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Analytical data are produced for some kind of decision-making whether it is regulatory or monitoring. Data that are closely controlled (quality assurance) provide reliable evidence for use in court or to make assessments of pollution in the environment.
In the collection, storage and transport of samples intended for organic analysis, the field personnel should be aware of possible contamination and/or degradation that can occur in organic samples. The following information will help eliminate problems with sample analysis.
Quality data can only be obtained from environmental samples that are properly collected, preserved and promptly shipped to the laboratory for analysis. The procedures involved in this process include: 1) collecting the samples using appropriate sampling techniques; 2) selecting proper sample containers; 3) preserving the samples immediately after collection either chemically or by cooling to 4°C, whichever is appropriate; 4) clearly identifying the samples and completing the corresponding laboratory sheets; and 5) carefully packaging and promptly shipping the samples to the laboratory for analysis.
Sediments for organic and inorganic chemical analyses are most often collected using grab, dredge or core methods. The chosen method should target the goals of the study plan and complement any other biological tests that may be conducted at the site or with sediments from the site. Samples slated for different types of physical and chemical analysis may need to be collected and handled in slightly different ways. The level of precautions that must be taken to prevent contamination of samples will depend on the type of analysis to be performed and the study objectives.
Refer to section 701.4 General Sediment Sampling Equipment and Procedures for suggested equipment list and suitability as well as procedures for collection equipment.
Sample Containers - Samples for organic analysis and inorganic (metals) analysis must be in separate containers. Containers are prepared by and should be obtained from the Wisconsin State Laboratory of Hygiene (SLOH) if it is the laboratory doing the analyses. Other laboratories may provide their own containers and should be contacted to find out their requirements for appropriate sample jars. The following information pertains to analyses to be performed by SLOH.
Sediment samples should be submitted to the laboratory in a container appropriate for the analyses requested.
If additional analyses or information about special preservation and handling procedures for SLOH are required, contact the Inorganic Chemistry Unit for instructions:
The Wisconsin State Laboratory of Hygiene
Inorganic Chemistry Unit
(608-262-3458)
Soil and sediment samples should be submitted to the laboratory in a container appropriate for the analyses requested. All containers are prepared by and should be obtained from the State Laboratory of Hygiene.
A portable balance for measuring GRO and DRO samples is available from the Central Office. Contact Tom Janisch at (608) 266-9268 for availability information.
If additional analyses or information about special preservation and handling procedures are required from the State Lab of Hygiene, contact the Inorganic Chemistry Unit for instructions:
The Wisconsin State Laboratory of Hygiene
Organic Chemistry Unit
(608) 262-2797
If chemical and/or physical analyses are required on sediment samples also slated for toxicity or bioaccumulation tests at the Aquatic Life Toxicity Testing Laboratory (A.K.A. Biomonitoring Lab), the lab can perform the sediment homogenization and fill sample jars for the chemical analyses from the same sediment that will be used for the bioassays. Clean, five gallon, polyethylene buckets are available from the Biomonitoring lab for holding and transport of sediment samples for toxicity and bioaccumulation tests (see section on Bioassays). Small buckets are also available if only toxicity tests and chemical and physical analyses are planned. If a laboratory other than the Biomonitoring Lab is used, the testing lab should be contacted for information on appropriate sample containers and procedures.
The Wisconsin State Laboratory of Hygiene
Aquatic Life Toxicity Testing Laboratory
977 Jonathan Drive
(608-265-4023)
Quart-size plastic bags (from the store) can be used for particle size samples. Double bag the sample and fill 1/2-3/4 full. Label both bags in permanent marker with STORET #, District code, Field #, date and collector's name. There is no separate lab slip, but the "particle size analysis" box should be checked on the new sediment lab slip in order to keep the data tracked together. Particle size analysis is usually contracted for every chemical analysis sample, so make sure to collect sediment for this analysis. The Biomonitoring Lab will also subsample sediments for particle size analysis if toxicity tests are being conducted.
Quality control audits are conducted on representative portions of all sample bottles from the State Lab of Hygiene for chemical analysis to verify that they are free from contaminants. These audits are performed before any bottles are approved for use. Because of the considerable effort expended in assuring the quality of sample bottles, it is important that they be used only for the parameters specified on the label.
Information should be obtained about the quality control of sample containers obtained from analysis laboratories other than the State Lab of Hygiene when the contract for service is being set up to make sure appropriate procedures are used to prevent contamination.
The sample container cleaning procedures and details regarding the Quality Assurance audit protocols are described in the "Organic Chemistry Manual", and section 5 and 6 of the State Laboratory of Hygiene's Quality Assurance Manual prepared by the Water Chemistry Unit. Labs other than SLOH should be contacted for QA protocols.
See 701.4 General Sediment Sampling Equipment and Procedures for a description of equipment and procedures for collecting sediment.
The following steps for cleaning new or used sediment sampling equipment and containers are recommended by EPA (1994):
Clean equipment can be protected from contamination during transport (i.e., exhaust, pickup beds, boat motors, etc.) by wrapping in aluminum foil.
Request and obtain appropriate sample containers ahead of time (see above).
Quality control procedures to be followed at the sites should be written down for all field staff if a formal QAPP is not written.
All sediment samples for chemical analysis should be preserved as soon as possible after collection by cooling to and maintaining a temperature of ~4°C (ice cold) by putting samples on ice in a cooler.
Keep samples shaded from sunlight to prevent breakdown of chemicals by UV light.
The SLH provides "blue ice packs" in each sample kit designed for VOC, GRO and DRO analysis, although samples should first be cooled to 4°C on ice. Plastic bottles can also be filled with water, frozen, and placed in the shipping container. Samples should be pre-chilled if these cooling materials are used for shipping.
For soil or sediment samples to be analyzed for GRO, it is required to add 25 ml of premeasured methanol to two of the sample vials at the time of collection. (Vials of methanol are available at the DNR district office.) The third vial is used for determining moisture of the sample.
For soil samples to be analyzed for VOCs, the collector should consult the individual program needs for the appropriate preservation requirements which may include methanol preservation.
Contact the contracted laboratory for additional preservative requirements for specific parameter requests.
When cooling is required during shipping, the samples should be pre-cooled in an ice chest, and later placed in a field pack with a suitable quantity of ice or "Blue Ice". Ice should not be placed in the field pack loose. It should be securely sealed in a heavy plastic bag to prevent leakage during shipment. Plastic quart sample bottles or plain 250 mL bacteria sample bottles filled with water and frozen, may be used in place of ice cubes (they leak less and may be reused). However, if sample bottles are used, clearly label them as "ICE". DO NOT USE metals bottles, nutrient bottles, or bottles designated for specific tests as ice containers. A great deal of Quality Assurance effort goes into preparing these bottles before they are approved for use.
Properly packaging sediment samples for shipping is important for maintaining sample quality and safety of persons contacting the samples.
After collection, check each sample to make sure the container lid is securely closed and the sample is properly preserved. The exterior of each sample container should be wiped clean with a wet cloth.
Check all samples for secure, correct and complete labels that match the accompanying lab sheets (see below).
Styrofoam field packs for shipping environmental samples are available from the State Laboratory of Hygiene. A whirl-pak (plastic bag) is included in the pack and should be used to protect the laboratory sheets from moisture damage during shipment. Dividers, included in the packs, help protect the sample bottles during shipment and should be used whenever possible. When sealing the field packs, secure all four sides of the lid by wrapping with reinforced tape. The tape should be completely wrapped around the pack to make sure that the lid is secure. When more than one field pack is needed to ship various sample portions from a single sampling site, tape the field packs together. This will prevent sample sorting errors and will allow the lab to match the bottles with the correct laboratory sheets.
A cooler lined with a polyethylene bag can be used instead of the foam pack if necessary, but be sure to pack sample jars to avoid breakage during shipping and handling.
Different laboratories may have their own lab sheets that should accompany all samples. For samples sent to the State Lab of Hygiene the laboratory sheets are printed by the Fish/Sediment Contaminant Database after the appropriate information is entered. The appropriate information includes:
 | STORET number| a sample description | the sampling
program | name and address of the person to whom the report
should be sent | Last name of the sample collector | primary
station number and/or county code number | field information,
| tests (parameters) requested | |
To help field staff record the appropriate information a sediment sample information form has been developed. Please complete it with a waterproof pen. An electronic copy of this form is available from the download section.
The laboratory sheet is an important link between the laboratory and field personnel. The laboratory relies on the sheet to obtain the information necessary to prepare and analyze the sample properly.
If storage time limitations are recommended for the sample parameters, coordinate with the laboratory before collecting samples to let them know the sampling schedule.
Alert the receiving laboratory of any samples that are known or believed to contain high levels of specific contaminants, including an estimated concentration if possible. This can be done either over the phone before the samples arrive or with an enclosed written warning. The advanced notice allows the lab to handle highly contaminated samples in a way to prevent human exposure as well as cross-contamination of samples in the lab. Additionally, the lab will be able to process and analyze the samples more quickly if they know before analysis that the contaminant concentration is high.
Samples should be shipped with an "overnight" mail service or personally delivered to the laboratory or shipped or delivered to the Central Office for temporary storage so that the samples arrive before all of the ice melts in the shipping container. Monday, Tuesday or Wednesday are the best days to ship samples to assure they do not sit in a mail room with no refrigeration over the weekend. Even "overnight mail" can take longer than 24 hours, so Thursdays can be risky. DO NOT send samples on Fridays unless you have made previous arrangements with the lab and/or Central Office.
All sediment samples for the DNR (unless other arrangements for a special project have been arranged) should be shipped to the Central Office care of Linda Talbot:
Department of Natural Resources
C/O Linda Talbot
Box 7921, 101 S. Webster St.
Madison, WI 53707
Phone: (608) 266-8148
NOTE: Samples are logged in and assigned to the appropriate lab account numbers as well as checked against the lab contract for parameters and numbers of samples. Additionally, sampling information may need to be keyed into the computer from the lab slip by Central Office before samples are sent to the lab, after which lab slips are gone forever. Because sediment samples are run under special contracts with the lab and not under the Basic Agreement like the surface water samples, this sample transfer and tracking is necessary. This process allows the DNR to best utilize the analysis dollars.
Call the Madison office or laboratory before shipping samples to make sure someone will be available to receive the samples and take care of them. If using a lab other than SLOH or you have made arrangements to deliver samples directly to the lab, coordinate with Linda Talbot for the appropriate log in of samples and lab slip information.
If a sample bottle seal is questionable and no additional bottles are available, place the entire bottle in a whirl-pak (250 mL bottles only). This will contain the sample and prevent any preservative from contaminating other samples in the field pack.
The outside of the sample containers should be completely free of contaminated material before the samples are shipped. If this is not possible, the laboratory should be made aware of these samples before shipment.
If the submitter believes a sample contains a Department of Transportation (DOT) regulated material or hazardous material, refer to the "Sample Shipping Requirements"; section in the Field Procedures Manual (DNR, 1993).
Baudo, R., Giesy, J., and H. Muntau, (Eds.). 1990. Sediments: Chemistry and Toxicity of In-Place Pollutants. Lewis Publishers, Boca Raton, FL.
EPA. 1985. Sediment sampling quality assurance user's guide. Environmental Monitoring Systems Laboratory. Las Vegas, Nevada. EPA/600/4-85/048.
EPA. 1994. Methods for Measuring the Toxicity and Bioaccumulation of Sediment-associated Contaminants with Freshwater Invertebrates.
WDNR. 1993 (draft). Field Procedures Manual. Office of Technical Services, Bureau of Water Resources Management.
WDNR. 1990 (draft). Quality Assurance Guidance for Inplace Pollutant Monitoring Activities. Unpublished document on file at Office of Technical Services, Bureau of Water Resources Management.
State Laboratory of Hygiene. 1994. Organic Chemistry Manual.
State Laboratory of Hygiene. 1992. Inorganic Chemistry Manual.
Rev. 0, September 1998
This document is intended solely as guidance and does not contain any mandatory requirements except where requirements found in statute or administrative rule are referenced. This guidance does not establish or affect legal rights or obligations and is not finally determinative of any of the issues addressed. This guidance does not create any rights enforceable by any party in litigation with the State of Wisconsin or the Department of Natural Resources. Any regulatory decisions made by the Department of Natural Resources in any matter addressed by this guidance will be made by applying the governing statutes and administrative rules to the relevant facts. (From Manual Code 1210.1)