Clean Harbors Deer Trail, LLC

Waste Analysis Plan

Appendix C
October 2004

WASTE ANALYSIS PLAN

ANALYTICAL METHODS
APPENDIX C
I.

METALLIC ANALYTES
A.

Sample Preparation Methods (Reference: SW-8461)

Method 3005:

Acid Digestion of Water for Total Recoverable or Dissolved Metals

for Analysis by Flame Atomic Absorption (FLAA), Inductively
Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES), or
Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

Method 3010:

Acid Digestion of Aqueous Samples and Extracts for Total Metals

for Analysis by Flame Atomic Absorption (FLAA), Inductively
Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES), or
Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

Method 3015:

Microwave Assisted Acid Digestion of Aqueous Samples and

Extracts for Analysis by Flame Atomic Absorption (FLAA),
Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICPAES), or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

Method 3020:

Acid Digestion of Aqueous Samples and Extracts for Total Metals

for Analysis by Graphite Furnace Atomic Absorption Spectroscopy
(GFAA) or Inductively Coupled Plasma-Mass Spectrometry (ICPMS)

Method 3031:

Acid Digestion of Oils for Metals Analysis by Flame Atomic

Absorption (FLAA) or Inductively Coupled Plasma-Atomic
Emission Spectroscopy (ICP-AES)

Method 3040:

Dissolution Procedure for Oils, Greases, or Waxes

Method 3050:

Acid Digestion of Sediments, Sludges, and Soils for Analysis by

Flame Atomic Absorption (FLAA), Inductively Coupled PlasmaAtomic Emission Spectroscopy (ICP-AES), or Inductively Coupled
Plasma-Mass Spectrometry (ICP-MS)

Method 3051:

Microwave Assisted Acid Digestion of Sediments, Sludges and Oils

for Analysis by Flame Atomic Absorption (FLAA), Inductively
Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES), or
Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)
Microwave Assisted Acid Digestion of Siliceous and Organically
Based Matrices

Method 3052:

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

Method 3060:

B.

Alkaline Digestion for Hexavalent Chromium by SW-846 Methods

7196 (Colorimetric) or 7199 (Ion Chromatography)

Methods for Determination of Metals (Ref: USEPA SW-8461)

Method 6010:
Method 6020:
Method 7000:
Method 7020:
Method 7040:
Method 7041:
Method 7060:
Method 7061:
Method 7080:
Method 7090:
Method 7091:
Method 7130:
Method 7131:
Method 7140:
Method 7190:
Method 7191:
Method 7195:
Method 7196:
Method 7197:
Method 7199:
Method 7200:
Method 7201:
Method 7210:
Method 7211:
Method 7380:
Method 7420:
Method 7421:
Method 7430:
Method 7450:
Method 7460:
Method 7470:
Method 7471:
Method 7480:
Method 7481:
Method 7520:
Method 7550:
Method 7610:

Inductively Coupled Plasma Atomic Emission Spectroscopy (ICPAES)

Inductively Coupled Plasma Mass Spectroscopy (ICP-MS)
Atomic Absorption Methods
Aluminum (AA, Direct Aspiration)
Antimony (AA, Direct Aspiration)
Antimony (AA, Furnace Technique)
Arsenic (AA, Furnace Technique)
Arsenic (AA Gaseous Hydride)
Barium (AA, Direct Aspiration)
Beryllium (AA, Direct Aspiration)
Beryllium (AA, Furnace Technique)
Cadmium (AA, Direct Aspiration)
Cadmium (AA, Furnace Technique)
Calcium (AA, Direct Aspiration)
Chromium (AA, Direct Aspiration)
Chromium (AA, Furnace Technique)
Chromium, Hexavalent (Coprecipitation)
Chromium, Hexavalent (Colorimetric)
Chromium, Hexavalent (Chelation/Extraction)
Chromium, Hexavalent (Ion Chromatography)
Cobalt (AA, Direct Aspiration)
Cobalt (AA, Furnace Technique)
Copper (AA, Direct Aspiration)
Copper (AA, Furnace Technique)
Iron (AA, Direct Aspiration)
Lead (AA, Direct Aspiration)
Lead (AA, Furnace Technique)
Lithium (AA, Direct Aspiration)
Magnesium (AA, Direct Aspiration)
Manganese (AA, Direct Aspiration)
Mercury in Liquid Waste (Manual Cold-Vapor Technique)
Mercury in Solid or Semisolid Waste (Manual Cold-Vapor
Technique)
Molybdenum (AA, Direct Aspiration)
Molybdenum (AA, Furnace Technique)
Nickel (AA, Direct Aspiration)
Osmium (AA, Direct Aspiration)
Potassium (AA, Direct Aspiration)

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

Method 7740:
Method 7741:
Method 7760:
Method 7761:
Method 7770:
Method 7780:
Method 7840:
Method 7841:
Method 7870:
Method 7910:
Method 7911:
Method 7950:
Method 7951:

H.

Selenium (AA, Furnace Technique)

Selenium (AA, Gaseous Hydride)
Silver (AA, Direct Aspiration)
Silver (AA, Furnace Technique)
Sodium (AA, Direct Aspiration)
Stromium (AA, Direct Aspiration)
Thallium (AA, Direct Aspiration)
Thallium (AA, Furnace Technique)
Tin (AA, Direct Aspiration)
Vanadium (AA, Direct Aspiration)
Vanadium (AA, Furnace Technique)
Zinc (AA, Direct Aspiration)
Zinc (AA, Furnace Technique)

ORGANIC ANALYTES (Ref. USEPA SW-8461)

A

Extractions and Preparations

Method 3500:
Method 3510:
Method 3520:
Method 3535:
Method 3540:
Method 3541:
Method 3545:
Method 3550:
Method 3580:
Method 5030:
Method 5035:

B.

Organic Extraction and Sample Preparation

Separatory Funnel Liquid-Liquid Extraction
Continuous Liquid-Liquid Extraction
Solid-Phase Extraction (SPE)
Soxhlet Extraction
Automated Soxhlet Extraction
Accelerated Solvent Extraction
Ultrasonic Extraction
Waste Dilution (Solvent Dilution Prior to Cleanup)
Purge-and-Trap
Closed-System Purge-and-Trap and Extraction for Volatile Organics
in Soil and Waste Samples

Cleanup Methods
Method 3600:
Method 3610:
Method 3611:
Method 3620:
Method 3630:
Method 3640:
Method 3650:
Method 3660:
Method 3665:

Cleanup
Alumina Column Cleanup
Alumina Column Cleanup and Separation of Petroleum Wastes
Florisil Column Cleanup
Silica Gel Cleanup
Gel-Permeation Cleanup
Acid-Base Partition Cleanup
Sulfur Cleanup
Sulfuric Acid/Permanganate Cleanup

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

C.

Gas Chromatographic(GC)Methods
Method 8000:
Method 8015:
Method 8021:
Method 8031:
Method 8032:
Method 8061:
Method 8070:
Method 8080:
Method 8081:
Method 8082:
Method 8100:
Method 8121:
Method 8140:
Method 8141:
Method 8150:
Method 8151:

D.

Gas Chromatographic/Mass Spectrometry (GC/MS) Methods

Method 8260:
Method 8270:
Method 8280:

Method 8290:

E.

Gas Chromatography
Nonhalogenated Volatile Organics (Includes Alcohols)
Halogenated Volatile Using Photoionization and Electrolytic
Conductivity Detectors in series: Capillary Column Technique
Acrylonitrile
Acrylamide
Phthalate Esters, Capillary Column with ECD
Nitrosamines
Organochlorine Pesticides and PCBs
Organochlorine Pesticides and PCBs as Aroclors: Capillary Column
Technique
Polychlorinated Biphenyls (PCBs): Capillary Column Technique
Polynuclear Aromatic Hydrocarbons
Chlorinated Hydrocarbons: Capillary Column Technique
Organophosphorus Compounds
Organophosphorus Compounds: Capillary Column Technique
Chlorinated Herbicides
Chlorinated Herbicides using Methylation or
Pentafluorobenzylation Derivatization: Capillary Column Technique

Volatile Organic Compounds: Capillary Column Technique

Semivolatile Organic Compounds: Capillary Column Technique
The Analysis of Polychlorinated Dibenzo-P-Dioxins (PCDDs) and
Polychlorinated Dibenzofurans (PCDFs)
Appendix A: Signal-to-Noise Determination Methods
Appendix B: Recommended Safety and Handling
Procedures for PCDDs/PCDFs
Polychlorinated Dibenzodioxins (PCDDs) and Polychlorinated
Dibenzofurans (PCDFs) by High-Resolution Gas
Chromatography/High Resolution Mass Spectrometry
(HRGC/HRMS)

High Performance Liquid Chromatographic (HPLC) Methods

Method 8315:
Method 8316:
Method 8318:
Method 8330:
Method 8331:

Determination of Carbonyl Compounds

Acrylamide, Acrylonitrile and Acrolein
N-Methylcarbamates
Nitroaromatics and Nitramines
Tetrazene, Reverse Phase

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

F.

Miscellaneous Screening Methods

Method 3810:
Method 3820:
Method 8275:

Method 9078:
Method 9079:
III.
A.

Headspace
Hexadecane Extraction and Screening of Purgeable Organics
Semivolatile Organic Compounds (PAHs and PCBs) in
Soils/Sludges and Solid Wastes Using Thermal Extraction/Gas
Chromatography/Mass Spectrometry (TE/GC/MS) for Screening
Screening Method for Polychlorinated Biphenyls in Soil
Screening Method for Polychlorinated Biphenyls in Transformer Oils

MISCELLANEOUS ANALYTICAL METHODS

USEPA SW-8461 Methods
Method 1010: Pensky-Martens Closed-Cup Method for Determining Ignitability
Method 1020: Setaflash Closed-Cup Method for Determining Ignitability
Method 111O: Corrosivity Toward Steel
Method 1310:
Method 1311:
Method 1312:
Method 1320:
Method 1330:
Method 9010:
Method 9012:
Method 9013:
Method 9020:
Method 9021:
Method 9022:
Method 9023:
Method 9030:
Method 9035:
Method 9036:
Method 9038:
Method 9040:
Method 9041:
Method 9045:
Method 9050:
Method 9056:
Method 9060:
Method 9065:
Method 9066:
Method 9070:
Method 9071:

Extraction Procedure EP Toxicity Test

Toxicity Characteristic Leaching Procedure (TCLP)
Synthetic Precipitation Leaching Procedure
Multiple Extraction Procedure
Extraction Procedure for Oily Wastes
Total and Amenable Cyanide5 (Colorimetric, Manual)
Total and Amenable Cyanide5 (Colorimetric, Automated)
Cyanide Extraction Procedure for Solids and Oils5
Total Organic Halides (TOX)
Purgeable Organic Halides (POX)
Total Organic Halides (TOX) by Neutron Activation Analysis
Extractable Organic Halides (EOX) in Solids
Sulfides
Sulfate (Colorimetric, Automated, Chloranilate)
Sulfate (Colorimetric, Automated, Methylthymol Blue)
Sulfate (Turbidimetric)
pH Electrometric Measurement
pH Paper Method
Soil pH
Specific Conductance
Determination of Inorganic Anions by Ion Chromatography
Total Organic Carbon (TOC)
Phenolics (Spectrophotometric, Manual 4-AAP with Distillation)
Phenolics (Colorimetric, Automated 4-AAP with Distillation)
Total Recoverable Oil and Grease (Gravimetric, Separatory Funnel
Extraction)
Oil and Grease Extraction Method for Sludge Samples

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

Method 9080:
Method 9081:
Method 9090:
Method 9095:
Method 9100:
Method 9131:
Method 9132:
Method 9212:
Method 9213:
Method 9214:
Method 9215:
Method 9250:
Method 9251:
Method 9252:
Method 9253:
Method 9310:
Method 9315:
Method 9320:

Cation-Exchange Capacity of Soils (Ammonium Acetate)

Cation-Exchange Capacity of Soils (Sodium Acetate)
Compatibility Test for Wastes and Membrane Liners
Paint Filter Liquids Test
Saturated Hydraulic Conductivity, Saturated Leachate
Conductivity, and Intrinsic Permeability
Total Coliform: Multiple Tube Fermentation Technique
Total Coliform: Membrane Filter Technique
Chloride (Potentiometric, Ion Selective Electrode)
Cyanide (Potentiometric, Ion Selective Electrode)
Fluoride (Potentiometric, Ion Selective Electrode)
Sulfide (Potentiometric, Ion Selective Electrode)
Chloride (Colorimetric, Automated Ferricyanide AAI)
Chloride (Colorimetric, Automated Ferricyanide AAII)
Chloride (Titrimetric, Mercuric Nitrate)
Chloride (Titrimetric, Nitrate)
Gross Alpha and Gross Beta Radioactive Isotopes
Alpha-Emitting Radium Isotopes
Radium 228

Chapter 7- USEPA SW-8461

Section 7.1:
Ignitability
Section 7.2:
Corrosivity
Section 7.3.3.2:
Test Method to Determine Hydrogen Cyanide Release from
Wastes
Section 7.3.4.1:
Test Method to Determine Hydrogen Sulfide Release from
Wastes

B.

ASTM3 Methods
Method ASTM D850
Method ASTM D4981-82
Method ASTM E680-79
Method ASTM D240
Method ASTM DI 29
Method ASTM D3120-82
Method ASTM D323
Method ASTM D2709-68
Method ASTM DI 557
Method ASTM D4978-89
Method ASTM D4980-89
Method ASTM D4982-89

Boiling Point
Determination of the Presence of Oxidizers
Determination of Drop Weight Impact Sensitivity of
Solid-Phase Hazardous Materials, Modified
BTU Value
Sulfur Content
Sulfur Content
Vapor Pressure
Water and Sediment in Distillate Fuels by Centrifuge
Bulk Density/Specific Gravity
Sulfides in Waste
pH
Flammability Potential

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

Method ASTM D2887

Boiling Point of Petroleum Products and Fractions by

Gas Chromatography, Modified
Shake Extraction (Leaching) of Solid Waste and
Water

Method ASTM D3987

IV.

WATER METHODS (Ref. USEPA 600/4-79-0202)

A.

Series 100 Methods - Physical Properties

Method 120.1:
Method 130.1:
Method 130.2:
Method 150.1:
Method 160.1:
Method 160.2:
Method 160.3:
Method 160.4:

B.

Specific Conductance
Hardness, Colorimetric, Automated EDTA
Hardness, Titrimetric EDTA
pH, Electrometric Measurement
Total Dissolved Solids
Total Suspended Solids
Total Solids
Total Volatile Solids (Ash)

Series 200 Methods - Metals

Method 200.0:
Method 200.7:
Method 200.8:
Method 202.1:
Method 204.1:
Method 204.2:
Method 206.2:
Method 206.3:
Method 208.1:
Method 208.2:
Method 210.1:
Method 210.2:
Method 213.1:
Method 213.2:
Method 215.1:
Method 215.2:
Method 218.1:
Method 218.2:
Method 218.3:
Method 218.4:
Method 218.5:

Atomic Absorption Methods

Inductively Coupled Plasma (ICP) Methods Atomic
Emission Spectrometric Method for Trace Element Analysis
Inductively Coupled Plasma-Mass Spectrometry (ICPMS)Methods - for Trace Element Analysis
Aluminum (Atomic Absorption, Direct Aspiration)
Antimony (Atomic Absorption, Direct Aspiration)
Antimony (Atomic Absorption, Furnace Technique)
Arsenic (Atomic Absorption, Furnace Technique)
Arsenic (Atomic Absorption, Direct Aspiration)
Barium (Atomic Absorption, Direct Aspiration)
Barium (Atomic Absorption, Furnace Technique)
Beryllium (Atomic Absorption, Direct Aspiration)
Beryllium (Atomic Absorption, Furnace Technique)
Cadmium (Atomic Absorption, Direct Aspiration)
Cadmium (Atomic Absorption, Furnace Technique)
Calcium (Atomic Absorption, Furnace Technique)
Calcium (Titrimetric, EDTA)
Chromium (Atomic Absorption, Direct Aspiration)
Chromium (Atomic Absorption, Furnace Technique)
Chromium (Chelation-Extraction)
Chromium, Hexavalent (Atomic Absorption, ChelationExtraction)
Chromium, Hexavalent (Atomic Absorption, Furnace
Technique)

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

Method 219.1:
Method 219.2:
Method 220.1:
Method 220.2:
Method 236.1:
Method 239.1:
Method 239.2:
Method 242.1:
Method 243.1:
Method 243.2:
Method 245.1:
Method 245.2:
Method 249.1
Method 249.2:
Method 258.1:
Method 270.2:
Method 270.3:
Method 272.1:
Method 272.2:
Method 273.1:
Method 279.1:
Method 279.2:
Method 282.1:
Method 282.2:
Method 286.1:
Method 286.2:
Method 289.1:
Method 289.2:
C.

Cobalt (Atomic Absorption, Direct Aspiration)

Cobalt (Atomic Absorption, Furnace Technique)
Copper (Atomic Absorption, Direct Aspiration)
Copper (Atomic Absorption, Furnace Technique)
Iron (Atomic Absorption, Direct Aspiration)
Lead (Atomic Absorption, Direct Aspiration)
Lead (Atomic Absorption, Furnace Technique)
Magnesium (Atomic Absorption, Direct Aspiration)
Manganese (Atomic Absorption, Direct Aspiration)
Manganese (Atomic Absorption, Furnace Technique)
Mercury (Manual Cold-Vapor Technique)
Mercury (Automated Cold-Vapor Technique)
Nickel (Atomic Absorption, Direct Aspiration)
Nickel (Atomic Absorption, Furnace Technique)
Potassium (Atomic Absorption, Direct Aspiration)
Selenium (Atomic Absorption, Furnace Technique)
Selenium (Atomic Absorption, Gaseous Hydride)
Silver (Atomic Absorption, Direct Aspiration)
Silver (Atomic Absorption, Furnace Technique)
Sodium (Atomic Absorption, Direct Aspiration)
Thallium (Atomic Absorption, Direct Aspiration)
Thallium (Atomic Absorption, Furnace Technique)
Tin (Atomic Absorption, Direct Aspiration)
Tin (Atomic Absorption, Furnace Technique)
Vanadium (Atomic Absorption, Direct Aspiration)
Vanadium (Atomic Absorption, Furnace Technique)
Zinc (Atomic Absorption, Direct Aspiration)
Zinc (Atomic Absorption, Furnace Technique)

Series 300 Methods - Inorganic Non-Metals

Method 300.0:
Method 310.1:
Method 325.2:
Method 335.1:
Method 335.2:
Method 335.3:
Method 340.2:
Method 340.3:
Method 350.1:
Method 350.3:
Method 351.1:
Method 351.2:

Determination of Various Anions by Ion Chromatography

Alkalinity (Titrimetric pH 4.5)
Chloride(Colorimetric, Automated Ferricyanide)
Cyanide (Amenable to Chlorination Titrimetric,
Spectrophotometric)
Cyanide (Total, Titrimetric, Spectrophotometric)
Cyanide (Total, Colorimetric, Automated UV)
Fluoride (Potentiometric Ion Selective Electrode)
Fluoride (Colorimetric, Automated Complexone)
Nitrogen (Ammonia, Colorimetric, Automated Phenate)
Nitrogen (Ammonia, Potentiometric, Ion Selective Electrode)
Nitrogen (Kjeldahl, Total, Colorimetric, Automated Phenate)
Nitrogen (Kjeldahl, Total, Colorimetric, Semi-Automated
Block Digester AAII)

Clean Harbors Deer Trail, LLC

Waste Analysis Plan
Appendix C
October 2004

Method 351.4:
Method 352.1:
Method 353.2:
Method 353.3:
Method 354.1:
Method 360.1:
Method 360.2:
Method 375.1:
Method 375.4:
Method 376.1:
Method 376.2:
D.

Series 400 Methods - Organics

Method 405.1:
Method 415.1:
Method 415.2:
Method 420.2:

E.

Biochemical Oxygen Demand (BOD), 5 Day

Total Organic Carbon (TOC), Combustion or Oxidation
Total Organic Carbon (TOC), UV Promoted, Persulfate
Oxidation
Phenolics, Total (Colorimetric, Automated 4-AAP with
Distillation)

Series 500 Methods - Organic Compounds in Drinking Water

Method 531.1:

F.

Nitrogen (Kjeldahl, Total, Potentiometric, Ion Selective

Electrode)
Nitrate (Colorimetric, Brucine)
Nitrate-Nitrite (Colorimetric, Automated Cadmium
Reduction)
Nitrate-Nitrite (Colorimetric, Manual Cadmium Reduction)
Nitrite (Spectrophotometric)
Oxygen (Dissolved, Membrane Electrode)
Oxygen (Dissolved, Modified Winkler [Full Bottle
Technique)
Sulfate (Colormetric, Automated Chloranilate)
Sulfate (Turbidimetric)
Sulfide (Titrimetric, Iodine)
Sulfide (Colorimetric, Methylene Blue)

Determination of N-Methylcarbamoyloximes and NMethylcarbamates in water by high Pressure Liquid

Chromatography

Series 600 Methods - Organic Compounds in Waste Water

Method 608:
Method 613:
Method 614:
Method 615:
Method 624:
Method 625:

Determination of Organochlorine Pesticides and PCB's by

Gas Chromatography (GC)
Determination of 2,3,7,8-Tetrachlorodibenzo-p-Dioxin by
Gas Chromatography-Mass Spectrometry (GC-MS)
Determination of Organophosphorous Pesticides by Gas
Chromatography (GC)
Determination of Phenoxy Acid Herbicides by Gas
Chromatography (GC)
Determination of Purgeable Volatile Organics by Capillary
Gas Chromatography-Mass Spectrometry (GC-MS)
Determination of Semivolatile Organics by Capillary Gas
Chromatography-Mass Spectrometry (GC-MS)