeration within 2 degrees of the specified preservation temperature.

(c) Samples requiring thermal preservations at 6 o C may be stored at temperatures from above their freezing point to 6 o C.

(d) Samples shall be stored separately from all standards, reagents, food and other potentially contaminating sources. Samples shall be stored in areas that prevent or minimize cross-contamination.

(e) Sample extracts, digestates, leachates or concentrates, resulting from any initial preparatory step, shall be stored as specified in this subsection .

History: CR 06-005 : cr. Register April 2008 No. 628 , eff. 9-1-08.

Note

The laboratory should establish procedures to ensure and document that the sample containers it provides do not contribute contaminants before they are used for collecting samples. Microsoft Windows NT 6.1.7601 Service Pack 1 Sample preservation procedures and holding times are given in 40 CFR 136 , ch. NR 219 , SW–836 "Test Methods for Evaluating Solid Waste" as cited in item 24 of Appendix III of this chapter, and may be specified in the analytical methods. Microsoft Windows NT 6.1.7601 Service Pack 1 The preservation status of samples may be recorded as "received on ice" only if solid ice is present around samples when they are received at the laboratory. The preservation status of samples refrigerated with ice packs, such as "blue ice", should not be recorded as "received on ice". Microsoft Windows NT 6.1.7601 Service Pack 1