DEP SOPs
 

Site index

Home
comments to table 2.1

 

 

Created by:

 

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

 

2.1        GENERAL

 

2.1.1     Use of Protocols

      The protocols that are outlined in this document must be carefully reviewed before making the decision to adopt the SOPs.

 

2.1.2     Organizations Adopting all SOPs

 

      2.1.2.1  Organizations that adopt all SOPs that are relevant to their operations will be given approval for all analytical methods or sampling capabilities that are consistent with the submitted equipment and instrumentation lists.

 

      2.1.2.2  Determination of approval status will occur within one month of submission.

 

      2.1.2.3  Note that approval MAY NOT include all capabilities (i.e. analytical methods or sampling protocols) that are listed in the CompQAP.  Approval will be contingent on the use of

approved analytical methods (see 2.3.3.4.b), adoption of all appropriate SOPs, and use of appropriate equipment and/or instrumentation.

 

2.1.3     Organizations Adopting Portions of the SOPs

 

      2.1.3.1  An organization that does not wish to adopt all SOPs pertinent to their operations must submit a full Comprehensive Quality Assurance Plan specified by DER-QA-001/90, however, the selected SOPs may be incorporated by reference.

 

      2.1.3.2  Organizations that adopt all pertinent sample collection protocols may be given limited approval pending status subject to the requirements specified in 2.1.2 above.

 

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

 

      A Statement of Intent is required when adopting all or portions of the protocols listed in this document.

1.   The Statement is a two-part document which must be completed and signed by the appropriate parties.

 

2.   The Statement MUST BE SUBMITTED WITH SUPPORTING INFORMATION.  If adopting all SOPs, the organization must submit tables which include lists of personnel, methods and equipment (Section 2.3).  If adopting some of the SOPs, the organization

must submit a CompQAP with the Statement (Section 2.4).

 

3.   The document WITH ORIGINAL SIGNATURES must be submitted with all other required information; it will not be accepted if submitted without supporting documentation (see 2.3 and 2.4) or if a copy of facsimile is submitted.

 

4.   This document may be obtained from the a DER District Office or by writing to the Florida Department of Environmental Regulation, DER Library, 2600 Blair Stone Road, Tallahassee, Florida 32399-2400.

 

5.   This document shall not be retyped or modified.  A Statement of Intent that has been retyped by the organization WILL NOT BE ACCEPTED.

 

2.2.1     Part I - List of SOPs

 

      2.2.1.1        The first part is a list of all SOP activities and protocols.  Complete this portion by:

a.         Filling in the name and address of the organization and the CompQAP number (if already assigned);

b.         Placing an "X" or checkmark by each of the SOPs that your organization intends to adopt.  If the organization does not have the capability, personnel or equipment to perform certain tasks (i.e. hazardous waste sample collection, wastewater sample collection, etc.), DO NOT check the associated SOPs.

 

      2.2.1.2        Mandatory SOPs that must be Adopted

a.         If an organization intends to follow only adopted SOPs, Table 2.1 identifies the document chapters and/or sections that must be adopted and checked on the Statement of Intent.

b.         Organizations that adopt portions of the SOPs must indicate those that are to be adopted.  NOTE:  THE INFORMATION THAT IS NOT ADOPTED BY SOPs MUST BE DISCUSSED IN THE TEXT OF THE CompQAP (see Section 2.4).

 

      2.2.1.3        Before determining the status of your QA Plan, this part of the statement will be checked for inconsistencies and/or omission of pertinent SOPs as well as correlation between the SOPs and the submitted equipment and instrument lists.

 

2.2.2     Part II - Certification

 

      2.2.2.1        The second part of this document is a certification.  This portion certifies that the organization:

a.         Has obtained copies of all documents specified by the SOPs;

b.         Intends to follow all SOPs noted in Part I;

c.         Has the equipment and capability to perform the protocols specified by Part I; and

d.         Is committed to generating data of a known and verifiable quality.

 

      2.2.2.2        The Statement of Intent must be signed by at least two individuals:

a.         An individual who will be ultimately responsible for the quality, and reliability of all data generated by the organization (usually the laboratory manager, director of field operations, etc.); and

b.         The Quality Assurance Officer(s) of the organization.

 

      2.2.2.3        The Statement must be properly dated and signed.


TABLE 2.1

MANDATORY SOP CHAPTERS TO BE ADOPTED

 

 CHAPTER/SECTION TITLE

 LABORATORY ONLY

FIELD (SAMPLE

COLLECTION ACTIVITIES)

FULL SERVICE FIELD & LAB

CHAPTER 3  -  ORGANIZATION AND RESPONSIBILITY X X X
CHAPTER 4  -  SAMPLING PROCEDURES      

 

Section 4.0  -  General

 

 

Section 4.1  -  Equipment Decontamination

 

 

Section 4.1.1

General Concerns

X (1)

X

X

 

Section 4.1.2

Reagents

X (1)

X

X

 

Section 4.1.3

General Decontamination Protocols

X (1)

X

X

 

Section 4.1.4

Sampling Equipment

X (1,2)

X

X

 

Section 4.1.5

Wastewater Automatic Samplers

X (1,2)

X (2)

X (2)

 

Section 4.1.6

Field Filtration Equipment

X (1,2)

X (2)

X (2)

 

Section 4.1.7.1

Teflon Tubing

X (1,2)

X (2)

X (2)

 

Section 4.1.7.2 - 5

Non-Teflon Tubing

X (1,2)

X (2)

X (2)

 

Section 4.1.8

Pumps used for Purging and/or Sampling

X (1,2)

X (2)

X (2)

 

Section 4.1.9

Field Meters, Flow Meters, and

 

 

 

 

 

    other Field Instruments

X (1,2)

X (2)

X (2)

 

Section 4.1.9

Non-Sampling Equipment

X (1,2)

X (2)

X (2)

 

Section 4.1.10

Analyte-Free Water Containers

X (1,2)

X (2)

X (2)

 

Section 4.1.11

Ice Chests and Shipping Containers

X (1,2)

X (2)

X (2)

 

Section 4.2  -  Aqueous Sampling Procedures

 

 

Section 4.2.1

General Sampling Concerns

 

X (3)

X (3)  

 

Section 4.2.2

Specific Sample Handling Procedures

 

X (3)  

X (3)  

 

Section 4.2.3

Surface Water

 

X (4)

X (4)

 

Section 4.2.4

Wastewater

 

X (4)

X (4)

 

Section 4.2.5

Groundwater

 

X (4)

X (4)

 

Section 4.2.6

Wells with In-Place Plumbing

 

X (4)

X (4)

 

Section 4.2.7

Potable Wells Sampling

 

X (4)

X (4)

 

Section 4.2.8

Drinking Water Supply Systems

 

X (4)

X (4)

 

Section 4.2.9

Temporary Well Points

 

X (4)

X (4)

 

Section 4.2.10

Air Stripper and Remedial Treatment Systems

 

X (4)

X (4)

 

Section 4.2.11

Bioassay

 

X (4)

X (4)

 

Section 4.3  -  Solid Matrix Sampling Procedures

 

Section 4.3.1

General Sampling Concerns

 

X (3)  

X (3)  

 

Section 4.3.2

Specific Sample Handling Protocols after Sample Acquisition

 

X (3)  

X (3)  

 

Section 4.3.3

Composite Soil Samples

 

X (3)  

X (3)  

 

Section 4.3.4

Soil Sampling

 

X (4)

X (4)

 

Section 4.3.5

Sediment Sampling

 

X (4)

X (4)

 

Section 4.3.6

Fish Tissue Sampling

 

X (4)

X (4)

 

Section 4.3.7

Shellfish Sampling

 

X (4)

X (4)

 

Section 4.3.8

Domestic Wastewater Residual Sampling

 

X (4)

X (4)

 

Section 4.3.9

Hazardous Waste Sampling

 

X (4)

X (4)

 

Section 4.3.10

Macrobenthic Invertebrates

 

X (4)

X (4)

Section 4.4  -  Sample Handling

 

Section 4.4.1

Sample Container Cleaning

X (5)

X

X

 

Section 4.4.2

Sample preservation, container types

 

 

 

 

 

    and holding times

X

X

X

 

Sources of preservation

 

X (6)

X (6)

X (6)

 

Section 4.4.3

Sample Dispatch

 

X

X

 

Section 4.4.4

Field Reagent Handling

 

X

X

 

Section 4.4.5

Field Waste Disposal

 

X

X

 

CHAPTER 5  -  SAMPLE CUSTODY AND DOCUMENTATION

 

 

 

 

Section 5.1

General Requirements for Custody and

 

 

 

 

 

 

    Documentation

X

X

X

 

 

Section 5.2

Preparation of Field Sampling Supplies

 

 

 

 

 

 

    and Equipment

X (1,5)

X

X

 

 

Section 5.3

Custody and Documentation Requirements for

 

 

 

 

 

 

Field Operations

 

X

X

 

 

Section 5.4

Custody and Documentation Requirements for

 

 

 

 

 

 

Laboratory Operations

X

 

X

 

 

Section 5.5

Electronic Data Documentation

X (4)

X (4)

X (4)

 

 

Section 5.6

Legal or Evidentiary Custody Procedures

X (4)

X (4)

X (4)

 

 

CHAPTER 6  -  ANALYTICAL PROCEDURES

 

 

 

 

CHAPTER 7  -  CALIBRATION PROCEDURES AND FREQUENCY

 

 

 

 

Section 7.1

Introduction

X

X

X

 

 

Section 7.2

General Considerations

X

X

X

 

 

Section 7.3

Standard Receipt and Traceability

X

X

X

 

 

Section 7.4

Frequency of Standard Preparation and

 

 

 

 

 

 

    Standard Storage

X

X

X

 

 

Section 7.5

Minimum Calibration Requirements for

 

 

 

 

 

 

    Field Instruments

 

X

X

 

 

Section 7.6

Laboratory Instruments

X

 

X

 

 

Section 7.7

Support Equipment Calibration

X

 

X

 

 

Section 7.8

Calibration Documentation

X

X

X

 

 

Section 7.9

Definitions

X

X

X

 

 

CHAPTER 8  -  PREVENTATIVE MAINTENANCE

X

X

X

CHAPTER 9  -  MINIMUM QC REQUIREMENTS AND ROUTINES TO CALCULATE AND

    ASSESS PRECISION, ACCURACY AND METHOD DETECTION LIMITS

 

Section 9.1.1

Minimum Field Quality Control Requirements

 

X

X

 

Section 9.1.2

Minimum Laboratory Quality Control

 Requirements

X

 

X

 

Section 9.2

Routine Methods used to Assess Precision

 

 

 

 

 

and Accuracy

X

 

X

 

Section 9.3

Method Detection Limits and Practical

 

 

 

 

 

Quantitation Limits

X

 

X

 

Section 9.4

Documentation

X

X

X

 

 

CHAPTER 10  -  DATA REDUCTION, VALIDATION AND REPORTING

X

X

X

 

CHAPTER 11  -  CORRECTIVE ACTION

X

X

X

 

CHAPTER 12  -  PERFORMANCE AND SYSTEM AUDITS

X

X

X

 

CHAPTER 13  -  QUALITY ASSURANCE REPORTS

X

X

X

 

X  -  Section must be adopted, subject to the following comments:

 

(1)  Laboratories providing equipment cleaning services must adopt this section

(2)  Adopt only those protocols for which equipment is provided (laboratories) and/or listed (field and full service)

(3)  Mandatory if protocols discussed in the subsection are adopted

(4)  Adopt only if applicable

(5)  Laboratories providing sample containers must adopt this section

(6)  The manner in which preservatives are provided/obtained must be specified


2.3        COMPQAP FORMAT WHEN ALL SOPS ARE ADOPTED

 

      Organizations adopting the SOPs that are pertinent to their operations are required to submit the following information:

 

2.3.1     Laboratory or Full Service Organization

      1.   Statement of Intent;

      2.   Names of the key personnel within the organization;

      3.   Table of Method numbers, matrix identification and QA Objectives for Precision and Accuracy;

      4.   List of all analytical instrumentation and support equipment.

      5.   List of sampling capabilities (if applicable); and

      6.   List of sampling equipment (if applicable).

 

2.3.2     Sample Collection (Field Activities)

      1.   Statement of Intent;

      2.   Names of the key personnel within the organization;

      3.   Table of Method numbers for field measurements;

      4.   List of sampling capabilities; and

      5.   List of sampling equipment.

 

2.3.3     Submission Format and Requirements

 

      2.3.3.1        General Requirements

a.         All Comprehensive QA Plans shall be submitted to the QA section in 3-ring loose leaf binders.  This allows the QA section and the consultant to easily update or amend specific pages or sections by removing outdated sections and inserting the new revisions.

b.         All plans must be submitted as final plans.  Draft documents or documents identified as draft will be returned unreviewed.

c.         Incomplete plans or plans that do not conform to the formats specified in this document shall be returned unreviewed.

d.         Only one (1) copy of the plan must be submitted to the DER QA Section.  Note:  DER program managers may request additional copies of the approved QA Plan for their records, however, only one plan should be submitted to the QA section.

e.         The QA Plan must be submitted in numbered sections which correspond to the list of topics outlined in Section 2.3.1 or 2.3.2 above.  All sections (except the Statement of Intent) must be identified with a document control header which shall be placed in the upper corner opposite the binding of each document page with the following information:

      1.   Section No. - identifies the Section/Element

      2.   Date - is the date of the revision

      3.   Page          of          - identifies the specific page within in the section, and the total number of pages in the section (see Fig. 2.1).

      NOTE:  SECTIONS ARE TO BE NUMBERED ACCORDING TO TITLES IN SECTIONS 2.3.3.3 THROUGH 2.3.3.6 OF THIS DOCUMENT.

 

      2.3.3.2        Statement of Intent - Complete per instructions in Section 2.2 above.

 

      2.3.3.3        Section 1.0 - Key Personnel

a.         Provide a list of the salaried employees with title.

b.         The list should include KEY PERSONNEL, only.  Key personnel are defined as:  all individuals from the owner/director/manager through line supervisors.

c.         Provide a list of branch offices (including address and phone number) IF this CompQAP is to be used by more than one office.  Key personnel (with title) for each office shall be identified

 

      2.3.3.4        Section 2.0 - Organization Abilities (Methods, Matrices, QA Targets and Sampling Capabilities)

 

            This section must outline the capabilities of the organization in terms of analytical or testing methods (this section) AND, IF APPLICABLE, sampling capabilities (Section 2.3.3.5).  All information shall be presented in table form.  The number of tables that will be required are dependent on the capabilities of the organization and are outlined on Table 2.2.

      The instructions in this section pertain to the required tables for analytical and field measurement capabilities:

 

a.         General Requirements

      1.   This section must include ALL field, biological and chemical analytical (measurement) capabilities of a laboratory on consulting firm that are pertinent to DER programs and rules.  The components in each method must be listed separately.

      2.   This information must be presented in table form as described in Section 2.3.3.4.c below.

      3.   The analytical methods for field measurement parameters (pH, specific conductance, temperature, etc.) must be presented as a separate table.  If equipment such as OVAs are used to screen samples in the field, the method should not be listed in this section.  The equipment must be listed on the list of field equipment (Section 2.3.3.6.a)and pertinent calibration and preventative maintenance SOPs must be checked on the Statement of Intent.

      4.   Precision, Accuracy and Detection limits or goals must be provided for all parameters (EXCEPT field measurements and screening methods).  If not available from in-house data, literature or method values may be used but must be identified with appropriate annotations.  DER encourages generation of in-house QA objectives for all components (unless otherwise specified by the method) and expects that this table will be completed with in-house data no later than one year after final approval.

      5.   The precision, accuracy and detection limits presented in the CompQAP shall be the routine target values used by the consultant.  Deviations from these criteria must be addressed in quality assurance project plans.

 

b.         Approved Methods

      1.   All analyses must be performed in accordance with currently accepted DER methods (listed on Tables 2.3, 2.4 and 2.5).

            2.         If there is no DER approved method for a specified component, the following alternatives may be used:

a.         DER will review proposed existing methods other than those listed in Tables 2.3, 2.4 and 2.5 and approve the use of the method, if appropriate.  Sources of such methods may be (see references in Appendix B for specific revision dates):

1.   Standard Methods

2.   ASTM - American Society for Testing Materials

3.   USGS - U.S. Geological Survey

4.   AOAC - Methods of Analysis of the Association of Official Analytical Chemists

.

Figure 2.1 DOCUMENT CONTROL HEADER PLACEMENT

 

 

Table 2.2 REQUIRED TABLES IN SECTION 2.0 OF COMPQAPs THAT ADOPT ALL SOPs

 

Table Identification

Laboratory

Field

Full-Service

 

 

 

 

Analytical Test Methods

X

 

X

Sample Preparation Methods *

X

 

X

Field Measurements

 

X

X

Sampling Capabilities

 

X

X

 

      *      Required only if SW 846 methods are proposed as analytical test methods.

 

      Laboratory   - Provides only analytical services

      Field            - Provides only sample collection services

      Full-Service - Provides both sample collection and analytical services

 


Table 2.3 DER APPROVED ANALYTICAL METHODS AND REFERENCES FOR WATER

AND BIOLOGICAL ANALYSES

 

DRINKING WATER

      These methods must be used when analyzing potable waters for compliance with Chapters 17-550, 17-551, 17-555 and 17-560, F.A.C. and/or for certification under the HRS Drinking Water Certification program.

      1)      40 CFR Part 141, National Primary Drinking Water Regulations, July 1, 1991 Edition, Code of Federal Regulations, Subpart C (Monitoring and Analytical Requirements, sections

141.21 to 141.30) and Subpart I (Control of Lead and Copper, section 141.89).

      2)      "Methods for the Determination of Organic Compounds in Drinking Water," EPA 600/4-88-039, December 1988.

      3)      Chapter 10D-41, sections 50 to 62, F.A.C., Amended 11-15-90, HRS Laboratory Certification Rules (Drinking Water Analyses).

      4)      "Methods for Chemical Analysis of Water and Wastes," EPA 600/4-79-020, revised March 1983.

      5)      Standard Methods for the Examination of Water and Wastewater, APHA-AWWA-WPCF, 17th Edition, 1989.

      6)      "Manual for Certification of Laboratories Analyzing Drinking Water, Criteria and Standards Quality Assurance" EPA 570/9-90-008, April 1990 as updated by Change I (EPA

570/9-90-008A), October 1991 and Change 2 (EPA-814B-92-002), September 1992.

      7)      40 CFR Part 136, Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act, July 1, 1991, Appendix A.

 

      NOTES:

      1)      "500" series methods shall be used only for regulatory analysis of drinking water (see above statement) unless approved by DER for use in other matrices or programs. 

      2)      Only Methods 502.1, 502.2, 503.1, 504, 505, 507, 508, 508A, 515.1, 524.1, 524.2 and 531.1 from Reference 2 and Methods 604, 606, 609, 612, 613 and 625 from Reference 7 are approved for analysis of drinking water by state certified laboratories.

 

SURFACE WATER, GROUNDWATER, AND WASTEWATER (DOMESTIC/INDUSTRIAL) EFFLUENTS

      1)      40 CFR Part 136, Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act, Tables IA, IB, IC, ID, and IE, as published in the Federal Register, Vol. 65, No. 165, pp. 50758-50770, October 8, 1991.

      2)      Methods for Chemical Analysis of Water and Wastes, EPA 600/4-79-020, revised March 1983.

      3)      "Test Methods for Evaluating Solid Waste, Physical Chemical Methods", Third Edition (EPA SW-846), 1986 as amended by Final Update 1, November 1990.

      4)      40 CFR Part 261, Identification and Listing of Hazardous Waste, July 1, 1991, Appendix III (Chemical Analysis Test Methods).

 

      NOTES:

      1)      Laboratories analyzing samples in support of NPDES Permits are limited to methods specified in Reference 1 above or those specifically approved for use by EPA.

      2)      Only those methods in Reference 2 which are specified in Reference 1 are approved.

Table 2.3, cont.

DER APPROVED ANALYTICAL METHODS AND REFERENCES FOR WATER

AND BIOLOGICAL ANALYSES

 

      3)      Methods and protocols specified by References 3 and 4 above must be used when analyzing samples in support of RCRA related activities.

 

      Approved Methods to be used in support of DER Rules and Programs:

      1)      Pesticides and Herbicides:

     a.     "Methods for the Determination of Nonconventional Pesticides in Municipal and Industrial Wastewater," EPA 821 RR-92-002, April 1992.  Note:  methods in the Appendix (EV-024 and EV-025) require method validation from the laboratory.

     b.     N-Methyl Carboxylamines and N-Methyl Carbamates - EPA Method 531 (600/4-88-039).  Approved ONLY for the analysis of these components in groundwater samples.

 

      2)      Inorganics:**

      a.      BROMINE - SM 408E, SM 4500-Cl-G - The approved method is for residual chlorine.  However, in the absence of chlorine, the DPD colorimetric procedure can be adapted to measure bromine content of the sample.  In such case, the validity of this assumption must be verified by using another procedure for chlorine which is not affected by the presence of bromine (i.e. negligible interference).

     b.     BROMATES - EPA 300.0 B - "Determination of Inorganic Anions in Water by Ion Chromatography" by Jack D. Pfaff, Carol A. Brockoff, and James W. O'Dell, U.S. EPA, Cincinnati, Ohio, 45268.

     c.     CHLOROPHYLLS - SM 1002G, SM 10200 H

     d.     CORROSIVITY (CaCO3 Stability, Langelier Index):

1)   SM 203, SM 2330

2)          ASTM D513-82

     e.     EDB in groundwater:

1)   EPA 601 modified using an electron capture detector instead of an electrolytic conductivity detector

2)   EPA 504

3)   HRS (Florida Department of Health and Rehabilitative Services) Method for the analysis of EDB

4)   EPA 8011

     f.     ODOR - SM 207, SM 2150

     g.     SALINITY:

1)   SM 210A, SM 2520 B

2)   SM 210B, SM 2520 C

3)   SM 210C

     h.     TASTE:

1)   SM 211 A, B, SM 2160 B, C, D

2)   ASTM 1292-86

     i.     TOTAL DISSOLVED GASES - SM 2810

     j.     TRANSPARENCY - 17-3.031(6), F.A.C.

     k.     UN-IONIZED AMMONIA - DER-SOP - DER Central Analytical Laboratory, Tallahassee, FL, Revision No. 1, October 3, 1983.  (Available from the DER QA Section)

 

**      Methods coded SM XXX are from Standard Methods for the Examination of Water and Wastewater, 16th Edition, 1983, those coded SM XXXX are from the 17th Edition, 1989 (except Chlorophyll where SM 1002G is from the 16th Edition and SM 10200H is from the 17th Edition).  Methods coded ASTM are from the American Society for Testing Materials.

Table 2.3, cont.

DER APPROVED ANALYTICAL METHODS AND REFERENCES FOR WATER

AND BIOLOGICAL ANALYSES

 

BIOLOGICAL

      Microbiological

      1)      Drinking Water Analyses - 40 CFR Part 141, Subpart C (Monitoring and Analytical Requirements, section 141.21), July 1, 1991.

      2)      Water and Wastewater Analyses - 40 CFR Part 136, Table IA as published in the Federal Register, Vol. 65, No. 165, pp. 50758-50770, October 8, 1991. Table 2.3, cont.

      3)      "Microbiological Methods for Monitoring the Environment" EPA 600/8-78-017, 1978.

      4)      Standard Methods for the Examination of Water and Wastewater, APHA-AWWA-WPCF, 17th Edition, 1989.

 

      Bioassay

      1)      "Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms (Fourth Edition)" EPA 600/4-90-027, September, 1991.

      2)      "Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms (Third Edition)" EPA 600/4-91-002, 1991.

      3)      "Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms (Second Edition)" EPA 600/4-91/003, 1991.

 

      Macrobenthic Identification and Enumeration

      1)      "Macroinvertebrate Field and Laboratory Methods for Evaluating the Biological Integrity of Surface Waters", ORD, Washington, D.C., November 1990

 

      2)      Standard Methods for the Examination of Water and Wastewater, Part 10500, 17th Edition, APHA, 1989.

 


 

Table 2.4 DER APPROVED ANALYTICAL METHODS AND REFERENCES FOR

SEDIMENTS, SOILS, RESIDUALS AND SOLID AND HAZARDOUS WASTES

 

SOILS AND SEDIMENTS

      1)      "Test Methods for Evaluating Solid Waste, Physical Chemical Methods", Third Edition (EPA SW-846), 1986 as amended by Final Update 1, November 1990.

      2)      "Procedures for Handling and Chemical Analysis of Sediments and Water Samples" EPA/Corps of Engineers, EPA/CE-81-1, 1981.

      3)      *"USEPA Contract Laboratory Program Statement of Work for Inorganic Analysis", ILMO 2.0 (July 1990) and ILMO 2.1 (September 1991).

      4)      *"USEPA Contract Laboratory Program Statement of Work for Organic Analysis", ILMO 2.0 (July 1990) and ILMO 2.1 (September 1991).

      5)      Estuarine Sample Preparation and Analysis - Deepwater Ports Maintenance Dredging and Disposal Manual, Department of Environmental Regulation, Coastal Zone Management, Revision 4, December 1984.

 

DOMESTIC AND INDUSTRIAL SLUDGES (RESIDUALS)

      1)      "Test Methods for Evaluating Solid Waste, Physical Chemical Methods", Third Edition (EPA SW-846), 1986 as amended by Final Update 1, November 1990.

      2)      "POTW Sludge Sampling and Analysis Guidance Document" USEPA Permits Division, August 1989.

 

SOLID AND HAZARDOUS WASTES

      1)      "Test Methods for Evaluating Solid Waste, Physical Chemical Methods", Third Edition (EPA SW-846), 1986 as amended by Final Update 1, November 1990.

      2)      40 CFR Part 261, Identification and Listing of Hazardous Waste, July 1, 1991, Appendix III (Chemical Analysis Test Methods).

      3)      *"USEPA Contract Laboratory Program Statement of Work for Inorganic Analysis", ILMO 2.0 (July 1990) and ILMO 2.1 (September 1991).

      4)      *"USEPA Contract Laboratory Program Statement of Work for Organic Analysis", ILMO 2.0 (July 1990) and ILMO 2.1 (September 1991).

 

      *      Methods from these references shall be used and/or referenced by laboratories under direct contract to EPA to perform analyses for Superfund (CERCLA) site investigations.


 

Table 2.5 DER APPROVED METHODS FOR SPECIAL CONDITIONS

(INCLUDES DRAFT AND MODIFIED METHODS)

 

SOLID SAMPLES (Soils, Sediments, Sludges, Residuals, etc.):

 

      1)      Total Recoverable Hydrocarbons (Petroleum) - SW 846 method 9073 (draft)*

      2)      Total Halides:

a)          SW 846 method 5050/9056

b)          SW 846 method 5050/9252

c)          SW 846 method 5050/9253

      *      Copy available from the DER QA Section

 

 

MODIFIED METHODS:

 

EPA Methods 300.0 (Revised August 1991) and 9056 - Method 300.0 may be used for the analysis of the METHOD SPECIFIED ions in groundwater and surface water. Method 9056 may be used for the METHOD SPECIFIED ion EXCEPT for fluoride.

 

EPA Methods 601, 602, 624 and 625 - Capillary columns may be used instead of the specified packed columns if the laboratory can meet the performance criteria (precision, accuracy and method detection limits) of the method.

 

EPA Methods 601 & 602 - The photoionization detector and electrolytic conductivity detector may be used in series if the laboratory can meet the performance criteria of the specified methods.

 

EPA Methods 602, 8020, & 8021 - May include the analyses for xylenes and methyl tert-butyl ether (MTBE).  Note:  required for Chapter 17-770 work.

 

EPA Method 610, 625, 8100, 8310, 8250 & 8270 - May include the analyses for 1-methylnaphthalene and 2-methylnaphthalene.  Note:  required for Chapter 17-770 work.

 

EPA Method 5030/8010 - Must be modified to analyze for EDB in soils.  An electron capture detector instead of a electrolytic conductivity detector must be used.


b.            If no appropriate method exists in any of the above-referenced documents, a full method validation package (as outlined in Rule 17-160.520, F.A.C.) must be submitted as an appendix to the CompQAP

            3.            Modified or Alternative Methods

a.            Modified Methods - Any modification to approved analytical methods must be identified in the table as  "mod", and details of the modification must be provided as an attachment even if the modification has been approved by DER or EPA.

b.            Alternative methods - A laboratory who wishes to use an alternative method that is not listed on Tables 2.3, 2.4 or 2.5 must list the method number in the table, and added as an attached a method validation/equivalency package that has been prepared per the instructions in Appendix E of DER-QA-001/90.

c.            If components which are not specified by the analytical method are analyzed (e.g. malathion using method 608), a method validation package (see Appendix E of DER-QA-001/90) must be submitted for review and approval, and must be included as an appendix to the CompQAP.

 

ALL METHODS THAT DO NOT HAVE EPA OR DER APPROVAL MUST BE REVIEWED AND APPROVED BY DER BEFORE USING ON ANY DER-RELATED WORK.

 

c.            Methods Section Format - Laboratories must include a minimum of two tables (sample preparation and analysis methods); three if sample collection activities are included in capabilities.  Field QA Plans must include a table of analysis methods.

      1.      Sample Preparation - Sample preparation method numbers must be presented for any EPA SW 846 method that does not specify a sample preparation (extraction, digestion, clean up, etc.) method.  These sample preparation methods shall identify the sample preparation number and the appropriate methods to which the procedure applies (see Fig. 2.2).   

 

Figure 2.2 EXAMPLE OF SAMPLE PREPARATION TABLE

   


Section 4.0
7-22-95
Page 5 of 135

 

Table 2.1
SAMPLE PREPARATION METHODS

 

Sample Prep.

 

 

 

Method Number

Description

Matrix

Sample Prep for these Methods:

 

 

 

 

3005       

Acid Digestion       

Water

6010, 7020. 7040, 7080, 7130

3020       

Acid Digestion       

Water, Soil

7041, 7091, 7131

3015       

Microwave Digestion       

Water

6010

 

 

 

 

3510       

Liquid/Liquid Extraction

Water

8081, 8141

3540       

Soxhlet Extraction

Soil

8081, 8141

 


      2.      Analytical methods - This table must include information concerning analytes, method numbers, matrices and quality control criteria:

a.            Method Number

      1.      Method numbers must be provided for each proposed matrix and component.

            2.            List all equivalent methods (i.e. SW 846 and "600" series methods) if seeking approval to perform analyses by both methods.

b.            Matrix Identification - Since precision and accuracy objectives are matrix specific, each method must identify the matrices to be analyzed.  Identify the matrix groups as follows:

      1.      Drinking water

      2.      Water - Includes surface water, groundwater and wastewater (these may be identified separately)

      3.      Saline waters

      4.      Soils and sediments

      5.      Chemical wastes (includes sludges and residuals from domestic or industrial wastewater processing)

      6.      Biological tissues (includes shellfish, fish and mammalian)

c.            Component Name - All components (compounds or chemicals) that are to be analyzed must be listed.

      1.      If a primary method (ex. Method 608) has published addenda (ex.  Method 608.1 and Method 608.2) and if the components in the addenda are to be analyzed, these analytes may be included under the same method number heading.

      2.      Use component names as they are listed in the method.

d.            Precision Targets

      1.      Must be described by the maximum allowable variance and reported as the upper acceptable value (e.g. 5%).  The specific units (i.e. % RSD, RPD, I) shall be identified and calculated according to the formulas specified in Chapter 9 of this document.  NOTE:  RPD AND THE INDUSTRIAL STATISTIC WILL BE CONVERTED TO % RSD IN THE QA DATA BASE.

      2.      All precision limits must be generated from in-house data.  If no data exists, published method values or internal goals may be used until in-house values can be generated. 

      3.      All internal goals, literature or method reference data must be identified.

e.            Accuracy Targets

      1.      Must be reported as a range (e.g. 90-125%) and calculated per instructions in Chapter 9.

      2.      Accuracy target values should be derived from historical in-house data.  If unavailable, method targets or internal goals may be used until in-house values are available.

      3.      All internal goals, literature or method targets must be properly identified.

f.            Method Detection Limits (MDLs) or Practical Quantitation Limits (PQLs)

      1.      The method detection limit or practical quantitation limit for each component must be provided.

      2.      Identify the reporting units (e.g. mg/kg, ug/L, etc.) and whether MDL or PQL.

      3.      Do not mix MDL and PQLs on the same tables.  Enter values for only one of the two types.

4.      Specify the method by which the MDLs were calculated (see Chapter 9):  EPA, IUPAC or USATHAMA.

a.            Note:  Since PQLs are based on the determination of MDLs, the method by which MDLs are calculated is required EVEN IF PQLs are reported.

b.            The QA Data Base will convert all reported PQL values to MDLs using the definition of PQL specified in Chapter 9.  This means that all PQL values will be divided by a factor of 4.

5.      Criteria or Action level goals may be listed in lieu of MDLs or PQLs if these requirements are met:

a.            Criteria or action levels that must be met for a specified permit or program exceed the minimum detection limit of the method by two orders of magnitude (e.g. MDL is 2 ppb, the criteria or required reporting level is 200 ppb).

b.            These targets are identified by specific reference to Department Criteria or permit requirements.

c.            The use of elevated targets is justified in this section.

g.            QA Target Concentration Ranges

      1.      For each QA Target of precision and accuracy, identify the concentration level that was used to determine the value.  The following codes and concentration definitions shall be used:

a.            L - low range is the lower 20% of the linear calibration range.

b.            M - mid range is defined as the concentrations from 20% to 80% in the linear calibration range.

c.            H - high range is defined as the concentrations which are in the upper 80% of the linear calibration range.

h.            The following acronyms shall be used to prepare these tables:

      1.      EPA      refers to methods found in any EPA approved source

      2.      SM      refers to methods found in Standards Methods (specify edition)

      3.      ASTM      refers to method references from ASTM

      4.      USGS      refers to method references from the US Geological Survey documents

      5.      AOAC      refers to method references from the Methods of Analysis of the Association of Official Analytical Chemists

      6.      NA            Not applicable

      7.      MDL      Method Detection Limit

      8.      PQL      Practical Quantitation Limit

      9.      MOD      Modified Method

      10.      DW      Drinking water

      11.      SW      Surface water

      12.      GW      Groundwater

      13.      SED      Sediments (includes domestic sludges)

      14.      S            Soils

      15.      EFF      Effluent

      16.      HW      Hazardous Wastes (includes chemical wastes and sludges)

      17.      BIO      Samples from biological matrices (tissues, muscle, shellfish, etc.

      18.      SA            Saline waters

 

d.            Examples of the required formats for laboratory and field parameters are found in Figures 2.3 and 2.4.

 

Figure 2.3 EXAMPLE OF QA OBJECTIVES TABLE OF LABORATORY MEASUREMENTS


Section 5
6-15-94
Page 6 of 30

 

TABLE QRS

QUALITY ASSURANCE OBJECTIVES

 

Method

 

 

Prec.

Conc.

Accuracy

Conc.

MDL

#

Matrix

Analyte/Component

%RSD

Range

%R

Range

mg/kg

 

 

 

 

 

 

 

 

EPA 8060

Sed

Bis(2-ethylhexyl)phthalate  

30

L

29-137

L

670

 

 

Butyl benzyl phthalate

30

L

0-140

L

330

 

 

D-n-butyl phthalate

30

L

8-111

L

330

 

 

Diethyl phthalate 

30

L

0-100

L

330

 

 

Dimethyl phthalate

30

L

0-100

L

330

 

 

Di-n-octyl phthalate

30

L

19-132

L

330

 

 

 

 

 

 

 

 

EPA 8060

GW

Bis(2-ethylhexyl)phthalate

30

L

54-80

L

3

608

SW

Butyl benzyl phthalate

30

L

68-108

L

3

 

 

Di-n-butyl phthalate

30

L

78-114

L

3

 

 

Diethyl phthalate 

30

L

36-54

L

3

 

 

Dimethylphthalate 

30

L

54-90

L

3

 

 

Di-n-octyl phthalate

30

L

66-84

L

3

 

 

 

 

 

 

 

 

EPA 8080

GW

Aldrin

35

L

58-100

L

0.01

8081

SW

"-BHC

35

L

59-100

L

0.01

608

DW

$-BHC

35

L

61-100

L

0.01

608.1

EFF

*-BHC

35

L

61-100

L

0.01

608.2

 

(-BHC

35

L

60-100

L

0.01

 

 

Chlordane

35

L

45-119

L

0.2

 

 

p,p’-DDD 

35

L

55-115

L

0.02

 

 

p,p’-DDE

35

L

50-100

L

0.02

 

 

p,p’-DDT

35

L

60-120

L

0.05

 

 

Dieldrin

35*

L

60-120*

L

0.02*

 

 

Endosulfan I

35*

L

60-120*

L

0.05*

 

 

Endosulfan II

35*

L

45-100*

L

0.01*

 

 

Endosulfan sulfate

35

L

60-160

L

0.05

 

 

Endrin

35

L

30-147

L

0.01

 

 

Endrin aldehyde

35

L

30-100

L

0.01

 

 

Heptachlor

35

L

60-110

L

0.01

 

 

Methoxychlor

35

L

60-110

L

0.2

 

 

PCNB^^

35

L

50-100

L

0.05

 

 

Toxaphene

35

L

41-126

L

0.5

 

MDLs have been calculated based on the 40-CFR, Part 136 Method

 

*    QA Targets derived from literature values

 

^^   Additional component - Method validation study attached as Appendix A


 

 

Figure 2.4 EXAMPLE OF METHODS TABLE FOR FIELD MEASUREMENTS


Section 5.0
8-17-90
Page 5 of 27

 

TABLE XYZ
QUALITY ASSURANCE OBJECTIVES

Field Measurements
 

Method #

Matrix

Analyte/Component

EPA 150.1

W

pH

EPA 170.1

W

Temperature

SM 2510 B

W

Specific Conductance

EPA 360.1

W

Dissolved Oxygen

EPA 180.1

W

Turbidity

 


 

      2.3.3.5      Section 2.0 - Organization Abilities - Sampling Capabilities

      Organization that analyze samples must include this list as an additional list in Section 2.0.

 

a.            Sampling capabilities must be listed in table form by major matrix groups and major analyte groups.  The matrix groups shall be identified as:  groundwater, surface water, drinking water, wastewater, stormwater runoff, soils, sediments, tissues, shellfish, domestic wastewater sludges, hazardous waste sludges, and liquid hazardous wastes.

            The major analyte groups are defined as follows:

      1.      VOCs - Volatile Organic Compounds to include Methods 601, 602, 624, 502.1 and 2, 503, 504, 524.1 and .2, 8010, 8020, 8021, 8240, 8260, EDB and purgeable organic halides.

      2.      Extractable Organics - To include base neutral components (e.g. polynuclear aromatics), acid extractable components (e.g. phenols), pesticides, herbicides, and PCBs.

      3.      Metals - All metallic analytes

      4.      Inorganic Anions - To include inorganic anions and other non-metallic tests:  bromide; bromine; chloride; chlorine; iodide; nutrients (ammonia, Kjeldahl nitrogen, nitrate, nitrite, phosphate, o-phosphate); sulfate; silica; sulfite; acidity; alkalinity; dissolved oxygen and dissolved silica.

      5.      Organics - To include biochemical oxygen demand, chemical oxygen demand, oil and grease, total organic carbon, total recoverable petroleum hydrocarbons, phenolics, and surfactants.

      6.      Physical Properties - To include color, specific conductance, hardness, odor, pH, all residues (filterable, non-filterable, total, volatile and settleable), temperature and turbidity.

 

      7.      Microbiology - To include coliforms, streptococcus, enterococcus and other bacteria.

      8.      Other - Tests that must be included are:  cyanide; biotoxicity; macroinvertebrate identification; and radionuclides.

 

See Figure 2.5 for the specified format.

 

      2.3.3.6      Section 3.0 - Sampling Equipment and/or Analytical Instrumentation

 

      On SEPARATE LISTS, list the laboratory and/or field equipment that is used by the organization:

 

a.            Field Equipment

      1.      The sampling equipment list must be limited to equipment that the organization either owns or rents on a routine basis.

      2.      The list must be presented in format specified in Fig. 2.6.  Note that construction materials of all purging and sampling equipment (including tubing) must be specified.

      3.      In addition to sample collection/purging equipment, the following must be listed:

      a.            All field measurement equipment (pH meters, conductivity meters, etc.) and all field screening equipment (OVAs, GCs, etc.);

      b.            All field decontamination equipment; and

      c.            Miscellaneous and ancillary equipment (water level indicators, buckets, gloves, etc.).

 

b.            Laboratory Analytical Instrumentation and Support Equipment

      1.      The list of laboratory instrumentation must identify the type of instrument.  This list shall include but is not limited to:

a.            Gas Chromatograph (detector types must be listed;

b.            Mass spectrometer (identify whether MS or ITD);

c.            ICP (specify whether sequential or simultaneous);

d.            HPLC (detector types must be listed;

e.            Types of spectrophotometers (UV-VIS, IR, etc.); and

f.            Atomic absorption spectrophotometers including all auxiliary atomic absorption equipment (furnace, flame, hydride, cold vapor, etc.)

      2.      Support Equipment should include:

a.            Analytical balances;

b.            Microscopes;

c.            TCLP and/or EP Toxicity equipment; and

d.            Ovens, refrigerators, water baths and incubators.

 

      2.3.3.7      Submission of CompQAP on Diskette

a.            All information listed above may be submitted on diskette as an ASCII flat file.  The specific format may be obtained by writing or calling the QA Section or by accessing the information through the QA Bulletin Board.

b.            A CompQAP that is submitted in this manner must be accompanied by a signed and notarized hard copy of the Statement of Intent.

c.            The initial screening review and determination of the QA Plan status will be performed when the information is uploaded into the QA data base.  Additionally, the approved capabilities of your organization will be immediately accessible to DER Staff and the HRS Certification program.


Figure 2.5

EXAMPLE OF TABLE OF SAMPLING CAPABILITIES


Section 6.0
6-27-96
Page 1 of 10

 Table 6.5
 SAMPLING CAPABILITIES
 

Parameter Group

Sample Source

 

 

Extractable Organics

Drinking water, surface water, groundwater, sediments, soils, hazardous waste sludge

 

 

Volatile Organics

Drinking water, surface water, groundwater, sediments, soils, hazardous waste sludge

 

 

Trace Metals

Drinking water, surface water, groundwater, sediments, soils, hazardous waste sludge

 

 

Physical Properties

Surface water, groundwater

 

 

Inorganic Anions

Surface water, groundwater

 

 

Microbiology

Drinking water, surface water, groundwater, sediments, soils, domestic residuals


 

 

Figure 2.6

EXAMPLE OF FIELD EQUIPMENT TABLE  


Section 6.1

12-17-97

Page 3 of 34

 

SAMPLING EQUIPMENT USED BY QRS CONSULTANTS

 

Equipment

Construction

Use

Parameter Groups

Groundwater

 

 

 

Submersible Turbine Pump

SS Housing w/ PVC Tubing & Check Valve

Purging required

All; polishing

 

 

Sampling

Inorganic Anions, Metals

 

 

 

 

 

SS Housing w/ Teflon Tubing & Check Valve

Purging

All

 

 

Sampling

All except VOCs

 

 

 

 

Centrifugal Pump

Teflon Tubing w/ Check valve

Purging

All

 

 

 

 

Surface Water

 

 

 

Sample Container

Glass

Grab Sample

All except Si and F

 

 

 

 

 

Plastic

Grab Sample

Inorganic Anions Metals, Microbiology

 

 

 

 

DO Dunker

Glass

Grab Sample

All

 

Field Instruments

 

 

Equipment

Model & Mfg.

Use

pH Meter

Acme 4000

Determine Well Stability, Field Measurement

 

Miscellaneous Equipment

Equipment

Construction

Use

Parameter Groups

pH Standards

 

 

 

   4.0, 7.0 & 10

Original Container

Calibration  

pH

1+1 HCl

Plastic Container

Decontamination

All

1+1 Nitric

Plastic Container

Decontamination

All except Nox

Analyte Free Water

Glass

Decontamination Transport

All

 

Teflon Squeeze Bottle

Decontamination Dispensing

All

 


 

 

 

2.4              COMPQAP FORMAT WHEN ADOPTING PORTIONS OF THE SOPS

 

      The Comprehensive QA Plan must be submitted in the 15-element format specified in the DER Manual for Preparing Quality Assurance Plans (DER-QA-001/91, Revised 1992) and must contain all required information for those sections or activities that ARE NOT adopted by SOPs.

 

2.4.1      All topics specified by the DER Manual for Preparing Quality Assurance Plans must be included in this document.  The subject matter may be by reference to adopted SOPs or must be fully discussed in the QA Plan text.

 

2.4.2      A signed statement of intent (see Section 2.2 above) must be submitted and will REPLACE the title page.

 

2.4.3      All activities or protocols from the SOP that are listed on the statement of intent may be referred to by citation (see instruction below).  This means that the SOP information DOES NOT NEED TO BE COPIED INTO TEXT OR ATTACHED AS AN APPENDIX.

 

      2.4.3.1      A BLANKET REFERENCE TO THE ENTIRE SOP DOCUMENT IS NOT ACCEPTABLE.  That is, you must specify the section or subsection that are pertinent to your operations.

 

2.4.3.2      References to the POTW Sludge Sampling Document or the EPA Region IV Standard Operating Procedures and Quality Assurance Manual must state the protocol and specify the section, page number(s) and revision date.

      Example:

      "Waste sampling in pits, ponds and lagoons will follow 4.12.3, pp. 3-5, revised February 1991."

 

2.4.3.3      References to the SOPs written by the QA Section must state the protocol, the document title, section or subsection and revision date.

      Examples:

      "Sample Collection for Surface Water Samples will be performed in accordance with the documents and references specified in the DER Standard Operating Procedures for Laboratory Operations and Sample Collection Activities, Section 4.2.1, revised 6-92."

 

      "Sample containers will be obtained by option b in the DER Standard Operating Procedures for Laboratory Operations and Sample Collection Activities, Section 4.4.1, revised 6-92."

 

      "Laboratory sample documentation will be organized and maintained in accordance with the requirements specified in the DER Standard Operating Procedures for Laboratory Operations and Sample Collection Activities, Section 5.0, revised 6-92."