GREAT LAKES AGRICULTURAL RESEARCH SERVICE

N6084 JOHNSON ROAD

DELAVAN, WISCONSIN 53115

STANDARD OPERATING PROCEDURES

FIELD RESIDUE TRIALS

SOP l.0 General Procedures and Considerations

Revision No. 14 - Effective May 12, 2000

Prepared by: Susan K. Bellman; Principal Investigator

l. Purpose:

The purpose of this Standard Operating Procedure (SOP) is to summarize the procedures for conducting field residue trials at Great Lakes Agricultural Research Service, Inc. (GLARS). These trials will be conducted in a routine, documented format in order to comply with the EPA's Good Laboratory Practice Regulation 40 CFR part 160 (GLPs).

2. Standard Operating Procedures (SOPs):

Specific Standard Operating Procedures have been developed to assure that all phases of field residue trials are carried out in a standard procedure and to ensure that all personnel are trained in the same manner. See SOP 1.1 for details on writing and reviewing SOPs. The SOPs that are being used at the present time at GLARS can be found in SOP 0.0 Table of Contents and SOP 0.1 Table of Contents of Q.A. SOPs.

3. Personnel:

GLARS management should maintain records of education, training, and experience for all personnel. Prior to trial initiation, the president of GLARS will designate a Principal Investigator (PI) who will coordinate all phases of the trial (SOP 2.0).

Employees will be trained in safety procedures (see SOP 2.5) and in GLP procedures (see SOP 2.6).

4. Facilities and Equipment:

All facilities and equipment are to be maintained to ensure accurate application rates and to prevent contamination of residue samples (see SOP 2.1). Personnel involved with a field residue trial will be familiar with facilities, equipment, and proper maintenance techniques. Maintenance and cleaning procedures are detailed in SOP 2.2.

5. Trial Scheduling:

Trial scheduling for field residue trials is necessary to ensure that all studies are conducted in a routine, documented manner. Each trial conducted at GLARS will be assigned a GLARS trial number. This trial number will be used for tracking the trial's progress at GLARS.

Two types of project tracking schedules will be kept. The GLARS GLP Master Schedule will contain the information required in the GLPs. Confidential information will be coded. The GLARS Project Schedule will be used by GLARS personnel to identify trials by test substance, crop, location, etc.

An Application/Sampling Schedule (Wall Charts) will also be kept so that GLARS employees can plan their work schedules on a daily basis (See SOP 1.2).

6. Protocol:

Each residue trial conducted under the GLPs must have a protocol signed by the Study Director. The protocol should contain information concerning test substance, test system, application requirements, sampling requirements, and shipping.

7. Protocol or SOP Deviations:

There will be occasions when the protocol and/or a SOP are not followed. An amendment is a planned addition, deletion, or change to the protocol. The Study Director will generally write an amendment.

A deviation is an unplanned change or mistake that is usually noted after the fact. If no procedure for handling deviations is given by the Sponsor Company, the following procedure should be used:

1. The Principal Investigator should fill out a Deviation Form (See SOP 5.1).
2. The GLARS QA Auditor should be made aware of the deviation and acknowledge this by signing the deviation form.
3. If the occurrence is a protocol or SOP deviation that may affect the study outcome, the Study Director or his designate should be made aware of the deviation by phone.
4. After the deviation form has been signed by the Principal Investigator and the GLARS QA Auditor, it should be sent to the Study Director or his designate for acknowledgment. A copy should be kept in the FTN.
5. The Study Director is requested by GLARS to send a signed copy of the deviation acknowledgment back to GLARS.

8. Documentation of Raw Data:

Raw data are recorded values, observations, notes, calculations, correspondence, documentation of phone calls, original shipping receipts, etc. that enable the Principal Investigator to reconstruct the field residue trial. Raw data are the first point of entry and should be written in black ink, dated, and signed or initialed. It is acceptable for the person entering raw data to sign using his or her initials after signing the personnel page of the Field Trial Notebook (FTN). Generally the personnel page of the FTN asks for printed name, signature, and initials.

Transcribed data are any original raw data that have been copied from one location to another. Transcribed data should be identified as such, dated, initialed, and the original source documented.

There will be times when raw data will need to be changed (misspelling, etc.). The original data must not be obscured. The following procedure must be followed:

1. Draw a single line through the data entry to be changed.
2. Sign or initial adjacent to the change and record the date and reason for the change. Common abbreviations used by GLARS personnel and codes for changing raw data can be found in Appendix A of this SOP.

Non GLP data (i.e. field history, tillage information, etc.) will at times be entered into the FTN. The source of the non-GLP data should be mentioned.

9. General Filing Procedures:

GLP records need to be maintained in an orderly, precise manner. The following filing procedures will be used:

1. Only one trial shall be filed per Field Trial Notebook (FTN).
2. Additional papers added to the FTN should bear the GLARS trial number, the study number, and the company trial number.
3. FTNs will be stored in the GLARS office, in a fire proof, locked file cabinet. Files are accessible only to the GLARS Principal Investigator, Research Technician, Efficacy Technician, Farm Technicians, Farm Manager, and the Quality Assurance Auditor.
4. FTNs must be transported from the office to the field at various phases of each trial. During transport, care will be taken to minimize damage.
5. The finalized FTN will be transferred to the Sponsor Company (See SOP 8.0).

10. Copying:

Copies of raw data are routinely made during the conduct of a GLP trial. The following procedures are to be used when making copies:

1. Review each copy to make sure it is dark enough and legible.
2. Make sure that all of the information along the edge of the page has been copied. If necessary, reduce the page to make a good copy.
3. Stamp each copy "Exact Copy" using the red ink pad and initial and date the "Exact Copy" stamp. Some FTNs have an "Exact Copy" statement at the bottom of the page. This can be filled out instead of using the GLARS stamp.

11. Organizing the Field Trial Notebook (FTN):

Sponsor Companies generally will supply a Field Trial Notebook (FTN). If this notebook is not supplied or the company supplies loose forms, then GLARS will organize a FTN as described below.

Forms for the following information are provided in GLARS SOP 5.1 or as otherwise stated below. There are times when more than one page of the same form is needed. The first page should be 16A, the second page 16B, etc. The last page number should be circled. This method will be used unless the protocol or FTN instructions state otherwise.

A. Protocol and Amendments

B. GLP Compliance:

1. Signature page (i.e. the names, titles, signatures and initials) for all personnel who entered raw data into the FTN. The Q.A. Auditor does not sign this form, unless requested to do so (See SOP 8.0).
2. Statement of Compliance with the GLPs signed by the Principal Investigator.
3. The GLARS Quality Assurance Inspection Statement (see SOP 7.0).
4. Deviation forms (if applicable).

    C. Test Site:

1. Trial Location Road Map (see SOP 1.65).

2. Bellman Farm Field/PM Map for trials located on-site (see SOP 1.65).

3. Field Residue Trial Plot Map (see SOP 1.65).

4. Soil/Water Characterization, if required.

5. Field History (see SOP 1.65).

6. Test System Agronomic Information and Cultural Practices

7. Statement of Crop Destruction (if applicable)

    D. Weather Data:

1. Monthly Weather Data Reports (See SOP 8.0).

2. Historical Weather Data (if requested)

3. Irrigation Scheduling (if applicable)

    E. Test Substance (See SOP 1.3):

1. Test Substance Receipt Form

2. Test Substance receipt paperwork.

3. Test Substance Usage Form

4. Test Substance return paperwork, including Chain of Custody Form.

5. Monthly Chemical Storage Room Temperature Reports

    F. Calibration/Application:

1. Calibration Worksheet and/or relevant pages of Equipment Calibration Log Book.

2. Application Spray Chart

3. Application/Environmental Information

4. GLARS Rate Verification Form or Sponsor Company Form

    G. Sampling/Shipping:

1. Sampling Information (See SOP 4.0)

2. Shipping Information (See SOP 4.5)

3. Sample Chain of Custody form

4. Monthly Freezer Temperature Reports (See SOP 8.0)

8. Chronological Log
9. GLARS and/or Sponsor Company’s SOPs (any relevant or requested).
10. Memos, correspondence, misc. information such as CVs.

12. Test Substance Receiving, Storage, Usage, and    Disposal:

The EPA requires a detailed paper trail to certify that test substances have been maintained in satisfactory condition without possible deterioration or contamination. It is important that each test substance be received, handled, stored, and returned in a manner such that a complete record is maintained. See SOP 1.3 for details.

13. Residue Trial Design:

1. All field residue trials will be conducted at sites where GLARS can dictate or have control over those operations that can affect the outcome of the test.
2. Wherever possible, the site location will be representative of the major production areas for the target crop.
3. Field residue trials will not be combined with efficacy trials.
4. Refer to the protocol for minimum plot size, minimum buffer size, number of replications/subplots, and sample size (i.e. a large sample size will require a larger plot, etc).
5. Plot Layout:

1. The plot layout should leave enough buffer area between the treated plot and the untreated check plot such that no drift/volatility/runoff will occur to contaminate the check plot. Generally the UTC plot should be located upslope and upwind of the treated plot.
2. The buffer area can be planted to a commercial crop, cover crop, or left vacant. A common cover crop is red clover at 5-7 lb/acre plus annual ryegrass at 8-10 lb/acre.
3. Mark the 4 corners of the plot with wooden garden stakes and/or flags. The UTC plot is usually marked in white and the treated plot is usually marked with a different color such as orange or blue. Use colored flags or painted wooden stakes in tall crops like alfalfa. Use approximately 4-foot tall wooden stakes in aerial plots or in 2-year studies.
4. Place a plot label in the lower left-hand corner of the plot as you are facing the plot from the front. Generally the plot label will be a white index card attached to a garden stake. The label should contain the GLARS Trial number, the Treatment number, and any other information requested in the protocol.
5. The plot layout should be documented using a Location Map, a Bellman Farm Field/PM Map (on-site trials only), and a Trial Plot Map (See SOP 1.65).

14. Soil or Water Characterization:

Soil or water characterization samples are taken according to protocol specifications (See SOP 4.1). If soil and/or water characterization is not mentioned in the protocol it will be assumed that there is no requirement for such information.

15. Crop Maintenance:

Normal grower practice will be used to ensure a good, healthy crop. Refer to SOP 1.6 for crop maintenance procedures and crop development stages.

16. Crop Destruction:

The protocol should specify whether or not the treated crop should be destroyed. If crop destruction is required, it should be documented in the FTN. If crop destruction is not mentioned in the protocol it will be assumed that crop destruction is not required and will not be done.

17. Statement of Compliance with GLPs:

All completed residue trials should have a statement signed by the Principal Investigator stating that the work conducted at GLARS was done according to the GLP Regulation. If the Sponsor Company does not supply one, the GLARS Principal Investigator will use the one found in SOP 5.1.

18. APHIS Trials:

Periodically GLARS conducts trials under the APHIS Regulation. APHIS trials have several different requirements than GLP trials. See SOP 11.0 for details.

19. Archiving:

GLARS will archive historical records in such a way as to minimize deterioration of the documents in accordance with the GLPs.

The GLARS Archivist is responsible for archiving non-Q.A. data (See SOP 8.5).

The GLARS QA Auditor is responsible for archiving QA data (See SOP 7.0).

20. Quality Assurance:

21. Plan for Closing Great Lakes Ag-Research Service, Inc.:

If GLARS should go out of business at some time in the future, the following procedure will be followed:

1. All non-trial specific active logs and files will be archived.
2. All trial specific files will be returned to the appropriate Sponsor Companies.
3. The Sponsor Company for which GLARS has conducted the largest number of trials will be contacted and asked to take over responsibility for GLARS non-trial specific archived data. See SOP 8.5 for a list of archived data.
4. All other Sponsor Companies and the EPA will be notified in writing of the location of the archived data.