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appendix

 

 

Created by:

 

Florida Department of Environmental Protection - QA Section

 

Standard Operating Procedures

 

FOR LABORATORY OPERATIONS AND SAMPLE COLLECTION ACTIVITIES

 

IMPORTANT NOTICE

This site contains a hypertext version of the DEP's document created for intenal use.
This document is pubblished with absolutely no warranty. User shall not expect this document to be complete, accurate or up to date.

 

Stephane Grounauer

Southern DataStream Inc.

 

  

 

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TABLE OF CONTENTS

 

 

1.0  INTRODUCTION AND USE

1.1  USING THIS MANUAL

1.1.1 Manual Organization

 

1.2  GENERAL SUBMITTAL REQUIREMENTS

1.2.1 Time of Submittal.

1.2.2 Parties Responsible for Submitting Comprehensive QA Plans

1.2.3 Amendments to Approved Comprehensive QA Plans

2.0  INSTRUCTIONS FOR INCORPORATING STANDARD OPERATING PROCEDURES INTO COMPREHENSIVE QUALITY ASSURANCE PLANS

 

2.1  GENERAL

2.1.1 Use of Protocols.

2.1.2 Organizations Adopting all SOPs

2.1.3 Organizations Adopting Portions of the SOPs

 

2.2  STATEMENT OF INTENT TO COMPLY WITH THE DEPARTMENT OF ENVIRONMENTAL REGULATION STANDARD OPERATING PROCEDURES FOR LABORATORY OPERATIONS AND SAMPLE COLLECTION ACTIVITIES

2.2.1 Part I - List of SOPs

2.2.2 Part II - Certification

 

2.3  COMPQAP FORMAT WHEN ALL SOPS ARE ADOPTED

2.3.1 Laboratory or Full Service Organization.

2.3.2 Sample Collection (Field Activities)

2.3.3 Submission Format and Requirements

2.4  COMPQAP FORMAT WHEN ADOPTING PORTIONS OF THE SOPS

 

3.0  ORGANIZATION AND RESPONSIBILITIES.

 

3.1  QUALITY ASSURANCE OFFICER

 

3.2  TECHNICIAN or ANALYST LEVEL

3.2.1 Sample Collection

3.2.2 Sample Analyses

 

3.3  SUPERVISORS and/or SUBSECTION/SECTION MANAGEMENT

 

3.4  PROJECT MANAGEMENT

 

3.5  MANAGEMENT

 

4.0  SAMPLING PROCEDURES

 

4.0  GENERAL.

4.0.1  Sample Collection Order

4.0.2 Use of Protective Gloves

4.0.3 Container and Equipment Rinsing

4.0.4  Dedicated Equipment Storage.

4.0.5  Fuel-powered Equipment and Related Activities

4.0.6  Sampling Procedure References

4.0.7 Preservation

 

4.1  DECONTAMINATION.

4.1.1 General

4.1.2 Reagents

4.1.3  Decontamination/Cleaning Protocols - General Considerations

4.1.4 Decontamination/Cleaning Protocols - Sampling Equipment

4.1.5 Automatic Wastewater Samplers, Sampling Trains and Bottles

4.1.6 Filtration Equipment

4.1.7 Sample Tubing Decontamination

4.1.8 Pumps

4.1.9 Field Instruments and Drilling Equipment

4.1.10 Analyte-Free Water Containers

4.1.11 Ice Chests and Shipping Containers

 

4.2  AQUEOUS SAMPLING PROCEDURES

4.2.1 General

4.2.2 Special Parameter - Specific Handling Procedures

4.2.3 Surface Water Sampling.

4.2.4 Wastewater Sampling

4.2.5 Groundwater Sampling

4.2.6 Wells with In-Place Plumbing.

4.2.7 Potable Well Sampling

4.2.8 Drinking Water Supply System Sampling

4.2.9 Temporary Well Points

4.2.10  Airstripper and Remedial Treatment System Sampling

4.2.11 Bioassay Sampling.

 

4.3  SOLID MATRIX SAMPLING PROCEDURES

4.3.1 General Concerns.

4.3.2 Sample Handling Protocols after Sample Acquisition.

4.3.3 Composite Soil Samples

4.3.4 Soil Sampling

4.3.5  Sediment Sampling.

4.3.6 Fish Tissue Sampling

4.3.7 Shellfish Sampling.

4.3.8 Residual Sampling

4.3.9  Hazardous Waste Sampling.

4.3.10 Sampling Protocols for Macrobenthic Invertebrate Identification.

 

4.4  SAMPLE HANDLING

4.4.1  Sample Containers.

4.4.2 Sample Preservation and Holding Times

4.4.3 Sample Dispatch.

4.4.4 Field Reagent Handling

4.4.5 Field Waste Disposal.

 

5.0  SAMPLE CUSTODY AND DOCUMENTATION

 

5.1  GENERAL REQUIREMENTS FOR CUSTODY AND DOCUMENTATION

5.1.1 Record Keeping System Design - General Requirements.

5.1.2 Documentation Criteria

5.1.3 Record-keeping Protocols

 

5.2  PREPARATION OF FIELD SAMPLING SUPPLIES AND EQUIPMENT

5.2.1 Content Requirements For Sampling Kit Documentation

5.2.2 Documentation for Preservatives.

5.2.3 Documentation of Cleaning Procedures for Sampling Equipment and Containers for Samples, Reagents and Analyte-Free Water.

 

5.3  CUSTODY AND DOCUMENTATION REQUIREMENTS FOR FIELD OPERATIONS.

5.3.1 General Protocols

5.3.2 Sample Identification Requirements

5.3.3 Required Documentation

5.3.4 Required Information

5.3.5 Sample transport

 

5.4  SAMPLE CUSTODY TRACKING AND DATA DOCUMENTATION FOR LABORATORY OPERATIONS

5.4.1 Initial Check of Samples and Documentation

5.4.2 Verification of Sample Preservation

5.4.3  Rejection of Received Samples.

5.4.4 Sample Receipt Logging

5.4.5 Sample Storage.

5.4.6 Sample Disposal

5.4.7 Intralaboratory Distribution of Samples for Analysis

5.4.8 Laboratory Preparation of Samples for Analysis

5.4.9 Tracking for Interlaboratory Transfer of Samples/Subsamples

5.4.10 Sample Analyses Documentation Requirements

5.4.11 Documentation Requirements for Other Laboratory Operations

 

5.5  ELECTRONIC DATA DOCUMENTATION

5.5.1 Retention of Automatic Data Recording Products

5.5.2 Electronic Data Security.

5.5.3 Electronic Data Storage and Documentation

 

5.6  LEGAL OR EVIDENTIARY CUSTODY PROCEDURES

5.6.1 General Requirements

5.6.2 Required Contents for Custody Records

5.6.3 Required Information to be Included on COC Forms Used for Sample Transmittal

5.6.4 Chain-of-Custody Seals.

5.6.5 Controlled Access to Samples

5.6.6 Transfer of Samples to Another Party

5.6.7 Sample Disposal

 

6.0  ANALYTICAL PROCEDURES

 

6.1  LABORATORY GLASSWARE CLEANING PROCEDURES.

6.2  LABORATORY REAGENT STORAGE

6.3  LABORATORY WASTE DISPOSAL

6.3.1 General Disposal/Treatment Considerations.

6.3.2 Storage and Accumulation

6.3.3 Sample Disposal

 

7.0  CALIBRATION PROCEDURES AND FREQUENCY.

 

7.1  INTRODUCTION

 

7.2  GENERAL CONSIDERATIONS

 

7.3  STANDARD RECEIPT AND TRACEABILITY

 

7.4  FREQUENCY OF STANDARD PREPARATION AND STANDARD STORAGE

7.4.1 Standard Storage

7.4.2 Frequency of Standard Preparation

 

7.5  MINIMUM CALIBRATION REQUIREMENTS FOR FIELD INSTRUMENTS

7.5.1  General Considerations

7.5.2 pH Meters

7.5.3 Temperature

7.5.4 Dissolved Oxygen Meter

7.5.5 Specific Conductivity Meter

7.5.6 Chlorine Measurements

7.5.7 Organic Vapor Meters

7.5.8 Automatic Wastewater Samplers

 

7.6  LABORATORY INSTRUMENTS

7.6.1 Initial Calibration

7.6.2 Continuing Calibration.

7.6.3  General Calibration Recommendations by Specific Analysis or Analysis Type**.

 

7.7  SUPPORT EQUIPMENT CALIBRATION

7.7.1 Temperature Monitoring

7.7.2 Autoclaves.

7.7.3  Analytical Balances

 

7.8  CALIBRATION DOCUMENTATION

 

7.9  DEFINITIONS

 

8.0  PREVENTIVE MAINTENANCE.

 

9.0 MINIMUM QUALITY CONTROL REQUIREMENTS AND ROUTINES TO CALCULATE AND ASSESS PRECISION, ACCURACY AND METHOD DETECTION LIMITS

 

9.1  QC CHECKS

9.1.1 Minimum Field Quality Control Requirements

9.1.2 Laboratory QC Checks

 

9.2 ROUTINE METHODS USED TO ASSESS PRECISION AND ACCURACY

 

9.3  METHOD DETECTION LIMITS AND PRACTICAL QUANTITATION LIMITS

9.3.1 Method Detection Limits (MDLs)

9.3.2 Practical Quantitation Limit (PQLs).

9.3.3 Verification

 

9.4  DOCUMENTATION

9.4.1 Field QC Checks.

9.4.2 Laboratory Checks

9.4.3 MDL Studies

 

10.0 DATA REDUCTION, VALIDATION AND REPORTING

 

10.1 DATA REDUCTION

10.1.1  Manual Data Reduction

10.1.2  Computer/Integrator Reduction

10.1.3  Formulae and Calculations

 

10.2 DATA VALIDATION.

10.2.1  Data Integrity.

10.2.2  Data Validation

 

10.3 DATA REPORTING AND OVERALL PROJECT VALIDATION

10.3.1  Laboratory Data Reports

10.3.2  Engineering Project Reports

10.3.3  Project Validation.

 

10.4 DATA STORAGE

 

11.0 CORRECTIVE ACTIONS

 

11.1 QUALITY CONTROL MEASURES AND ACCEPTANCE CRITERIA

 

11.2 IDENTIFYING AND ASSESSING QC MEASURES

 

11.3 DETERMINING THE SOURCE OF QC PROBLEMS.

 

11.4 INITIATING CORRECTIVE ACTION

 

11.5 SPECIFIC CORRECTIVE ACTIONS

 

11.6 DOCUMENTATION AND NOTIFICATION OF AFFECTED PARTIES

 

11.7 CORRECTIVE ACTIONS FROM EXTERNAL SOURCES

 

12.0 PERFORMANCE AND SYSTEMS AUDITS

 

12.1 FIELD AUDIT REQUIREMENTS

12.1.1 Internal Audits.

12.1.2  External Audits

12.1.3  Project Audits - Data Validation by DER

 

12.2  REQUIREMENTS FOR AUDITS OF LABORATORY OPERATIONS.

12.2.1  External Audits.

12.2.2  Internal Audits

 

12.3 REGULATORY REQUIREMENTS.

 

13.0 QUALITY ASSURANCE REPORTS.

 

13.1 QA REPORTS TO DER.

 

13.2 REPORT FORMAT AND CONTENT

13.2.1 Requirements for a Full Report.

13.2.2 Contents

 

13.3 FREQUENCY

 

13.4 INTERNAL QA REPORTS.

 

LIST OF FIGURES

 

Figure 2.1 - Document Control Header Placement.

Figure 2.2 - Example of Sample Preparation Table.

Figure 2.3 - Example of QA Objectives Table of Laboratory Measurements.

Figure 2.4 - Example of Methods Table for Field Measurements

Figure 2.5 - Example of Table of Sampling Capabilities.

Figure 2.6 - Example of Field Equipment Table.

Figure 4.1 - Diagram of System for Collecting Organics through a Peristaltic Pump.

Figure 4.2 - Diagram of Recommended Field Filtration System for Trace Metals

Figure 13.1 - Title Page for QA Report to DER.

Figure 13.2 - Example of Audit Summary Table

 

LIST OF TABLES

 

Table 2.1 - Mandatory SOP Chapters to be Adopted

Table 2.2 - Required Tables in Section 2.0 of CompQAPs that Adopt all SOPs.

Table 2.3 - DER Approved Analytical Methods and References for Water and Biological Analyses

Table 2.4 - DER Approved Analytical Methods and References for Sediments, Soils, Residuals and Solid and Hazardous Wastes

Table 2.5 - DER Approved Methods for Special Conditions

Table 4.1 - Sampling Equipment - Construction and Appropriate Use

Table 4.2 - 40 CFR Part 136 Table II:  Required Containers, Preservation Techniques and Holding Times (Waster/Wastewater Samples)

Table 4.3 - Approved Water and Wastewater Procedures, Containers, Preservation and Holding Times for Parameters Not Found in 40 CFR 136

Table 4.4 - Recommended Sample Containers, Sample Volumes, Preservation Techniques and Holding Times for Residuals, Soil and Sediment Samples

Table 4.5 - Preservation Methods and Holding Times for Drinking Water Samples that Differ from 40 CFR Part 136 Table II     

Table 8.1 - Preventive Maintenance Activities.

Table 10.1 - Data Reporting Units.

Table 10.2 - Data Qualifier Codes

Table 11.1 - Acceptance Criteria and Corrective Actions for Quality Control Checks.

Table 11.2 - Probable Sources and Expected Corrective Actions

Table 13.1 - Quality Assurance Reports to DEP -  Submittal Frequency for Quality Assurance Project Plans

 

APPENDICES

 

APPENDIX A - Definitions.

APPENDIX B - Selected References.