As the Nation's principal conservation agency, the Department of the Interior has responsibility for most of our nationally owned public lands and natural resources. This includes protecting our fish and wildlife, preserving the environmental and cultural values of our nation's parks and historical places, and providing for the enjoyment of life through outdoor recreation.

The primary goal of the U.S. Fish and Wildlife Service (Service), a Bureau of the Department of the Interior, is the conservation and sound management of sport fishery and wildlife resources for the benefit of present and future generations of Americans. Attainment of this goal requires continual collection, analysis and synthesis of new information on which wise and timely management decisions can be based. As a part of this decision making process, the Service has the responsibility of determining the effects of environmental contaminants on organisms and their habitats. A significant part of this responsibility requires the determination of trace amounts of organic compounds in the tissues of fish, wildlife, invertebrates and plants, as well as in water and soil/sediments.

Studies conducted by the Service cover a wide spectrum of contaminant problems and geographic areas. These include studies involving organic compounds derived from agriculture, energy development, and industrial activities. Because of the diversity of studies and the unique requirements of individual studies, "batches" of samples submitted for analyses may vary considerably.

The Service is seeking contractors to perform organochlorine pesticides and PCB analyses, and other organic analyses, in plant and animal tissues, water, and soil/sediment. The Service is fully aware that there may be no technically qualified firms available which can accommodate the large annual estimated quantity of samples stated herein. Moreover, it is possible that the number of samples may be significantly higher during some years because of year to year inconsistencies in demand and available funding. Therefore, the Service is prepared to award one or more contracts in order to assure that there will be sufficient analytical capability to meet the estimated annual need.

See Section H.6

C.2 General Considerations

C.2.1 In accordance with the requirement listed herein, the contractor shall be responsible for all aspects of this effort and shall furnish all necessary services, materials, labor, and supplies not otherwise indicated to be furnished by the Government. The contractor will be responsible for analysis of all of the compounds as described herein.

C.2.2 The contractor must have available, all of the equipment required to perform the analyses as proposed. This will include gas chromatographs, a gas chromatograph/mass spectrometer, as well as the equipment needed to prepare the samples for analyses and the freezer capacity to store the samples prior and subsequent to the analysis.

C.2.3 Due to the nature of the field sample collection season, most of the samples submitted, under this program, arrive at the laboratory over a very short period of time each year. The laboratory should not plan on even sample submissions over the course of the year. The Service has tended to issue 60% of its analytical purchase orders during the months of June, July and August. Submissions tend to drop to near zero during October, November, and December, and slowly pick up starting in late January. A large freezer capacity is needed to store the samples and offerors should be prepared to perform within the required time-frames.

C.2.4 Extracts of samples submitted for analysis will be retained for one year after the analytical report is accepted. The contractor will be required to store up to one year, all un-analyzed portions of samples (up to 200 g) submitted for analysis during the period of performance until disposition is approved by the Service Project Officer. Method of storage will be by freezing at or below -20 degrees Celsius. Disposition includes either disposal or return to the appropriate location, F.O.B. origin, at the option of the COTR.

C.2.5 On occasion, the contractor will receive samples that require additional analyses to be performed at another laboratory. In these cases the contractor is required to homogenize and freeze the samples and ship, at government expense, the appropriate subsample, to the other laboratories within three weeks after receiving them. Samples are "received" when all of the follwoing criteria have been satisfied. For a specific batch(catalog), all samples:

• Have arrived at the laboratory intact(not broken) and properly labeled;
• Have the sample identification number as given in the catalog which was sent with the delivery order; and
• Match the work described in the delivery order.

C.2.6 Incorporation of Technical Proposal

The contractor's technical proposal will be incorporated herein by reference into any contract awarded as a result of this solicitation. In the event of a conflict between the provisions of the technical proposal and any other clause of this contract(including, but not limited to, the statement of work), the conflict shall be resolved in accordance with FAR 52.215-33, Order of Precedence. For this contract, the contractor's technical proposal will be deemed to be subitem (f)(last in the order of precedence).

The detailed technical content of the proposal is an important factor in the selection of the contractor for award of this contract. It is agreed therefore, that in the performance of this contract, the contractor shall not deviate significantly from the approved methodologies without the prior approval of the COTR. If it is necessary for the contractor to significantly deviate from approved procedures in order to comply with the requirements of this contract, the contract shall be modified at the discretion of the Government at no increase in cost/price or extension of the delivery schedule.

C.3 Sample Types and Preparation

Sample types to be submitted may include animal tissues (whole bodies or organs, fish, wildlife, invertebrates, eggs), plants, sediment, and water. Additionally, unusual samples will at times be submitted.

C.3.1 Sample Homogenization

The contractor must be capable of homogenizing samples with the following wet weight ranges:

animal or plant tissues - up to 5 kg
soil or sediment - up to 5 kg

While most samples will weigh from 30 g to 1 Kg, on occasion, samples may even exceed the ranges listed above. If problems occur in homogenizing such samples, advise is available from the COTR. Samples should be homogenized so that replicate analyses meet the criteria listed in section C.4 of this contract, under Quality Control.

C.3.2 Organochlorine Scan (CLIN 101)

Offeror will fully describe the methods to be used for analysis, and must supply evidence that such methods meet the quality control standards stated below. Generally methods involve solvent extraction(Soxhlet for tissues and sediments/soils, and mixing for water), cleanup( Gel Permeation Chromatography and/or Florisil column chromatography), separation of pesticides from PCBs(Silica gel column chromatography), and quantification by electron capture capillary gas chromatography and confirmation by mass spectrometry.

C.3.3 An organochlorine scan shall include quantification of the following compounds:

C.3.4 Quantification of Individual Aroclors (CLIN 102A)

Upon request, the contractor will analyze PCB fraction and provide quantification of PCBs as Aroclor 1242, 1248, 1254, and 1260. This analysis will always be ordered in addition to the Organochlorine Scan.

C.3.5 Congener Specific PCB Scan(CLIN 102B & C)

Offeror will fully describe the methods to be used for analysis, and must supply evidence that such methods meet the quality control standards stated below. Generally methods involve solvent extraction, cleanup( including carbon column for planer PCBS,)and quantification by electron capture capillary gas chromatography and/or by mass spectrometry.

An Individual Congener scan shall include quantification of all of the PCB Congeners. It is understood that some co-elutions will occur. Offeror should specify which congener co-elutions are expected using their method. PCB congeners will be designated using the Ballschmiter-Zell numbering system.

This analysis will usually be ordered with the Organochlorine Scan but on rare occasions it may be ordered by itself. If ordered in conjunction with an organochlorine scan, it is assumed that much of the sample preparation work would only be done once and a discount would be offered. The amount of the discount should be listed on CLIN 102B.

C.3.6 Additional Required Determinations

Each OC/PCB/Dioxin/Furan analysis of a tissue sample will include quantification of the percent lipid.

Each analysis of any kind of a non-water sample will include a quantification of the percent moisture.

C.3.7 TOC and Grain Size (CLIN 103)

Upon request, offeror will analyze soil/sediment samples for percent Total Organic Carbon(TOC) and/or Grain size (reported as Percent clay, sand, and silt).

C.3.8 Rapid Turnaround (CLIN 104)

See section F.4.2.

C.3.9 Full data reports.(CLIN 105)

Upon request, the contractor will provide a report, on paper, that includes copies of all of the raw data. The report will include copies of every record related to the analysis that exists at the laboratory. Specifically any existing documents related to receipt of the samples, logs on sample storage and preparation, reports on instrument calibration, instrument printouts, calculation sheets, data summaries, internal QC documents, analyst notes or any other information about the sample in question. The request for a full data report can be made before or after the analysis.

C.3.10 Non-Mandatory Analyses (CLIN 106-122)

The Service has frequent need for other types of organic analyses. It is not required that an offeror provide them.

C.3.11 Aliphatic and Aromatic Hydrocarbon Scans (CLIN 106)

Offeror will fully describe the methods to be used for analysis, and must supply evidence that such methods meet the quality control standards stated below. Generally methods involve solvent extraction, separation of aliphatics from aromatics (silica/ alumina column chromatography), and quantification aliphatics by capillary gas chromatography using flame ionization detection, and quantification of aromatics by gas chromatography/mass spectrometry using selected ion monitoring.

C.3.12 An aliphatic scan shall include quantification of the following compounds:

C.3.13 An aromatic scan shall include quantification of the following compounds:

C.3.14 Organophosphate and Carbamate Pesticides (CLIN 107 )

Offeror will fully describe the methods to be used for analysis, and must supply evidence that such methods meet the quality control standards stated below. Generally methods involve solvent extraction, and quantification by capillary gas chromatography using a Nitrogen-Phosphorous Detector for carbamates and Flame Photometric Detector for organophosphates.

C.3.15 Organophosphate Scan

An organophosphate scan shall include quantification of the following compounds:

C.3.16 Carbamate Scan

A carbamate scan shall include quantification of the following compounds:

C.3.17 Dioxin and Furan Analysis (CLIN 108)

Offeror will fully describe the methods to be used for analysis, and must supply evidence that such methods meet the quality control standards stated below. Generally methods involve solvent extraction, cleanup, and quantification by high resolution gas chromatography-high resolution mass spectrometry. Offeror should propose a full Dioxin/Furan scan which includes:

A simplified scan of 2,3,7,8 TCDD & 2,3,7,8-TCDF should also be offered.

C.3.18 Other Non-Mandatory Analyses(CLIN 109- )

On occasion the Service has a need for other organic determinations. These have included:

It is not required that an offeror provide these services, but if any offeror desires to do so, they should provide methods, prices, and quality assurance data.

C.3.19 Additional Analyses Proposed

Also, offerors are encouraged to propose additional organic analyses they routinely perform. Offerors may propose additional analytes, previously listed analytes at lower detection limits-Any method that is routinely performed and would be considered an organic analysis can be offered. Methods, prices, and quality assurance data should be provided.

C.4 Quality Control

C.4.0 Offerors must supply a copy of a quality assurance plan which describes the steps they take to assure a valid analysis. The operation of the laboratory must be in conformance with applicable portions of the Good Laboratory Practices regulations as stated in 40 CFR,part 160. Specifically:

SUBPART B Organization & Personnel

• 160.29 a,b,d,e
• 160.31 a,b,d,e,f
• 160.33 b,c,f
• 160.35 a,b.6

SUBPART C Facilities

• 160.41
• 160.51 

SUBPART D Equipment

• 160.61
• 160.63 a,b,c

SUBPART E Testing Facilities Operation

• 160.81 a(SOPs must exist and deviations must be documented),b.3,b.5,b.11,c
• 160.83

SUBPART G Protocol for and Conduct of a Study

• 160.130 e

SUBPART J Records and Reports

• 160.185 a.6 (see reporting requirements)

Additionally, the plan must address the following topics and meet any minimums listed (for the purposes of this program, all samples are treated as one of four matrices, animal tissue, plant tissue, soil/sediment, or water):

C.4.1 Assuring a Valid Sample.

• Sample validation upon receipt: condition, identification, and integrity.
• Storage requirements: time and conditions prior to and after analysis.
• Actions required if problems arise in a. or b. above must be clearly defined in Standard Operating Procedures. Especially if a storage system failure occurs.

C.4.2 Assuring a Valid Measurement Process.

1. Only validated methods should be used. Validation includes, at a minimum:

1. Calculation of the Method Detection Limit for each analyte in each matrix.
2. Documentation that minimum acceptable precision has been achieved.
3. Documentation that minimum acceptable accuracy has been achieved.
4. Standard Operating Procedures must be up-to-date, and followed.
5. A state of control must be demonstrated through control charts covering both precision and accuracy.
   
   
2. Instrument Calibration can be accomplished using any standard technique. The following are minimum requirements to verify calibration.
   
   
1. Standards must be "in-date" as defined in a Standard Operating Procedure.
2. Standards must be run for each analyte where practical. SOPs will clearly state when quantitation of an analyte is based on the instrumental response of another.
3. Linearity must be demonstrated with at least three concentrations, in addition to zero and a regression coefficient of >0.995 for each analyte.
4. Mid-range calibration standards must be analyzed after every tenth sample.
5. Standard curves must be analyzed at the beginning and end of a run, and at least daily for multi-day runs.
   
   
3. Samples must be quantified within the demonstrated linear range for the analytical run.
   
4. Limit of detection measurements must be made at least annually. This limit is considered the minimum limit of detection. It is recognized that on an infrequent basis, it may be necessary to adjust detection limits upward to account for interferences in the samples.
   
5. Control charts demonstrating a state of control in both precision and accuracy will be established and maintained for each matrix.

C.4.3 Assuring Precision.

Samples will be analyzed in duplicate at a rate of 5%, with at least one duplicate per matrix per analytical run. This requirement is waived when there is insufficient sample to perform a duplicate analysis.

C.4.4 Assuring Accuracy.

1. At a rate of 5 %, with at least one spike per matrix per analytical run, a sample will be fortified with a known quantity of analyte and analyzed as part of the run. The spike level should be between 10 and 50 times the limit of detection. If there is insufficient sample to analyze a spike of the submitted samples, a "clean" matrix can be used for the spike.
   
2. At a rate of 5%, with at least one per analytical run, a procedural blank will be analyzed.

C.4.5 Reports.

1. Electronic. The Fish and Wildlife Service has established a data base for contaminant analyses. Section J-1 contains specifications detailing the data format and method of transfer that will be used. The validation process described therein is performed by the Service and is provided for your information. Contractor reports cannot be accepted prior to passing this validation. Contractors must be willing to participate in the future development of this system.
   
2. Paper Reports

Paper reports must be available upon request. These reports must include the following:

1. A Description of the samples, their condition on receipt, and storage prior to analysis.
2. A brief summary of the analytical procedures.
3. Analytical results, reported as ppm wet weight, or as % in the case of moisture, lipid, TOC, or grain size determinations.
4. Quality Assurance Report including:
   
1. Results of procedural blank analyses.
2. Results of duplicate analyses, including a computation of the average, and the relative percent difference.
3. Results of spiked sample analyses, including the percent recovery, and the amount in the original sample.
4. Estimate of the limit of detection, on a sample by sample basis.(This can be included in the results section).
5. Discussion of any problems with the analyses

C.4.6 Limits of Detection

For the purposes of this contract, the Limit of Detection is the "Method Limit of Detection" as described by the Environmental Protection Agency in 40 CFR Part 136, Appendix B. In summary, the limit of detection is defined as the Student's t for 99% confidence times the standard deviation of seven replicate measurements of the same low level sample.

Minimum Acceptable Limits of Detection

a- Parts per million (Wet Weight)
b- Parts per million (Dry Weight)
c- As low as possible(to be determined when & if samples are submitted
1- Such as p,p'-DDT
2- Such as toxaphene or PCB-TOTAL or PCB-1254

C.4.7 Precision and Accuracy Acceptance Criteria

The principal measure of accuracy used to assess the quality of data submitted will be the recovery of spiked analyte. The average recovery of most organochlorine, organophosphate, and carbamate pesticides, PCBs, aliphatic and aromatic hydrocarbons from spiked tissue should be between 80 and 120 %. The average recovery of Dioxins, Furans and individual PCB congeners from spiked tissues should be between 60 and 110%.

Additionally, when charted the spike recoveries must indicate that the procedure is in a state of control. Approximately 95 % of the points should be within 2 standard deviations of the mean. In computing the averages, only valid spikes will be used. In a valid spike, the amount of analyte added is at least as much as was present in the sample originally. It is understood that some of the more volatile analytes, such as HCB or naphthalene, will not meet this criterion. In the proposal, the offerer should list those compounds for which the proposed method will not meet this requirement.

Separate charts are to be maintained for each matrix, for each analyte.

The principal measure of precision will be the average relative percent difference (RPD) between duplicates. It is understood that an acceptable RPD will change depending on the proximity of the analyte concentration to the limit of detection. Data reported under this contract will be evaluated according to the table below based on the average analyte concentration of the duplicate pair.

Duplicate Analyses Acceptance Criteria

Additionally, when charted the RPDs must indicate that the procedure is in a state of control. Approximately 95% of the points should be within 2 standard deviations the mean.

Separate charts are to be maintained for each matrix, for each analyte. Separate charts can be maintained for each concentration group, or alternatively a Range Ratio chart can be maintained.

• Average moisture and lipid RPDs should be less than 5 %.
• Average Total Organic Carbon RPDs should be less than 10 %.
• Average grain size RPDs should be less than 20%.

In computing Relative Percent difference, if the concentration of analyte is less than the limit of detection, take half the limit of detection for use in the calculation.

In addition to the quality control performed in conjunction with the actual analyses, the Service will on a periodic basis send proficiency check samples to the laboratory. These samples may or may not be labeled as such. The contractor will be paid for performing these analyses. Any group of samples analyzed by the contractor is subject to call back to the Service for reanalysis in one of its own laboratories. The service will, on occasion, request copies of all raw data for the purpose of conducting a data audit. It is a requirement that the contractor take whatever steps are necessary to correct any deficiencies uncovered.

Contractor shall provide copies of control charts to the COTR, on request.

Inspections of the facilities, or site audits (both announced and unannounced) will be made at the discretion of the Service.

C.4.8 Confirmation of Analyte Identification by Mass Spectrometry

It is required that the identity of compounds identified by gas chromatography (unless the detection is by mass spectrometry) be analyzed by mass spectrometry, for the purpose of confirming analyte identification at a rate such that both of the following are met.

10% of the samples in a single submission are analyzed

1 sample per matrix is analyzed

If all of the analytes are less than the detection limit for performing the mass spec confirmations this requirement is waved. The maximum acceptable mass spectrometric limit of detection is ten times the limit stated above for the various analytes.

Confirmations should be based on GC/MS by Electron Impact (EI) Mass Spectrometry using full scanning or multiple ion scanning with 3 or more ions monitored. It is assumed that the analyst possesses the chemical being confirmed and that all comparisons are made with analyses of this material.

To report an analyte as "CONFIRMED", the spectrum must contain at least three of the major ions. It is usually best that these be the heavier ions since these are less likely to be subject to interference. For the above ions to be accepted their mass chromatographic peaks should be at least three times the background noise, they must be coincident with each other and match the retention times of the standard run under the same conditions. The relative abundances of the three selected ions must be within 30 % of the expected abundances of these ions as determined from analysis of a standard of the compound run on the same instrument and under the same conditions. The three ions must be either selected from separate and unique isotopic cluster groups or if they are within a cluster group the isotopic peaks should be in the correct proportions and the isotopic ratio tolerance match to the standard should be no greater than 20%.

A concentration estimate should accompany the spectral determination and it should be within an order of magnitude of the concentration reported using gas chromatography.

To report an analyte as "TENTATIVELY CONFIRMED" the spectrum must contain at least two of the more abundant ions. For the above ions to be accepted their mass chromatographic peaks should be coincident with each other and match the retention time of the standard run under the same conditions. One of the two ions must be the highest mass which occurs at > 20% of the base peak. The two ions must be selected from either separate and unique isotopic cluster groups or if they are within a cluster group the isotopic peaks should be in the correct proportions.

A concentration estimate should accompany the spectral determination and it should be within an order of magnitude of the concentration reported using gas chromatography.

If an analyte appears to be present, based on gas chromatography, at a concentration higher than the limit of detection for mass spectrometry, and the identity of that compound can not be confirmed or tentatively confirmed by mass spectrometry, it should be assumed that the gas chromatography result is due to an interference. The report should be adjusted (for all samples controlled by the mass spec sample in question) to read < the former result. The detection limit is redefined as the apparent concentration due to the interference.

C.4.9 Corrective Actions

It is required that whenever a quality control sample does not meet the standards listed above, that the procedures be reviewed by the contractor in an attempt to ascertain the cause of the error. If errors are found, the analyses should be repeated from the point of the error. If no errors can be found and the quality control failure appears to indicate that most of the scan is questionable, the analyses should be repeated. If it appears the quality control failure impacted a small number of the analytes within the scan, the Fish and Wildlife Service Quality Assurance Officer should be contacted for a decision. Any corrective action must be applied to all samples analyzed concurrently with the sample which initiated the action.

It can not be stated strongly enough that simply flagging quality control errors is NOT a sufficient action.

C.4.10 Review of Analytical Reports

Each report will be reviewed by the Service Quality Assurance Officer. If any questions arise or problems are discovered the laboratory will be contacted and any required corrective action will be discussed. Payment for services will be authorized, only, after the Service Quality Assurance Officer has approved the report.

C.5 Access to Methods Used

Much of the data provided under the contract will be submitted as part of a scientific publication. It is required that successful offerors provide the Service with either a literature citation that completely describes the methods used or provides the Service with an electronic copy of the Procedures used which will published by the Service on the World Wide Web.